Location via proxy:   [ UP ]  
[Report a bug]   [Manage cookies]                

Pretreatment of Textile

Download as docx, pdf, or txt
Download as docx, pdf, or txt
You are on page 1of 169

qwertyuiopasdfghjklzxcvbnmqwertyuiopas

dfghjklzxcvbnmqwertyuiopasdfghjklzxcvbn
mqwertyuiopasdfghjklzxcvbnmqwertyuiopa
sdfghjklzxcvbnmqwertyuiopasdfghjklzxcvb
Pretreatment of Textile

nmqwertyuiopasdfghjklzxcvbnmqwertyuio
Preparation for Dyeing and Printing
4/13/2022
pasdfghjklzxcvbnmqwertyuiopasdfghjklzxc
Abel Taye

vbnmqwertyuiopasdfghjklzxcvbnmqwertyui
opasdfghjklzxcvbnmqwertyuiopasdfghjklzx
cvbnmqwertyuiopasdfghjklzxcvbnmqwerty
uiopasdfghjklzxcvbnmqwertyuiopasdfghjkl
zxcvbnmqwertyuiopasdfghjklzxcvbnmqwer
tyuiopasdfghjklzxcvbnmqwertyuiopasdfghj
|Page

klzxcvbnmrtyuiopasdfghjklzxcvbnmqwerty
Table of Contents
Acknowledgment........................................................................................................................................................................................................ iv
1. Introduction............................................................................................................................................................................................................ 1
1.1 Introduction to Pretreatment..............................................................................................................................................................................1
1.4 Process sequence in pretreatment processing...................................................................................................................................................16
2. Singeing and Desizing........................................................................................................................................................................................... 19
2.1 Singeing........................................................................................................................................................................................................... 19
2.4 Desizing........................................................................................................................................................................................................... 33
3. Scouring................................................................................................................................................................................................................. 62
3.3 Scouring........................................................................................................................................................................................................... 62
4. BLEACHING............................................................................................................................................................................................................ 82
4.1 Introduction to Bleaching................................................................................................................................................................................ 82
4.2 Bleaching of cellulosic fibres with NaOCl: Influence of process parameters....................................................................................................87
4.3 Bleaching with NaClO2 (sodium chlorite).........................................................................................................................................................96
4.4 Bleaching with H2O2 (hydrogen peroxide)......................................................................................................................................................102
5. Mercerization....................................................................................................................................................................................................... 111
6. Optical whitening agents................................................................................................................................................................................. 139
7. Combined pre-treatment processes.................................................................................................................................................................... 148
7.1 Introduction................................................................................................................................................................................................... 148
8. Preparation of Protein Fibres............................................................................................................................................................................... 156
8.1 Carbonization................................................................................................................................................................................................. 156
8.2 Wool Scouring................................................................................................................................................................................................ 158

i|Page
8.4 Wool Bleaching.............................................................................................................................................................................................. 161
8.5 Silk degumming.............................................................................................................................................................................................. 164
8.6 Bleaching of silk............................................................................................................................................................................................. 177
9. Preparation of synthetic fibers & blends.............................................................................................................................................................179
9.1 Introduction................................................................................................................................................................................................... 179
9.2 Bleaching of synthetic fibers.......................................................................................................................................................................... 183
Regenerated cellulosic fibers........................................................................................................................................................................... 183
Bleaching of Nylon:.......................................................................................................................................................................................... 184
Bleaching of acrylic fibre:................................................................................................................................................................................. 184
Bleaching of polyester:.................................................................................................................................................................................... 185
9.3 Scouring of blends.......................................................................................................................................................................................... 186
Polyester- cotton.............................................................................................................................................................................................. 186
Polyester-wool blend....................................................................................................................................................................................... 186
Acrylic/wool blends.......................................................................................................................................................................................... 187
9.4 Bleaching of blends........................................................................................................................................................................................ 188
Polyester/cotton.............................................................................................................................................................................................. 188
Polyester/wool blends..................................................................................................................................................................................... 188
Nylon/ Wool blends......................................................................................................................................................................................... 189
10. Assessment of various pretreatment processes................................................................................................................................................191
10.1 Desizing........................................................................................................................................................................................................ 191
10.2 Degradation of Cotton during Desizing........................................................................................................................................................194
10.3 Scouring....................................................................................................................................................................................................... 196
10.4 Degradation of cotton during alkaline scouring...........................................................................................................................................199

ii | P a g e
11. Heat Setting....................................................................................................................................................................................................... 205
11.1 Heat Setting................................................................................................................................................................................................. 205
11.2 Heat setting behavior of different fibres......................................................................................................................................................212
11.3 Effect of setting on Properties: Dyeing, handle, pilling, shrinkage...............................................................................................................220
12. Machinery for preparation of textiles................................................................................................................................................................228

iii | P a g e
Acknowledgment

First of all I express my heartiest thanks and gratefulness to Almighty God for his divine blessing makes me possible to complete this
book successfully. I fell grateful and wish my profound indebtedness to Instructor Mr. Befkad for his entire Advice, endless patience,
scholarly guidance, and continual encouragement starting from the beginning up to the end. Deep knowledge & keen interest of some
Wolkite university staff in department of Textile lab. At last but not the least, I would like to acknowledge my parents for their
approval, support & love to complete the book. Finally I would like to acknowledge that i remain responsible for the inadequacies and
errors, which doubtlessly remain.

iv | P a g e
1. Introduction
1.1 Introduction to Pretreatment
Need for preparation/ pretreatment

The basic objective of pretreatment processing is removal of added or natural


impurities present in textile fibers to improve the absorbency. This prepares
the textile substrate for downstream processes like dyeing, printing, finishing
etc.
4. BLEACHING
Improvement in absorbency brings about
4.1 Introduction to Bleaching
Improved comfort
After desizing and scouring most of the textile fabrics especially
the natural ones, retain slight coloration. The source of the colour
Improved downstream processing
may be:
Improved here means not only higher dye/finish uptake but also more
uniform treatment. Flavone pigment in case of cotton

In case of silk, degumming Soil and dirt


improves acquired
luster from atmosphere
but reduces absorbency

The nature and amount ofContact


naturalwith plant parts
impurities and seeds
present etc.on the fiber
depends
type (generally high in natural
Colourfibers).
acquired Induring
general, syntheticprocessing
mechanical fibers do not
e.g., grease, oil etc.
have any natural impurity. Added impurities are the additives or chemicals
The objective
which are added to facilitate of bleaching
certain processes like isweaving
to destroy this natural
(sizing) or or acquired
color to bring the
prevention of static (lubrication/antistatic textilesduring
treatment in a white
meltstate.
spinning).

Pretreatment stage This may be necessary when:

Is non- value –added stage The fabric


of the has to process
coloration be supplied in white colour

Is often not optimized It needs to be dyed in pastel shades

It needs auxiliaries
Makes excessive use of chemicals, to be printed
and utilities
If the fabric
Is characterized by high carry-over is to be dyed
of preparation in dark shades, then bleaching becomes
residues

1 | P a This
g e makes it imperative to understand the science of impurity removal and
functions of various chemicals and auxiliaries used in pretreatment.

Major Textile fibers


an optional process.

In case of cotton, the motes or the seed coat fragments are visible
on woven or knitted fabrics after scouring. These appear as specks
of brown or black colors on fabric surface. The color of these
motes is also destroyed by bleaching.

Dyeing an unbleached fabric in pastel shades might mask the


brightness of applied color. Many times these bleached fabrics are
given treatment with Optical brightening agents to confer extra
whiteness. Bleaching also removes residual impurities left by other
pretreatment processes like desizing, scouring etc. In that sense, the
absorbency of a cotton fabric may increase after bleaching.

Although reductive bleaching has been used in past to bleach wool


and silk, today almost all textile material are bleached by oxidative
desizing agents.

Broadly speaking, bleaching agents can be classified as:

Oxidative bleaching agents and reductive bleaching agents

Oxidative bleaching agents can be further divided into

Peroxy compounds and Chlorine based compounds

Examples of Peroxy Examples of Chlorine based


compounds compounds

Hydrogen peroxide Bleaching powder

Sodium hypochlorite Sodium hypochlorite

2|Page
Sodium perborate Lithium hypochlorite

Potassium permanganate Sodium chlorite

Peracetic acid

Examples of reductive bleaching agents

Sulphur dioxide

Sodium
hydrosulphite

Sulphoxylates

Acidic sodium
sulphite

Sodium bisulphites

thioureadioxide
increases

The main bleaching agents are:

Sodium hypochlorite (NaOCl)

Sodium Chlorite (NaClO2)

Hydrogen peroxide (H2O2)

The use of oxidative bleaching dates back to the end of eighteenth


century, when solid bleaching powder (based on chlorine) was

3|Page
used for bleaching of cellulosic textiles. The discovery of peroxide
bleaching in 1925 has gradually resulted in replacement of other
bleaching processes with peroxide/peroxygen based bleaches. Out
of the main bleaching agents mentioned above, H2O2 has virtually
replaced chlorine based bleaching. It must be mentioned here that
hypochlorite and chlorite based bleaching is still prevalent in some
developing countries to some extent.

Bleaching with sodium Hypochlorite (NaOCl):

NaOCl is sodium salt of Hypochlorus acid (HOCl). It can be


prepared by passing chlorine gas in a solution of NaOH or by
electrolysis of NaCl solution (aqueous). Sodium hypochlorite is a
strong oxidising agent, with a redox potential of 1400-1550 mV.
Cl2 acts as an oxidising agent in presence of water (moisture) only.
Dry chlorine gas does not have oxidising power.

Cl2 + H2O →HCl +HOCl

HOCl →HCl + [O] ↑

Formation of HOCl is important as it provides the nascent oxygen


molecule responsible for oxidation (bleaching). NaOCl solution in
water undergoes the following reaction:

NaOCl + H2O →NaOH + HOCl

HOCl is a weak acid. Aqueous NaOH solution has a pH of 11-11.5


due to the presence of strong NaOH.

Bleaching occurs due to the following reaction:

4|Page
HOCl →HCl + [O] ↑

In acidic medium, the consumption of hypochlorite is very fast and


can lead to cellulose degradation by oxidation. The reaction is
given below:

NaOCl + HCl → NaCl + HOCl

HOCl + HCl → H2O + Cl2

4.2 Bleaching of cellulosic fibres with NaOCl: Influence


of process parameters
The conditions like concentration, pH, time etc influence bleaching
process in a major way. Generally, cotton is bleached with NaOCl
solution containing 1-3 gpl available chlorine at room temperature
in the pH range 9.5-11.

Available Chlorine or active chlorine   is a unit of   concentration  


used for   hypochlorite -based   bleaches. One gram of 100% active
chlorine bleach has the same bleaching power as one gram of
chlorine. It is based on the assumption that hypochlorite ions can
liberate equivalent amount of iodine by oxidation from a potassium
iodide solution. The amount of iodine liberated is measured
indirectly by titration. Since the same amount of iodine can also be
liberated by equivalent amount of Cl2 gas, the term available
chorine has become popular. In that sense, avilable chlorine is a
measure of active oxidizing matter in the bleach solution. It is
important to determine active or available chlorine in a bleach

5|Page
solution since the bleach may also contain some fraction of
chloride ions (a byproduct of bleach decomposition) which has no
bleaching power. Only hypochlorite ions have bleaching (and
oxidizing power to liberate I2 and cause bleaching).

Liquid bleaches sold for domestic use are typically 3–10% active
chlorine, and should be diluted to 1–2% active chlorine before use.
Commercial domestic bleaching powder is typically about 40%
active chlorine.

Active chlorine values are usually determined by adding an excess


of  potassium iodide  to a sample of bleach solution and  titrating
the  iodine  liberated with standard  sodium thiosulfate  solution.

H2O −
ClO−       + 2I−       + 2 H+   → I2 + Cl
+

(Hypochlorite (Potassium (Acidic (Common


(Iodine)
ion) iodide) solution) salt)

Similarly

Cl2  + 2I−  → I2  + 2Cl−

And (determination of liberated I2 by titration)

2S2O32−  + I2  → S4O62− + 2I−

From the above equations it can be seen that 2 moles of thiosulfate


are equivalent to 70.9 grams (1 mole) of active chlorine or 51.5 g
of hypochlorite ions. In other words a 51.5 gpl solution of OCl− (or
75 gpl NaOCl) is equivalent to 70.9 gpl solution of available

6|Page
chlorine.

Effect of pH

The concentration of different chemical species in bleach bath


depends on ph. The figure 1 given below shows a graph where
relative change in different types of chemical entities with pH
change is shown.

Figure 1 Effect of pH on relative fraction of different chemical


entities in hypochlorite bleach bath

This plot can be divided in three distinct zones:

7|Page
In acidic region (upto pH-5) the sodium hypochlorite hydrolyzes to
form free hypochlorous (HOCl) acid. At lower pH values
hypochlorous acid decomposes and the chlorine gas is liberated
which has no bleaching action. The fraction of free hypochlorous
(HOCl) acid increases as the pH increases and at pH 5, almost all
the hypochite exists as free hypochlorous acid.

At pH-7-7.5, both hypochlorous acid and hypochrorite ions are


present in almost same concentrations.

In the pH range 9-11.5, most of the hypochlorite is present in the


form of OCl− ions and not as free acid. From the figure above it is
clear that consumption of available chlorine is quite low and
oxidation of colored impurities is rather slow. This has less adverse
impact on cotton fibre itself and hence is known as the practical
leaching range for natural cotton fibres.

In the figure 2 below, rate of consumption of available chlorine


resulting in cellulose oxidation from the bleach bath is plotted
against ph.

8|Page
Figure 2 Rate of oxidation of cellulose in terms of the consumption
of half the total available chlorine.

It can be easily seen that rate of oxidation at around pH 7 is the


highest. This means cotton can degrade as the rate of consumption
of available chlorine is quite high. Hence pH-7 is an unsafe zone

9|Page
for bleaching.

The table 1 shown below also quite clearly shows the fraction of


HOCl with change in ph. It is evident that between pH 5 to 10,
there is a drastic change in the concentration of free acid.

Table 1 Change in free acid change in pH

Fraction of
pH hypochlorit
e as HOCl

10.0 0.003

9.0 0.03

8.0 0.21

7.43 0.50

7.0 0.73

6.5 0.91

6.0 0.96

5.0 0.997

The degradation occurring to cotton is measured in terms of cupra


ammonium fluidity. In the figure below, one can see the
degradation of cotton with increasing ph. It is easy to see that the
maximum degradation is occurring near pH-7 region, the same

10 | P a g e
region where the rate of consumption of available chlorine was the
highest. If compared with above figure it looks almost reverse of
that. Hence on can surmise that bleaching with hypochlorite in the
neutral pH range (6-8) is dangerous for cellulosic fibres

Figure 3 Cupra-ammonium fluidity of cotton with change


in pH

Therefore, the best conditions for bleaching are:

11 | P a g e
pH 6-7 (bleaching time 1 min.)

However it is very difficult to control such short time. (can lead to


cotton degradation)

So practical bleaching conditions are:

pH 9-11.5

At pH 9 ------------- time to bleach - 45 min

At pH 11.5 ---------- time approximately 4 hrs.

Temperature --------- Room temperature

Concentration -------- 2-3 gpl available chlorine

Commercial solutions of NaOCl are available as 40% (~ 400 gpl)


solutions.

Bleaching With Sodium Hypochlorite

The advantages of using Sodium hypochlorite as a bleaching agent


are:

It is economical

Risk of catalytic damage is low (this is a problem with


H2O2 bleaching)

Since it is a room tempretaure process, the energy costs are low

However, use of NaOCl is associated with certain disadvantages

12 | P a g e
due to which its use is on the wane. These are:

Fibre damage can take place if temperature and ph are not


controlled.

It results in formation of AOX.

Bleached material can turn yellow on storage

Can degrade many dyes and FBAs (simultaneous dying and


bleaching or bleaching and FBA treatment is not possible)

It cannot be used for bleaching of synthetic or protein fibres.

It does not produce a very satisfactory white.

The residual hypochlorite needs to be removed from the fibres


after bleaching, as it may damage the fibres due to lowering of Ph
on storage (by absorption of CO2 gas from the atmosphere).

The residual hypochlorite, also termed as residual chlorine is


removed by treatment with a reducing agent. This is done by
treating the bleached and rinsed fabric with 2-2.5% of a reducing
agent for 15 mins at 40 °C. Sodium Sulphite, bisulphite,
hydrosulphite, thiosulphate may be used. The treatment is also
known as antichlor treatment.

4.3 Bleaching with NaClO2 (sodium chlorite)


Sodium chlorite is another Chlorine containing oxidising bleaching
agent. It remains stable at high pH and has to be activated with

13 | P a g e
acids or acid liberating agents to bring down the pH when
bleaching takes place.

The bleaching species in Sodium chlorite is ClO 2 gas which is


liberated at pH below 6. The equations below show the
decomposition of chlorite into ClO2 gas and other components.

These acid generators (activators) include Sodium Chloroacetate,


Triethanol Amine, Ammonium Persulphate etc.

Active chlorine values are usually determined by adding an excess


of  potassium iodide  to a sample of bleach solution and  titrating
the  iodine  liberated with standard  sodium thiosulfate  solution.

Acids like formic acetic, phosphoric acids may be used to bring the
pH down. Other alternatives are esters like ethyl lactate or diethyl
tartarate which hydrolyse to give lactic and tartaric acid
respectively.

The figure 4 shown below shows the composition of Sodium


Chlorite solution with changing ph. Time – 1-2 hr

14 | P a g e
Figure 4 Effect of pH on the composition of sodium
chlorite liquors.

Reactions:

4ClO2– + 2H+ → 3ClO2 + Cl– + 2OH–

5ClO2– + 2H+ → 4ClO2 + Cl– + 2OH–

ClO2 is a toxic corrosive gas.

NaClO2 + HCl → NaCl + HClO2           pH 2.5

15 | P a g e
HClO2 → 4ClO2 + HCl +2H2O              at lower pH

NaClO2 is stabilized at higher ph.

As can be seen in the figure above, with reducing pH chlorite ions


start forming chlorous acid (HClO 2). This is a weak acid and
remains un-dissociated at strong acidic conditions. However,
below pH 6, it starts forming ClO2 which is a corrosive and toxic
gas and is supposed to be responsible for bleaching. Formation of
excessive ClO2 gas may result in wastage of the bleaching agent
and may also damage the substrate.

At pH 1-2, the rate of bleaching and the evolution of ClO 2 gas is


very rapid. Hence a balance is struck between the liberation, the
evolution of ClO2 and the rate of bleaching by adjusting the pH in
the range of 3.5-4. This is done with acetic or formic acid and
buffered with Sodium dihydrogen phosphate.

Use of NaClO2 also results in formation of AOX but it is about


only 1/10th of that generated by hypochlorite.

In the figure 2 below, rate of consumption of available chlorine


resulting in cellulose oxidation from the bleach bath is plotted
against ph.

Salient features of NaClO2:

Redox potential – 1040-1200 mV

Bleaching temperature – 70-90 °C

16 | P a g e
Suitable pH for bleaching – 3-4.5(4+-0.2)

Problem of Corrosion with NaClO2 Bleaching:

The CO2 gas released during bleaching has the tendency to corrode


most of the equipment used in the construction of bleaching
equipment. The following approached are used to minimize the
corrosion of bleaching equipment:

Use of corrosion resistant materials like Stainless Steel with 2.5%


Molybdenum. Titanium can be used as the material of construction
but it is very costly. The other option is to have normal stainless
steel vessels lined with Ti, glass or ceramics. Glass fiber reinforced
plastic can also be used as a choice for corrosion resistant material
of construction.

Use of ClO2 scavenging chemicals. These chemicals scavenge and


bind the liberated ClO2 and suppress the corrosion of construction
materials. These are (NH4)H2PO4, sodium and ammonium nitrate,
nitric acid, melamine, urea etc.

Use of chlorite stable surfactants. The foam of the surfactant can


trap the ClO2 gas formed and prevent it from coming in contact
with the walls of the equipment.

Effect of Process Parameters on Bleaching

Effect of Temperature:

NaClO2 is a fibre gentle bleaching agent. It does not affect


cellulose adversely even if bleached at high temperature (100 °C)

17 | P a g e
for several hours.

At boil, the bleaching time is a few hours (1-4).

However, bleaching at ambient temperature may require overnight


batching.

The rate of bleaching rate double for every 10 °C rise in the


process.

Advantages and Disadvantages of Chlorite Bleaching

It can be used for both cotton and synthetic fibres. Since it works
in acidic conditions, it is better suited to bleach synthetic fibres
which are susceptible to alkaline ph.

Since it is used in acidic conditions, hardness of water does not


impair the process (low ash content) .

Leaves material soft. Hence it can be preferred for knitted fabrics.

It can give good white colour with excellent mote removal even
without kier boiling.

It causes very little or no cellulose degradation.

It is insensitive to the presence of metal ions.

Disadvantages

1. More expensive than NaOCl or H2O2.

2. It cannot be used to bleach silk and wool (pink

18 | P a g e
coloration ).

ClO2 can corrode the metals used in construction of


3.
processing vessels.

ClO2 is also a toxic gas, so care should be taken in


4.
handling the bleaching process.

Since in works at acidic pH, wax removal is not very


5.
satisfactory.

Antichlor Treatment

Antichlor treatment is given with Sodium thiosulphate or Oxalic


acid 85-95 °C for goods to be dyed subsequently.

For white goods, an FBA or softening treatment maybe given at


pH 6-7.

4.4 Bleaching with H2O2 (hydrogen peroxide)


H2O2 is gradually replacing other oxidative bleaching processes.
The reasons for its dominance are:

Since it’s by products are only water and oxygen, it is an eco


friendly agent.

It is a versatile and universal bleaching agent. It can be used at


almost any temperature, in batch or continuous processes for
almost all the fibres.

H2O2 is supplied as concentrated transparent solutions in dark

19 | P a g e
bottles. It is quite stable in acidic pH and can decompose in
presence of alkalis or UV light.

Mechanism

H2O2 → H+ + HO2–

HO2– → HO– + [O]

Perhydroxyl ion (HO2–) is the bleaching agent. Its redox potential is


810- 840 mV.

For bleaching to take place, the stabilized H2O2 needs to be


activated with alkalis. In alkaline medium H2O2 decomposes as per
the following reaction:

H2O2 + OH– → OOH– + H2O

The perhydroxy ions formed in the reaction are the actual


bleaching agents which decompose to provide nascent Oxygen (O)
which oxidizes organic compounds including colouring matter.

Above pH 10.8, the formation of HO2– ions is so rapid that it


decomposes to liberate O2 gas which has no bleaching power. The
raid rate of formation can also degrade cotton. Hence pH in
H2O2 bleaching is maintained between 10.5-10.8.

Auxiliaries Used In H2O2 Bleaching

Activator

Stabilizer

20 | P a g e
Sequestering agents

Activators:

Commercially available H2O2 is stabilized at acidic ph. For it to act


as an oxidizing beaching agent, the pH of H2O2 solution must be
increased to basic range with the help of an alkali. The most
commonly used alkali used in raising the pH of the bleach bath is
sodium hydroxide (NaOH).

Stabilizers:

The stabilizers are added to regulate the perhydroxyl ions to


prevent rapid decomposition of bleach bath and fibre damage.
These may act by:

Buffering action

Sequestering of heavy transition metal ions

Complexing with perhydroxy ions dispersing action

The most popular stabilizer used in H2O2 bleaching is Sodium


Silicate. It is easily available, economical and effective. The
preferred ratio of Na2O and SiO2 in silicates is 1:1. The silicate is
supposed to provide stabilization by formation of a complex with
perhydroxyl ions which are released slowly at elevated
temperature. The silicate also provides a buffering action and its
solution is colloidal in nature.

The stabilizing action of silicates is improved by Ca or Mg ions


and hence water of hardness between 2-5° is recommended.

21 | P a g e
It is difficult to maintain the colloidal form of silicates in the
industrial processes, deposition of silicates on goods as well as
equipment interior walls takes place. The deposition produces a
harsh feel on the goods.

Deposition on the equipment surface makes it abrasive. A thorough


rinsing of goods can be helpful in removal of harshness on the
fabric.

Sequestering Agents

It has been shown earlier that in the presence of alkalis,


H2O2 undergoes heterolytic fission resulting in formation of
perhydroxyl ion. However, presence of transition metals or UV
light causes H2O2 to undergo homolytic fission to two hydroxyl
radicals (OH•). The metal actions can have a catalytic effect on the
decomposition of H2O2. The rate of decomposition may be so high
that cellulose is attacked and oxycellulose formed. The
oxycellulose thus formed results in poor mechanical properties. In
extreme case, holes may form on the substrate due to severe
localized action.

To minimize the harmful effects of metal cations, sequestering


agents are often used. These are compounds which sequester the
metal cations, rendering them harmless. Some examples are:

Poly phophonates

Poly hydroxyl carboxylic acids

Amino poly carboxylic acids

22 | P a g e
Phosphonic acids

Poly acrylic acids

The most common sequestering agents are di-ethylene tri-amine


penta acetic acid (DTPA) and ethylene di-amine tetra acetic acid
(EDTA) as sodium or magnesium salts.

DTPA (Di-Ethylene Tri-Amine Penta


Acetic Acid)

23 | P a g e
EDTA (Ethylene Di-Amine Tetra
Acetic Acid)

The sequestering agents prevent the metal ions from catalytically


decomposing peroxide solutions by chelating them. The complexes
formed may be complicated 3 dimensional structures involving
water of salvation molecules. Generally these metal ions are held
by five membered rings and one sequestering agent molecule may
interact with one metal ion. A simplified representation of 3-D
structure of the complex is shown below:

24 | P a g e
Figure 5 A simplified
representation of EDTA-metal
complex

Effect of Process parameters:

Effect of pH:

25 | P a g e
In acidic pH, H2O2 is stable, hence very little bleaching takes place.
Since NaOH is a strong alkali, it is difficult to plot variation of
bleaching efficiency as a function of time. However, concentration
of alkali does have an effect on whiteness which is shown in the
figure below.

Figure 6 Change in reflectance of bleached


cotton fabric with increasing NaOH
concentration in bleach bath

Effect of temperature:

26 | P a g e
In practice, the bleaching of cotton is carried out at or around boil
(90-100 °C). However, rapid bleaching is possible in pressurized
equipment at 120 °C. Bleaching at low temperature (~80 °C) will
result in concomitant increase in process time.

Advantages of Peroxide bleaching

It is a universal bleaching agent. It can be used for bleaching of


natural, synthetic and blended fibres.

It is possible to combine scouring and bleaching.

No antichlor treatment is required.

It is noncorrosive and does not produce unpleasant odour.

No AOX problem, no harmful by-products.

Residual size and wax removal continuous through bleaching;


results in improved absorbing and TEGEWA rating.

Disadvantages

Use of silicates as stabilizers has a risk of silica stain formation on


goods and silica deposits forming on plant machinery

Catalytic damage to cotton can occur in presence of transition


metal cations.

Not very effective for synthetic fibres.

Assessment of bleaching efficiency

Since the main objective of bleaching is to transform textile goods

27 | P a g e
into high, uniform whiteness, the most important assessment of
textile goods is assessment of whiteness. This is done by:

1. Comparing the sample against a standard which can be


magnesium oxide or barium sulphate. The standard has 100%
reflectance at all wavelengths. For bleached samples the
reflectance at 460 nm (blue region) is measured. Unbleached
cotton shows a reflectance of 55% which increases to 83-85% on
bleaching.

Other whiteness calibrations take into account the reflectance at


short as well as long wavelengths (for blueness and redness
respectively).

W(Harisson)= 100-(R670–R430)

and W(Stephensen)= R430 (R670- R430)

The term R430 refers to the yellowness which reduces whiteness.

2. Calorimetric method

One of the most popular whiteness indices is Hunter lab Whiteness


index (W Hunter). This system uses the Hunter L, a, b values for
evaluation of whiteness index which is given by

W= L-3b

This formula gave importance to blueness/yellowness but


neglected redness/greenness. Good bleached fabric should have a
WI > 75.

However, in case of Stansby, importance was given to all three

28 | P a g e
parameters. Thus

W(Stansby)= L-3b+3a

In Europe, Burger Index once used most widely is

W(Burger)= 0.333Y+1.060Z-1.277X

5. Mercerization
1844 - John mercer observed the effect.

1850 – Filed a patent for treatment of cotton with concen. NaOH


solution with improvement in strength & dyeability.

1890 – Horace Lowe; found if shrinkage is controlled, the fabric


becomes lustrous.

Tension Mercerization (Lowe) & Slack Mercerization (Mercer)

Mercerization is carried out for the following purpose.

Improving lustre (silky look, in tension mercerization only).

Improving tensile strength.

Improved dimensional stability.

Increasing uniformity of dyeing & improving color yield (savings


in dyestuff).

29 | P a g e
Improving Elasticity or Stretch material (in slack mercerization
only).

Mercerization is a process of impregnating the textile material


with a concentrated solution of cold NaOH, keeping it in contact
with this cold solution for a given time with or without tension,
and subsequently rinsing it.

MECHANISM-

Mercerization causes swelling in fibre

Swelling causes Cross-section to become rounder, loss of


convolutions & detwisting leading to more lustrous surface

Opening of fibre structure

Increase in amorphous content due to decrystallization

Although mercerization is accompanied by swelling, it is more


closely related to internal modification of fiber.

Effect is observed at 18-24 % w/w NaOH solutions.

Higher no of –OH groups available as compared to un-


mercerized cotton

Higher moisture regain, dye-uptake and reactivity

The effect of mercerization is related to the size of the sodium


hydroxide hydrates (NaOH. xH2O). The concentration of NaOH
30 | P a g e
solution determines the value of x or the size of the hydrate. A
dilute solution has larger sized hydrates, which can cause swelling
in cotton fibre by entering the amorphous phase of the fibre. At
higher concentrations, the hydrate volume is smaller. Such
hydrates cause lower swelling but have the ability to penetrate the
crystalline phase and change the crystal structure. Such changes
are capable of inducing important structural modifications in fibre
structure.

In the table given below, the composition of NaOH hydrate,


corresponding NaOH concentration and the type of hydrate
formation are shown:

Sodium Hydroxide Hydrates: Composition, Type and


Concentration of Maximum Frequency

NaOH
Composition of
Conc. (% Type of hydrate
hydrate
by Wt.)

NaOH.20H2O 6-9 Hydrated ion pair

NaOH.12H2O 13.5-15 Hydrated ion pair

Solvated dipole
NaOH.10H2O 18
hydrate

NaOH.H2O 69 Dipole hydrate

NaOH.7H2O 22.8-24.1 Solvated Dipole


hydrate + D.H. (7.4

31 | P a g e
A°)

NaOH.5H2O 30.2-30.9 Dipole hydrate

NaOH.4H2O 34.8-35 Dipole hydrate

NaOH.3.5H2O 38-38.8 Dipole hydrate

Dipole hydrate (Dia 6


NaOH.3.1H2O 41.8-42.6
A°)

NaOH.2H2O 52.6 Dipole hydrate

In the table given below, the variation in the hydrodynamic


volume with changing hydrate type is given.

Composition of Hydrodynamic
hydrate volume (dia Å)

Dipole Hydrate 5-8

Solvated dipole
8-10
hydrate

Hydrated ion pair 10-15

Separated Hydrated
15-20
ion pair

When a sodium hydroxide solution of a given concentration is


used for treatment of a cellulosic fabric (cotton), it forms a ternary

32 | P a g e
complex, the composition of which is governed by the
concentration of NaOH solution. This complex is known as soda
cellulose. These soda celluloses have well defined crystalline
character which is verified from their x-ray diffraction patterns.

Given below is the phase diagram of soda celluloses.

Phase diagram of soda


celluloses

In the figure given above, it can be seen that soda celluloses of

33 | P a g e
defined x-ray diffraction pattern are formed on treatment with
NaOH solutions of different concentrations at different
temperatures. Although it seems that there are well defined
boundaries for formation of various soda celluloses, in reality it is
not the case.

Na-Cell I forms when cotton or ramie is treated with 12-19%


(w/w) NaOH solutions at 20°C. Decomposition of Na-Cell I leads
to cellulose II formation. At higher concentrations, Na-Cell II is
formed. Drying of Na-Cell I results in formation of Na-Cell III.

Washing of Na-Cell I and II results in formation of Na-Cell IV. In


fact, Na-Cell IV is only a cellulose hydrate as washing removes
the alkali and decomposes the ternary complex. In a way it is a
swollen form of cellulose.

At low temperatures, Na-Cell V is formed. During washing of Na-


Cell V, Na-Cell IV is formed first and then Cellulose II is formed.

In the table given below, composition of Na-Celluloses and


corresponding hydrates is given.

Soda Celluloses: Composition and corresponding sodium


Hydroxide hydrates

Soda celulose Corresponding


Comoposition
type hydrate

34 | P a g e
C6H10O5 , NaOH, 3H2O
NaOH. 5H2O

NaOH. 7H2O
Na-Cell I
NaOH. 10H2O
(C6H10O5)2 , NaOH. 2H2O
NaOH. 12H2O
(C6H10O5)2 , NaOH. 1.5H2O

Na-Cell II C6H10O5 , NaOH. H2O NaOH. 3-3.5H2O

NaOH. 2H2O

Na-Cell III C6H10O5 , NaOH. 2H2O NaOH. 4H2O

C6H10O5 , H2O

C6H10O5 , 0-0.3NaOH. H2O


Na-Cell IV (Q) NaOH. 20H2O

C6H10O5 , 1.3 or 1.5NaOH. NaOH. 12H2O


2H2O

C6H10O5 , NaOH. 4-5H2O NaOH. 5H2O


Na-Cell V
NaOH. 7H2O

What are Cellulose I and Cellulose II?

The native form of cellulose which occurs in cotton and other

35 | P a g e
natural cellulosic fibres, is known as cellulose I. It has it unique
crystal diffraction pattern (monoclinic). It is a thermodynamically
less stable form of cellulose. When cellulose in converted to
regenerated cellulosic fibres like viscose, dissolution of cellulose
is an intermediate step. During regeneration, it gets converted to a
different crystalline form, known as Cellulose II.

During mercerization also, some native cellulose gets converted to


cellulose II. The extent of this conversion depends on process
conditions like temperature, tension, NaOH concentration etc.

In the table given below, the dimensions of unit cell of cellulose I


and II are given:

Crystal Dimension a Dimension b Dimension


Β (degrees)
form (Å) (Å ) c (Å )

Cellulose I 8.35 10.30 7.9 84

Cellulose II 8.14 10.3 9.14 62

The figure below arrangement of cellulosic chains in crystalline


register in cellulose I and II respectively. It is easy to see that the
formation of intra and inter chain hydrogen bond formation in the
two crystalline forms.

36 | P a g e
Swelling of cellulose fibres in Alkali solutions

It must be clear that mercerization involves disruption of


crystalline part of cellulose. For this to happen, alkali solutions of
sufficiently high concentrations which can form alkali hydrates of
such sizes which can enter the crystalline phase must be
employed. Swelling occurs during mercerization but it is not the
sufficient condition for mercerization to take place.

This will be clear from the figure shown below which shows
swelling of cotton fibres with different alkali concentrations at
different temperatures.

Cellulose--model films and the fundamental approach. Eero

37 | P a g e
Kontturi,  Tekla Tammelin,  Monika Osterberg

Chemical Society Reviews , 35(12):1287-304: 2007;

Swelling of cotton fibres at


different alkali concentration and
temperature

In the figure, the first sharp peak due to swelling appears at around
10% NaOH concentration. This could be very high at low
temperatures. In fact, if viscose was to be treated with 10% NaOH

38 | P a g e
solution at 0 °C, it will dissolve!

The swelling occurring at this concentration is solely due to


amorphous swelling and does not result in any of the effects
associated with mercerization. It is temporary in nature, but can
cause large shrinkage due to high degree of swelling involved.

At higher concentrations, the swelling goes down and increases


again at around 30% concentration. This swelling is caused by
disruption of crystalline phase of cellulose. Generally the
mercerization is carried out at 18-24% NaOH concentration and
the swelling caused is much less than that occurring at 9-10%
NaOH concentration. Hence it can be concluded that swelling is
necessary but not the sufficient condition for mercerization to
occur.

The effect of mercerization on various physical and other


properties of cotton is discussed in following sections.

Structural Modification

Effect of NaOH Concentration

It has been discussed that mercerization leads to conversion of


cellulose I to cellulose II. Native cellulose is Cellulose I and
regenerated cellulose (example – viscose) is cellulose II. However,
during mercerization, conversion of cellulose I to cellulose II is
only partial. Hence mercerized cotton is a combination of both
crystalline forms. The extent of conversion is dependent on
various process parameters like concentration of NaOH, time of

39 | P a g e
treatment, temperature and tension employed in the process.

In the figure given below, the effect of NaOH concentration on


crystallinity of cotton is given (time 60 sec, temp 20 °C, tension-
to maintain length change=0%)

Effect of alkali concentration of


crystallinity of cotton

From the figure it can be inferred that the formation of cellulose II


is favoured at higher alkali concentrations. The overall

40 | P a g e
crystallinity of cotton also goes down slightly on mercerization.

Effect of temperature

Temperature seems to have a similar effect on conversion of


cellulose I to cellulose II. Overall crystallinity also goes down.
This is shown in the figure below:

Effect of temperature on crystallinity of cotton


(time 60 sec, temp 20 °C, tension- to maintain
length change=0%)

Enhancement in lustre

41 | P a g e
Cotton owes its non lustrous appearance to its non uniform
twisted, convoluted, bean shaped fire cross section. As there is
continuous change in the fibre cross section along its length, it has
poor specular reflection which is responsible for high lustre. On
mercerization, the fibre swells gradually and the false twist and the
convolutions gradually disappear. The cross section becomes
almost circular and the fibre acquires the shape of a regular
uniform cylinder. This process of gradual change in the fibre cross
section is depicted in figure below:

Gradual change in cross section of cotton


fibre on mercerization

In the above figure, stage 1-5 show swelling of cross section of


fibre. It is easy to see conversion of a bean shaped flat cross
section to almost round shape and gradual disappearance of lumen.
Stage 6 and 7 are associated with removal of NaOH from fibre on
washing and drying. It is important to note that on loss of sodium
hydroxide during washing and subsequent drying, the fibre shrinks
in cross sectional area, but maintains its rounder shape. Overall,
there is very little gain in fibre volume due to mercerization, and
hence the density of the fibre remains unaffected.

The rounder, more uniform (convolution-less) and regular cross

42 | P a g e
section results in more specular reflection which results in higher
lustre. However, it must be noted that the process of removal of
convolutions and other surface irregularities (wrinkles and
creases) is greatly aided by tension. Hence tension mercerization
always results in more lustrous product as compared to a slack
mercerized one.

The presence of protruding fibre ends on the yarn surface


suppresses lustre. Hence cotton yarns meant to provide high lustre
must also be singed in order to maximize lustre.

Mechanical properties

Mercerization has been found to increase the tensile strength of


cotton fibres even though a drop in overall crystallinity is
recorded. The main reason for this phenomenon to occur is
swelling of fibres. The presence of many convolutions and false
twists in the fibres cause weak spots to be present. These weak
spots act as zones of stress concentrations due to lower cross
sectional area on application of a tensile stress. Swelling, which is
an integral part of mercerization process, removes convolutions
and false twists and the fibres acquire a more uniform cross
section along its length. With weak spots gone, the fibres exhibit
enhanced tensile strength as compared to a non-mercerized fibre.

Increase in tensile strength can be summarized as:

Removal of convolutions results in removal of weak spots at the


point of reversal

Fibres have more uniform, circular and smoother cross section

43 | P a g e
after mercerization

The fibrills are arranged parallel along the fibre axis

Fibre alignment along fibre axis is better in case of tension


mercerization as compared to slack mercerization

Effect of tension

Mercerization has a significant effect on mechanical properties of


cotton. In the figure given below, tenacity, breaking elongation
and Young’s modulus of cotton mercerized with 300 gpl NaOH
solution at 20 °C for 60 sec are plotted. The tension is varied to
allow 10% shrinkage to 4% stretch. The elongation and modulus
are indicated on secondary vertical axis. It is clear that the
enhancement in both tenacity and modulus is higher at higher
tension. It is easy to visualize this since it results in better
alignment of molecular chains in fibre axis direction (higher
orientation). However, in case of elongation, it is reverse. With
increasing tension, the elongation at break decreases
monotonically. It is to be expected as increasing orientation would
lead to lower elongation. At negative tension though (shrinkage
occurring) the breaking elongation is higher than that of
unmercerized cotton.

Hence it can be concluded that if improving the tenacity of cotton


yarn is the main objective, mercerization should be carried out
under tension.

Effect of Alkali concentration

44 | P a g e
The effect of alkali concentration on tenacity, breaking elongation
and Young’s modulus of cotton mercerized with NaOH solution of
variable concentration at 20 °C for 60 sec at constant length are
plotted in the figure given below. The alkali concentration is
varied from 100 to 300 gpl. Again, the elongation and modulus are
indicated on secondary vertical axis.

Effect of Tension on Mechanical Properties


of Cotton Yarn during Mercerization

45 | P a g e
Effect of NaOH conc. on Mechanical
Properties of Cotton Yarn Mercerized at
Constant Length

Dyeing Properties

Since mercerization results in change in physical structure of


cotton, as manifest in change in crystal structure, crystallinity and
lustre, it affects the dyeing behavior of cotton. The important
changes that cause this are:

Mercerization decreases the crystallinity (increases amorphous

46 | P a g e
content)

Modifies the texture

Overall effect – greater moisture absorption, greater reactivity


towards chemical reagents and dye molecules

Mercerized cotton has higher

Dye absorption ( dye pickup)

Rate of dyeing

Visual colour yield as compared to unmercerized cotton

Improvement is more marked in slack mercerization (lower


tension)

Increase in colour yield can allow for a saving of 15-50% in


dyestuffs. Indeed many times, this is the reason for subjecting
cotton goods to mercerization.

Interesting - mercerized cotton appears darker than unmercerized


cotton even when the dye absorption is same.

The effect of mercerization on dye absorption and apparent color


yield is shown in the figure below. The concentration of sodium
hydroxide is varied from 150 to 350 gpl.

47 | P a g e
Effect of Mercerization on Dyeing
Properties of Cotton Yarn at constant length
(dye- CI Direct blue 1)

The increased Visual color yield (darker shade) of mercerized


cotton is due to increased dye absorption as well as the optical
effect.

Kubelka Munk Equation

Defines the colour yield in terms of reflectance of dyed material

48 | P a g e
K – Light absorption factor, S – light scattering factor, C is
concentration and a is a constant

R - reflectance

K changes linearly with concentration (within some limits)

Upon mercerization

S decreases (less internal scattering from a rounder x-section)

Non uniformity of the operation causes increase in colour yield


(apparent)

Non-uniformity of the mercerization results in peripheral fibres


absorbing most of the dye. This may cause the cotton goods to
appear darker in shade.

If improving the dyeability is the only aim then 150-190 gpl


NaOH treatment is ideal.

In general, the increased dye absorption and the optical effect may
contribute roughly equally towards increased Visual colour yield
after mercerization.

Wetting agents for mercerization:

Mercerisation liquor of concentrated NaOH solutions is generally


applied at low temperatures (15-20 °C). Under these conditions,

49 | P a g e
liquors possess high viscosity and swelling of fibers is high and
rapid. This results in poor and non uniform penetration of cotton
textiles by NaOH solutions.

Sometimes goods are mercerized in greige or non-scoured state.


The presence of sizes or cotton waxes further hinders penetration
of NaOH in the cotton yarns/fabric. Therefore the use of wetting
agents to increase the wetting of goods by mercerizing liquor is
resorted to, which results in faster and more uniform treatment of
cotton goods.

Since the liquor is highly alkaline, the prospective wetting agent


must be:

Soluble and stable in alkali solutions of mercerizing strength

Should be efficient (effective at low concentration)

Should have low affinity to fiber

Should be low foaming

Normal wetting agents are not sufficiently soluble in moderately


concentrated caustic soda solution. Products based on cresylic acid
(a mixture of o-, m- and p-cresols) were used sometime back.
However these are toxic and non-biodegradable in nature and its
use in mercerization in on wane. Addition of solvent additives
such as alcohols (e.g. cyclohexanol), ethers, ketones, lower fatty
acid amides increases wetting power of mercerizing liquor.

The biodegradable wetting agents

50 | P a g e
Certain alkylarylsulphonates

some organophosphonates (e.g. sodium methyloctylphosphonate)

alkylated diphenyloxide sulphates (e.g. dodecyldiphenyloxide


sulphate)

especially sulphated aliphatic alcohols (e.g. 2-ethylhexyl


sulphate). most effective have chains with 4-8 carbons

Example: sulphated 2-ethylhexanol, activated with about 10%


butanol and unsulphated 2-ethylhexanol.

Hot mercerization

Although mercerization is an exothermic process and is more


efficient at lower temperatures (typically a temperature range of 15
to 20 °C is used), it has following drawbacks:

At lower temperatures, NaOH solution of mercerizing strength has


high viscosity and surface tension

When a yarn/fabric is mercerized, swelling of fibres at yarn surface


due to mercerization causes compaction of yarn structure

This results in poor penetration of NaOH solution in the core of


yarn

The treatment becomes non-uniform

The basic problem of poor penetration leading to non uniform

51 | P a g e
mercerization can be tackled by carrying out mercerization with
hot (60 to 100 °C) NaOH solution of mercerizing strength. This is
known as hot mercerization.

However, since mercerization won’t take place at high


temperature, the temperature of the treated fabric has to be brought
down.

Therefore, hot mercerization becomes a two stage process, in


which the first stage is treatment of cotton fabric with hot NaOH
solution of mercerization strength and the second stage is the
reduction in temperature of the treated fabric to bring about the
mercerization.

As the temperature of the fabric is brought down, swelling may


start and the fabric may shrink and hence the dimensions may need
to be maintained during cooling stage by desired applied tension.

Advantages:

Hot NaOH solution has low viscosity and higher penetration


power

Swelling of cotton fibres in hot NaOH solution is low, hence more


uniform treatment

Faster process, leading to: higher productivity and compact unit

Period of contact between material and NaOH can be reduced by


upto 50%

52 | P a g e
The fabric can be stretched to greater degree as the fabric
becomes more plastic

More uniform coloration

Better dye uptake (less colour yield)

Can permit elimination of scouring process

However, under conditions prevailing in hot mercerization,


degradation of cellulose at high temperatures in presence of air can
take place.

The sequence

Saturation of cotton with NaOH under relaxed conditions (50 oC


to boiling point) for 4-20 seconds

Controlled hot stretching

Cooling the stretched material to less than 25 °C temperature

Tension controlled washing (till NaOH concentration in fabric


falls below 60 gpl level)

Final washing under relaxed conditions

Since NaOH is also an agent for carrying out scouring of cotton


fibre, yarn/fabrics at high temperatures, hot mercerization can also
be suitably modified to carry out both mercerization and scouring

53 | P a g e
in one operation.

Sequence for combined mercerization and scouring

Hot saturation of fabric with alkali solution

Steaming of relaxed or stretched material for

10 min at atmospheric pressure

5 sec under pressure (130-140 °C)

Cooling and mercerization

Washing

There is another variation of hot mercerization. The sequence is as


follows:

Washing of fabric at 95 °C

Hot squeezing (high speed steam injection)

Impregnation in NaOH at 20 °C

Impregnation in NaOH at 30 °C

Stabilization under tension

54 | P a g e
Washing

The advantages of this variant are:

More uniform treatment faster process, hence process time can be


reduced

More productivity or more compact unit

Higher stretching is possible; this will result in higher mechanical


strength/lustre

Higher stretch is possible if stretching proceeds while cooling

Uniform dyeability

Dyeuptake is better but colour yield is lower

Mercerization of blends

Sometimes blends of cotton and viscose need to be mercerized to


bring dyeuptake and lustre of cotton at par with that of viscose

Problems faced in mercerization of cotton/viscose blends

Solubility of viscose in alkaline solutions causes weight and


strength loss

Dissolution occurs at 80-130 gpl concentration of NaOH

(Viscose becomes highly swollen)

This problem can be solved by using a modifying sequence of


55 | P a g e
mercerization as described below:

Hot impregnation (saturation with hot mercerization liquor to


minimize swelling of viscose)

Addition of electrolyte in the mercerizing liquor

Use of KOH or admixture of NaOH and KOH (KOH induces less


swelling)

HOT water rinse (at 90 °C); viscose solubility is less at higher


temperature

Addition of electrolyte (NaCl) in rinsing bath (electrolyte


suppresses swelling of viscose)

Machines for Mercerization:

Fabric Mercerization with Tension

1. Stenter type or chain mercerizing machine

2. Chainless mercerizing machine

3. Chainless and pad less mercerizing machine

56 | P a g e
Hank Mercerizing Machine

Yarn mercerization

Yarns are mostly mercerized in hank form. Yarn mercerizing


machines generally consist of two rollers, on which the hank can
be mounted. A device can be used to apply tension (to stretch) on
the hanks. After the hanks are mounted, the rollers can be lowered
into a tray which consists of caustic soda solutions of mercerizing
strength. The hanks are allowed to saturate with alkali, the tension
is generally applied later. After sufficient time is allowed for
mercerization (1-2 min) the hanks are squeezed and rinsed. The
tension is released once the residual alkali concentration drops
below 60 gpl. For optimum gain in tensile strength and lusture, a
tension causing stretch of 0.5-3% is applied, higher tension results

57 | P a g e
in lower tensile strength.

Fabric mercerizing machines:

Fabric mercerizing machines are generally continuous operation


machines with the ability to apply controlled lengthwise tension.
There are mainly two types of machines:

Those equipped with a chain to apply a controlled width wise


tension (Pad chain mercerizing machine)

Chainless machines, which apply the width wise tension by means


of expander bars or bowed roller (Chainless mercerizing machine)

Pad chain mercerizing machine

In these machines fabric is saturated with alkali solution and


padded. The saturated fabric passes over a set of rollers (airing
rollers) which allows the swelling or mercerisation to take place.
Fabric is again saturated and squeezed and passed into a stenter
where length and width wise tension is applied. Width wise tension
is applied using stenter clips on chain.

This is followed by sprinkling of fabric with water to remove


alkali. The tension is maintained till the alkali concentration drops
below 60 gpl. After this, fabric can be rinsed and neutralized in
open width washing machine (Tension may be relaxed).

The tension applied by means of clips in weft direction can be


higher which can impart higher lusture to the fabric. However the
tension in width wise direction can cause the fabric to expand in a
non uniform way, as shown in the figure below. Also there is a risk

58 | P a g e
of fabric getting torn near the edges where it is held by clips.

Chainless mercerizing machine tackle above problem by using


bowed rollers (figure below) to apply width wise tension. The clips
of chain mercerization machine are replaced by an expander unit
consisting of bowed rollers. The stretch or tension applied in weft
direction is determined by warp wise tension in the fabric which in
turn is controlled by oscillating rollers. Other features are more or
less similar to chain mercerization units.

Determination of degree of mercerization:

Although there are many methods to do this, one quantitative test


based on the ability of mercerized cotton to absorb barium
hydroxide is widely used. Mercerized cotton can absorb more
Barium hydroxide than un-mercerized cotton and this is the basis
for this test. The test method is described below:

Mercerized and un-mercerized cotton samples (2 gm each) are


treated with 30 ml of N/4 Barium hydroxide for two hours in
conical flasks at room temperature. Preferential absorption of
barium hydroxide by cotton samples reduces the strength of
Barium Hydroxide solutions. The amount of Ba(OH)2 absorbed can
be determined by taking 10 ml of Ba(OH)2 solution from each of
the flasks and titrating it with N/10 HCl, phenolphthalein being
used as an indicator. Fresh Ba(OH)2 is also titrated (blank titration)
to accurately assess the actual Ba(OH)2 in solution.

The Barium Activity Number is given as:

BAN = (B-M) / (B-C)*100

59 | P a g e
Where B = Volume of HCl (ml) required for blank titration

M = Volume of HCl (ml) required with mercerized cotton

C= Volume of HCl (ml) required with un-mercerized cotton

For completely mercerized cotton the value of BAN is around 155


and for semi mercerized cotton it varies in between 115 and 130.

6. Optical whitening agents


Most of the textile materials, especially the natural ones, appear
slightly yellowish of off white even after they have been bleached.
They are not bright white. The reason lies in slight absorbance by
these substrates in blue region of visible light which leaves these
materials appearing as slightly yellowish. This can be seen in the
following figure.

60 | P a g e
Across cultures, bright white has been regarded as signifying
purity and hence there have been efforts to achieve brighter
whites. Attempts have been made to tint white goods with blue
pigments since bluish whites are preferred over whites with
yellowish or greenish tinge.

To make whites brighter, one needs to increase the reflectance of


the bleached goods further. This is possible with certain additives
which absorb UV component of solar radiation and emit in visible
range (preferably in blue violet region). Thus, the overall
reflectance of the goods becomes higher than that of bleached

61 | P a g e
goods with a blue tinge to it, making it appear much brighter.

The first recorded evidence of OBA application happened in 1929


when Paul Krais applied aqueous extract of aesculetin-6-glucoside
(a naturally occurring OBA) on linen.

Aesculetin-6-glucoside

These agents have been known as Fluorescent Brightening Agents


(FBA) or Optical Whiteners (OBA). They are distinct from
blueing agents in that while blueing agents suppress overall
reflectance, the OBAs actually enhance it.

Mechanism of OBA action-

OBAs are designed to absorb light between 340 to 380 nm (UV


spectrum) & emit it in the range 425 to 450 nm (visible spectrum).

Effective OBAs must absorb strongly in UV region and emit a


large part of the absorb energy in the visible region. OBA
molecules have an extended conjugated bond system as it is
capable of strong fluoresce.

62 | P a g e
In the figure (colorants & auxiliaries-39 page no.-473) given
below, the ground and excited energy levels. (S 1,S2……) are
shown. So S1,S2…… represent singlet states with paired spins &
T1,T2……represents triplet states with unpaired spins.

The energy levels are further subdivided in to vibrational levels.

When an OBA is exposed to electromagnetic radiation, the


electrons are transported to one of the excited energy levels from
the ground level. The energy state and the vibrational level to
which it is transported depends on the amount of energy absorbed
(E=hν ) within an energy level

Absorption and fluorescence

63 | P a g e
processes

(S1,S2……). The electrons lose the energy very quickly (10 -12s) to
come down to the lowest vibrational level in existing energy level.
The return of the electron from the lowest vibrational level of an
excited energy state to one of the vibrational level in the ground
state (S0) is known as the fluorescence, and is accompanied by
release of energy in the form of EM radiation (emission)
corresponding to the frequency given by the relation

E = hν

Since the energy released by the electron during fluorescence is


always lower than the energy absorbed, the wavelength of emitted
radiation is always higher than that of absorbed radiation.

Hence, if absorption occurs in UV region, the emission may occur


in violet or blue region of visible spectrum. The difference
between the wave number of absorption and emission is known as
stokes shift. For maximum effectiveness, an OBA should absorb
around 370 nm and emit around 430 nm for a stokes’s shift of
around 60 nm. Depending on the nature of OBA, it can produce
violet, blue or green hued whiteness. This depends on the
wavelength/wave number in which the OBA is emitting. However
the hue of the OBA can also change with the concentration level.
With increasing concentration, the whiteness produced by an OBA
increases initially. However at higher concentration it starts
aggregating & a shift in fluorescence may be observed. A blue
tinged fluorescence may turn in to greenish hue which is
undesirable & rather than appearing white, the material may

64 | P a g e
appear coloured. This is shown in figure (page-479) below.

Typical absorption and emission


curves for an FBA

Chemistry of FBAs

Just like dyes, different OBAs are suitable for different fibre types.
Therefore, OBAs for cotton, wool & silk are anionic in nature, for
PET hydrophobic and for acrylic, cationic.

In general OBAs for cotton have poor light fastness (1-3) meaning

65 | P a g e
they need to be applied over and over again to maintain the
whiteness. For the same reason white paper turns yellowish
gradually due to destruction of OBA in it.

OBAs for cellulosic substrates

Brighters for cotton are anionic in nature and are applied in a way
similar to the application of direct dyes. A range of products
varying in substantivity from high to low is available. Low
substantivity OBAs are suitable for application by continuous
method while the high substantivity ones are applied by exhaust
method. OBAs can be applied during bleaching or in a separate
step after bleaching.

Since fading of OBAs on cellulosic substrates is faster due to poor


light fastness, they need to be fortified frequently. This is
generally done by formulating them in washing soaps and
detergents.

The most common OBAs for cellulosic fibres are based on triazine
derivatives of diaminostilbene disulphonic acid (DAST) with
following chemical structure.

66 | P a g e
Where M is alkali metal like Na or K, or ammonium cation

R1 is an aromatic amine residue/ its derivatives

R2 is generally aliphatic amine derivatives

e.g. N(CH2CH2OH)2 or -NH-CH2CH2OH

The following product (vic triazol)

Has a light fastness of 5 on cotton, which is very high for OBAs


on cotton. It is stable to chlorite & hypochlorite bleaching and can
be applied along with resin finish.

However, it is expensive.

Nylon –

OBA generally used for Nylon are anionic in nature like acid dyes.

67 | P a g e
These are generally applied from an acidic bath pH – (4-5).

The vic- triazole is shown above.

Polyester-

The OBAs for polyester are disperse type. They can be applied by
exhaust & pad-thermosol (continuous process) or by addition
directly in the melt (mass brightening) like in mass coloration.
Following OBAs are useful for polyester.

These can be applied by exhaust at 125-130 °C and by thermosol


operation at 160-220 °C.

68 | P a g e
Can be applied by thermosol process above 190 °C. The light
fastness of OBAs on PET is generally higher at 5-6.

Acrylic fibre -

OBAS for acrylic fibres are generally applied from acidic baths by
exhaustion around boil.

Derivative of 1,3-diphenylpyrozoline (figure below) can produce


very high whiteness of violet tinge, the OBA is unstable to chlorite
bleach and can produce LF of 4.

The following product is stable to chlorite and can be applied


during bleaching itself. It can also give a light fastness of around
4.

69 | P a g e
7. Combined pre-treatment processes

7.1 Introduction
As has been discussed so far, the pre-treatment processes are designed to
remove the specific type of impurity from a fibre. For example, the
specific processes to deal with removal of sizes, natural impurities and
colouring components are known as Desizing, scouring & bleaching
respectively. All these processes employ specific chemicals and process
conditions like temperature, pH, and time to optionally remove the specific
impurity. Most of the time these processes many not be compatible with
each other and hence have to be carried separately in specific sequence.

Now a day, industry has become increasingly aware about the optimal use
of resources like water, energy and on the other hand the fallout of
pollution caused by industrial textile processes. All these pre-treatment
processes consume large amount of water and energy. Combining any of
the two or all processes can result in huge savings in terms of water,
energy and reduced effluent load. In the subsequent sections, such

70 | P a g e
combined pre-treatment processes will be discussed.

Combined Desizing and scouring

Traditionally Desizing is carried out with acid or enzymes (starch based


sizes) which are carried out in acidic medium. This type of Desizing
cannot be combined with alkaline scouring where high pH is used. Now a
possibility of combining Desizing with scoring arises if Desizing can be
carried out in alkaline conditions. This is possible if oxidative Desizing is
carried out.

Following recipe can be used:

(Pad -steam)

Potassium per
- 3 gpl
sulphate

70
Sodium hydroxide -
gpl

Wetting agent - 1 gpl

Non ionic 10
-
detergent gpl

The fabric is padded and steam for 12 min. The fabric is washed in an
open soaper. The temperature in first compartment is at boil with gradually
reducing temperature in subsequent compartments.

Combined scouring and bleaching

The options available for cotton scouring are alkaline scouring with

71 | P a g e
sodium hydroxide, enzymatic scouring or solvent/emulsion scouring. The
approaches to combine scouring and bleaching are based on hydrogen per
oxide as it is carried out under alkaline conditions. Other per oxygen
compounds like potassium per sulphate (PPS) have been used in
H2O2 based single stage scouring and bleaching. An example is the
following recipe:

NaOH - 5%

H2O2 - 1

TEMP. - 70 °C

PPS - 0.5 %

Contavan GAL 0.4


-
(stabilizer) gpl

Time - 2 hrs

M:L ratio - 1:30

Attempts have also made to combine bio scouring with per acetic acid
bleaching. For example-

TAED - 2 gpl

0.15
Sodium per borate -
ml/l

Pectinase - 2 gpl

Egyptol (non ionic- 5 gpl

72 | P a g e
surfactant)

90
The treatment time -
min

Temperature - 60 °C

Washing is done with boiling water followed by cold water rinse and
drying.

Although this recipe can be used for one stage Desizing, scouring &
bleaching, best whiteness is obtained when the fabric is desized prior to
the treatment. It was also found that peracetic acid does not suppress the
activity of enzymes.

Combined Desizing, scouring and bleaching

The attempts to combine all three sequences are again based on alkaline
scoring and bleaching.

A process for combining all three preparatory processes (Desizing,


scouring & bleaching) was carried out by Gulrajani et.al.

They optimized a recipe which is given below:

Scouring agent - 4 %

Hydrogen per
- 1-2 %
oxide

Temperature - 95 °C

Time - 180 min

73 | P a g e
Sodium silicate - 2 %

0.1 % (sodium octyl


Wetting agent -
sulphosuccinate)

pH - 10.5 (soda ash)

The scouring agent has the following compositions:

Pine oil - 5 parts

Emulsifier - 4 parts

Perchloro
- 1 part
ethylene

The fabric is padded twice in to 80% pickup and stored in a J-box type
container.

After treatment, samples are washed with cold water and dried.

New concepts

In the last decades there have been some developments which have
focussed on the mechanical aspect of the process to improve the impurity
removal. These processes have developed systems which intensify the
interaction between the liquor and the fabric.

Some of these processes are:

Ben bleach concept

74 | P a g e
ROCO yet bleaching system

Kuster’s flexinip process

Dip sat vario process

Ben bleach system consists of four modules:

Ben-Injecta – for Desizing

Be –Impacta – Impregnation

Ben-Reacta – For steaming

Ben extracta – washing

Desizing is done in a separate module (Ben Injecta) for size removal.

In Ben bleach system, the steam at high temperature ( 100°C) is allowed to


impinge on the fabric in a narrow casing. Due to high turbulence caused in
the casing, penetration of the fabric by the steam is thorough. This ensures
intensive interaction between the steam and the size. This results in
dissolution of size material very quickly and efficiently without any
preswelling. It also reduces the size the desizing section. Ninety percent
removal of sizes, greases and waxes is claimed.

75 | P a g e
Steam passage
through the fabric
in a narrow casing,
Ben Injecta

In Ben Impacta, better and faster impregnation of fabric with controlled


liquor pick-up is ensured by having High liquor exchange through
turbulent flow.

In ben-Reacta, a combination steamer (fabric in tension in open width and


in plaited form) allow a steaming time from 1 to 60 min. Air-free
conditions and control of steam quality ensure constant conditions in
steamer.

76 | P a g e
In Ben-Extracta, energy and water are conserved using counter current
flow of wash liquor and liquor segregation. It is clear from
the figure below that space requirement is also lower.

Open width washer

77 | P a g e
without
intermediate
squeeze

8. Preparation of Protein Fibres

8.1 Carbonization
Objective: To remove cellulosic impurities from wool by treatment with
acid/acid producing salts.

Raw wool may also be contaminated with vegetable matter which may be
primarily cellulosic in nature, consisting of seeds, burrs, grass etc. The
wools destined to be processed by worsted route may have substantial
amount of vegetable matter removed during carding , gilling and combing.
However wools with high content of vegetable matter may need to be
treated chemically for its removal in the loose stock stage itself.

The most commonly employed method for removal of vegetable matter


from wool is treatment with mineral acids, especially sulphuric acid. The
treatment is based on the premise that the stability of wool to hot mineral
acids is higher than that of cellulose. The treatment with mineral acids
turns the cellulose into brittle carbonaceous mass which can be removed
by crushing it into a powder.

Sequences-

78 | P a g e
Acidification → Drying/Baking → 
rushing → Dusting → Neutralization

Processing Stages:

Treatment with (5-7% w/v) sulphuric acid & acid stable wetting agent.

Hydro extraction

Drying at 60-70 °C to low regain

Baking at 110 °C in dry heat for 2 min. (wool is relatively stable to acidic
conditions. The vegetable matter turns brown/black, becomes brittle)

Crushing to break the degraded vegetable matter to small fragments by


passing through heavy fluted rollers

Dusted & Neutralized with sodium bicarbonate.

Bleaching with acidic hydrogen peroxide to minimize yellowing caused by


carbonization

8.2 Wool Scouring


The type and level of impurities in wool fibres were discussed in chapter 1.
The amount of impurities especially the wool grease may be so high that it
may hinder the processing of wool. The transfer of wool grease from fibres

79 | P a g e
to metallic machine parts may lead to

Dirt/oil accumulation on processing equipment

Poor drafting performance

Therefore, wool is generally scoured at fibre stage. Due to the presence of


scales on wool fibre surface, it has a tendency to felt/shrink. Scouring
involves treatment with aqueous scouring liquors containing mainly
surfactants. Efficacy of scouring can be increased by mechanical agitation
or stirring action. However this may also lead to fibre entanglement.

Hence the scouring process design should address:

Effective contaminant removal from wool fibres

Minimal fibre entanglement

WOOL SCOURING- salient features

Generally done at raw wool stage.

Residual grease/wax is kept around 0.5-0.75%.

Modern machines used – Hopper bottomed


bowls.

Older machines – Long bowls with flat bottoms.

Older machines – 4-5 long bowls (35-40 m.)

Modern machines – At least six bowls (16-28

80 | P a g e
m.)

Wool scoring may be carried out in a series of bowls where the wool fibre
mass is transported from one bowl to another with gentle stirring. Non
ionic surfactants are primarily used for contaminant removal. Sodium
carbonate may be used as builder sometimes to facilitate contaminant
removal when immersion time is short. As wool gets cleaned
progressively, the composition of treatment bowls keeps changing.

The most important auxiliary used for wool scouring is a detergent. Alkyl
phenol ethoxylates have been used as highly effective detergents but are
being phased out due to environmental concerns. Due to the Eco-friendly
nature, fatty alcohol ethoxylates are nowadays being preferred over Alkyl
phenol ethoxylates. Typical composition of auxiliaries in a wool scouring
machine may be as tabulated below:

Typical recipe

Alkali Temperature
Soap (%) Time (Min)
(Na2CO3 %) ( °C)

I BOWL 0.75 0.20 49-52 2.5-3

II BOWL 0.5 0.1 46-49 2-2.5

III
0.25 0.1 43-46 2
BOWL

IV Water
- 40-43 1.5
BOWL only

pH should never be above 10.


81 | P a g e
Temp. – 35 – 40 °C but never above 60 °C.

8. Preparation of Protein Fibres

8.4 Wool Bleaching


Wool bleaching is generally carried out by oxidation, reduction or
combined oxidation/reduction process.

Oxidative bleaching-

Wool is invariably bleached with hydrogen peroxide. The chlorine based


oxidative bleaching agents are not suitable for wool.

General bleaching sequence is: pH -8.5-9 at 50-60°C for two hours.

The alkali used for activating should be mild. The stabilizers used are
phosphates, tetra sodium pyrophosphate or sodium tri polyphosphate.
Since wool can be damaged under alkaline condition, an alternative is to
bleach in acidic conditions using a per acid activator.

This is a BASF promoted process, bleaching is done at pH 5 with activator


prestogen W at 80°C for an hour.

Hydrogen peroxide and peroxy compounds can cause progressive


oxidation of disulphide bonds in wool, leading to fibre damage which can
be accentuated in subsequent dyeing. Hence prebleached wool should be
dyed preferably below 80°C.

Another variant of acidic bleaching was developed by IWS & BASF. In


this process, wool is padded with 350 gpl H2O2 solution acidified by 2 gpl
formic acid. By batching (cold-pad-batch) overnight, excellent bleaching is

82 | P a g e
obtained.

Reductive bleaching

Reductive bleaching of wool is carried out with following agents.

Thiourea dioxide

Sodium dithionite

Zinc formaldehyde sulphoxylate

Sodium formaldehyde sulphoxylate

Sodium dithionite is the preferred reducing agent. Bleaching is carried out


at 45-65°C at pH- 5.5-6 for 1 hour.

Bleaching can also be carried out with thiourea dioxide. It is a safer


alternative to other reductive bleaches.

To prevent heavy metal catalyzed decomposition of bleach bath, inclusion


of a sequestering agent is a must. The bleaching is carried out at pH 7 at
80°C for an hour. Bleaching species is thiourea dioxide.

Combined oxidative reductive bleaching –

Peroxide bleached wool has a reddish tone whereas reductively bleached


wool often has a greenish tinge but a natural white is generally the demand
of the industry. A sequential oxidative and reductive bleaching process is
supposed to peroxide a neutral white colour.

Bleaching with thio urea oxide is 3 times cheaper in cost and also has the

83 | P a g e
advantage of low COD & BOD.

In this approach wool is first bleached with alkaline H 2O2 at 60°C for 1
hour. To the bath thiourea is added and pH adjusted to 4.5-5.5. Thiourea is
converted to thiourea dioxide and bleaching is carried out at 60°C for
another 25 min, followed by washing and rinsing.

Thus in the first stage oxidative bleaching occurs with H 2O2 and reductive
bleaching takes place in the 2nd stage with thiourea dioxide.

8.5 Silk degumming


The main objective of silk degumming process is to impart soft handle and
lustre to silk by removing sericin, any impurities picked up during reeling
throwing etc. Some natural wax, coloring matter and minerals may also be
removed during degumming.

Since sericin forms bulk of the gum or the outer protective coat in a silk
filament, which also happens to be a protein, the process mainly consists
of cleavage of peptide bonds of sericin, either by hydrolytic or other
methods, and its subsequent removal from fibroin by solubilization or
dispersion in water .

Following are the main Degumming Processes:

a) Extraction with water.

b) Boil-off in soap.

84 | P a g e
c) Degumming with alkalies.

d) Degumming with acids.

e) Degumming with enzymes.

f) Degumming with organic amines.

Although both fibroin and sericin are proteins, they differ significantly in
their constitution. Given below is the typical amino acid composition of
fibroin and sericin:

Amino Sericin Fraction (mol %) Whole


Fibroin
acid I II III IV sericin

Gly 13.21 12.81 15.69 11.89 13.49 43.7

ALa 4.68 6.69 6.68 9.30 5.97 28.8

Val 2.97 2.21 3.21 4.16 2.75 2.2

Leu 0.86 0.96 1.27 6.26 1.14 0.51

ile 0.59 0.57 0.85 3.50 0.72 0.71

Pro 0.58 0.63 0.66 2.75 0.68 0.31

Phe 0.45 0.44 0.50 2.83 0.53 0.61

85 | P a g e
Try 0.19 0.20 0.25 0.23 0.21

Cy 0.17 0.15 0.12 0 0.15

Met 0.04 0.04 0.04 0.12 0.04

Ser 34.03 36.64 28.15 12.40 33.43 11.9

Thr 10.34 8.48 11.36 7.25 9.74 0.9

Tyr 2.53 2.43 3.15 2.45 2.61 5.1

Asp 16.94 16.95 16.13 12.64 16.71 1.3

Glu 4.73 3.64 4.09 11.32 4.42 1.0

Arg 3.20 2.65 3.68 3.93 3.10 0.46

His 1.25 1.22 1.49 1.87 1.30 0.16

Lys 3.28 3.29 2.64 7.11 3.30 0.31

It is clear from the above table that the main constituents of fibroin
are glycine, alanine and serine whereas in sericin it is serine, aspartic acid
and glycine . Hence any degumming method should target the peptide
bonds between the amino acids found in majority in sericin. However, in
practice, methods have been developed on empirical basis.

Extraction with water

Sericin removal can be achieved in water at high temperatures. It is not a


commercial process. Upto 96% sericin can be removed by extracting it

86 | P a g e
with water at 115 oC for 3 hours. Although there is still a doubt if the
removal occurs through hydrolysis or dissolution.

Boil-off in soap

It is an old process and seems to be still favored commercially. Olive oil


soap ( Marseille soap) is the most widely used soap. Following is a typical
recipe:

20-30 %
Marseille soap
owf

90-120
Time
min

Temperature 90-100 °C

M:L 1:40

Since large amounts of soap are used, this method works out to be
expensive. There have been attempts to first carry out partial degumming
with a spent or exhausted soap bath and complete the degumming in a
fresh bath. Alternately, addition of a small amount of alkali may result in
saving of both time and cost. Addition of upto 0.18% of free alkali does
not result in weakening of silk. However, excessive alkali in degumming
liquor may result in loss of strength, lustre and elasticity of silk.

The amount of sericin removal also depends on the type of soap used in
the degumming process. It is postulated that the degumming depends on
the alkali formed on hydrolysis of soap and the soaps hydrolyzing the most
have the highest degumming power. In the table given below, this

87 | P a g e
correlation is apparent.

Degree of
Kind of Degumming
hydrolysi
soap loss (%)
s (%)

Tallow 51.8 18.38

Olive oil 60.0 18.60

Coconut
28.8 16.77
oil

Caster oil 16.5 13.42

Arachis oil 55.0 18.23

Soya bean
60.0 18.71
oil

Cotton
61.0 18.24
seed oil

Chrysalis
53.0 18.03
oil

Sodium
0.75 3.09
caprylate

Sodium
1.25 7.15
laurate

88 | P a g e
Sodium
14.25 7.51
myristate

Sodium
38.0
palmitate

Sodium
59.75 19.44
stearate

Sodium
2.50 20.30
arachidate

Sodium
42.40 19.30
oleate

Sodium
10.30 12.10
ricinoleate

Degumming with Alkali Buffer

Though use of alkalis for degumming works out to be economical as


compared to soap degumming in terms of chemicals and labour cost,
improved productivity etc., it can leave silk yellowish and harsh. Hence
alkalis are not recommended to be used alone. With alkalis, the pH of the
boiling bath should be maintained between 9.5-10.5. Below pH 9.5, the
rate of degumming is too slow and above 10.5, the risk of chemical
damage is high. Hence many times, alkaline buffers like sodium
carbonate/sodium bicarbonate, sodium hydrogen phosphate/trisodium
phosphate and potassium tetraborate/boric acid have been used. Sodium
carbonate/sodium bicarbonate is the most widely used buffer. In addition
to the buffer, rate of degumming also depends on concentration of

89 | P a g e
electrolytes in degumming bath. The rate increases with increasing alkali
concentration. At a pH of 10 and temperature of 95 oC, the degumming
takes 60 min with 0.01 molar Sodium carbonate/sodium bicarbonate
concentration but at same pH and temperature, is completed in 20 min with
of 0.05 molar alkali concentration. A typical recipe is given below:

Sod. Carbonate (0.5


5.3 gpl
M)

Sod. Bicarbonate
4.2 gpl
(0.05M)

Non-ionic
3 gpl
Surfactant

Temperature 96 °C

Time 20 min

Presence of salt especially calcium salts in alkaline degumming liquor


increases the degradation of silk. Use of sequestering agents like sodium
hydrogen pyrophosphate has been known to reduce this damage.

Commercial alkali based degumming formulations generally may contain


protective agent for silk, sequestrants, wetting/emulsifying agent, buffer
salts, alkali etc. examples are Miltopan SE (Henkel), P-400 (Hepatex AG),
Sopajet L (Indifar), Setafin (Henkel), Idrosolvan S40 (Bozzeto) and
Serilan PCS (ROTA).

Degumming with alkalis happens due to systemic hydrolysis of peptide


bonds, a non specific reaction.

90 | P a g e
Degumming with Organic Acids

Although acidic degumming has not been explored much, it is relatively


safer than alkaline degumming. With acids, effective degumming occurs in
the pH range of 1.5 and 2. Silk degummed sampled with citric and tartaric
acid are found give results. Mineral acids may result in significant damage
to silk, hence generally only organic acids are used. A typical recipe is
given below:

Tartaric acid (0.05


8 gpl
M/L)

Non-ionic
3 gpl
Surfactant

Temperature 110 °C

Time 60 min

It has been observed that for different Acids (e.g. Lactic, Tartaric, Citric,
Oxalic, Malonic, Succinic, Trichloroacetic, Dichloroacetic,
Monochloroacetic):

Weight Loss is almost independent of the acid type.

Unlike alkalis, dilute organic acids are specific in


their attack on peptide bonds linking aspartic &
glutamic acid.

Attack on above link is around 100 times faster than


other bonds.

91 | P a g e
The mechanism of acid attack on silk peptide bonds is shown below:

The concentration of acid is chosen such that the carboxyl groups of


aspartic acid are left undissociated. This ensures faster cleavage of petide
bonds of aspartic acid as compared to other acids.

Degumming with Enzymes

Degumming with enzymes is considered to be a safer method which


results in minimal damage to silk. Since it is carried out at milder
temperature and pH, the natural hydrophobic impurities are not removed
effectively. One of the advantages of using enzymes for silk degumming

92 | P a g e
lies in the fact that enzymes specifically targeting peptides bonds occurring
in majority in sericin can be selected. Since the constitution of sericin and
fibroin is different, such enzymes will have minimum action on fibroin.
Enzymatic degumming is considered suitable only for yarn degumming.
They do not work well on fabrics, due to their inability to enter the
interstices of the fabric.

The main enzymes used for silk degumming are trypsin, papain and
bacterial enzymes.

Trypsin

Trypsin is a serine protease with the highest activity at pH range 7-9 and


37°C. Ammonium bicarbonate (0.1 M/l) can be used as buffer. It is applied
at 1- 2% owf for 1-4 h. There are studies which claim better degumming
results when alkalis are combined with proteolytic enzymes. In other
studies, it is reported that a pretreatment with alkaline solution swells
sericin and results not only in better degumming but also in better scouring
(wax, fat removal).

Papain

Papain is obtained from papyrus latex. It is the most effective at 70-90 oC


temperature and at pH-5. It is a sulphydryl enzyme and hence requires a
sulphydryl compound as an activator. Earlier, potassium cyanide and
hydrogen sulphide and later sodium hydrosulphide, sodium sulphoxylate,
sodium sulphite etc. have been used as activators. Papain has a wider
specificity towards polypeptides as compared to trypsin.

Bacterial enzymes

93 | P a g e
Bacterial enzymes can also be used for silk degumming. A bacterial
enzyme alkalase, developed by Novo nordisk is claimed to be more
effective than trypsin or papain.

Degumming with Aliphatic Amines

Aliphatic amines have been shown to be effective as degumming agents.


Methyl, dimethyl, ethyl and trimethyl amines can be used. Methyl amine,
due to its low boiling point is not suitable for commercial use. Amines
show good degumming (upto 90 % sericin removal) with little loss in
tensile strength. Given below is a typical recipe:

Trimethyl
0.25 mol/L
Amine

N.I.D. 3 gpl

Temperature 80 °C

Time 45 min

M:L ratio 1:25

Amines can also remove impurities like processing oil etc.

Comparative assessment of different Degumming Methods

Given below is a table which shows comparative assessment of different


degumming methods. Different methods have been evaluated on the basis
of weight and strength loss after degumming. The values with soap have
been taken as the basis. It can be seen that soap, alkali and acidic
degumming give the highest gum removal. However, alkali and acid both

94 | P a g e
cause significant strength loss which points to silk damage. On the other
hand amines seem to be good at degumming as well as retaining strength.
Enzymes while good at retaining strength are not able to remove the
sericin very effectively. This is a limitation especially with fabrics where
due to their large molecular size enzymes molecules are unable to enter the
interstices of the fabric. Hence enzymatic degumming may be preferred for
yarns rather than fabrics.

Weight Strength
Agent
Loss Loss

Marseille Soap 100 100

Carbonate + Bicarbonate
100 82.2
buffer

Tartaric acid 100 81.3

Methyl Amine 97.7 119

alkalase 85.5 112.9

ASSESSMENT OF DEGUMMING

The simplest method to assess degumming is based on weight loss.


However, in this case initial rapid weight loss may be followed by attack
on fibroin. UV absorption at 280 nm has also been used to assess extent of
degumming. Absorption is due to tyrosine and tryptophan.

A lot of staining methods are also available which are based on the ability
of a large molecular weight dye to differentiate between sericin and

95 | P a g e
fibroin. For example, picrocarmine stains sericin in intense red color while
the fibroin is colored yellow. Similarly, sericin in raw silk threads is
stained deep blue when immersed for 24 hours in a cold solution of litmus
while fibroin remains almost unstained.

8.6 Bleaching of silk


The natural colour of the silk varies with the type of the silk. Bulk of the
naturally occurring colour in the silk is actually contained in sericin. Since
the degumming process is not able to remove the sericin completely, Silk
fibre retains some of its natural tint after boiling off. Thus mulberry silk
retains some of its yellowish tings and in tussah silk it is even more
intensive. Thus the case of obtained white colour in silk by bleaching
varies with the silk variety. Generally oxidative & sometimes reductive
bleaching is employed in silk bleaching.

Silk is widely bleached with hydrogen peroxide with a typical recipe given
below:

Mulberry
Parameter Wild silk
silk

H2O2 (35%
15-20 ml/l 20-30 ml/l
w/v)

Stabilizer 2 gpl 4 gpl

M:L ratio 1:20 1:30

Temperature 75-80 80-90

Time (hr) 1-2 3-4

96 | P a g e
pH 8.5-9 8.5-9

The alkali used is either ammonia or tetra sodium pyrophosphate. Sodium


silicate as the stabilizer should be avoided as it can lead to formation of
silicic acid which can render silk harsh. Tetra sodium pyrophosphate and
fatty protein condensates are preferable.

9. Preparation of synthetic fibers & blends

9.1 Introduction
Synthetic or manmade fibers are generally free from natural impurities
which are present in most natural fibers. However the following may be
present in synthetic or manmade fibers which may require removal before
the material is dyed or finished:

a ) Sizing agents

b ) Spin finishes/anti static agents

c ) Processing/coning oils (in knits)

d ) Sighting colours/dirt

e ) Loom stains (grease, lubricants etc)

97 | P a g e
The sizing agents generally used with synthetic fibers are either water
soluble or self emulsifiable compositions. They are easily removed at
desizing stage. Therefore scouring of synthetic fibers is less cumbersome
than natural fibers. For most of the synthetic fibers, mild alkaline
conditions in presence of a surfactant are sufficient to remove the
impurities listed above.

Scouring of Polyester:

The scouring conditions are

Alkali (NaOH,
- 2 gpl
Na2CO3, NH4OH)

Temperature - 70-80 °C

Time - 30-60 minute

In case of a loom stain, spotting with a suitable emulsified organic solvent


may be necessary.

Scouring can also be carried out with anionic surfactant. Conditions are:

Anionic
- 1-2 gpl
surfactant

Temperature - 80-95 °C

Time - 20-30 minute

While scouring with alkali, it is important to note that harsh conditions


(high alkali concentration or higher temperature) may lead to polyester

98 | P a g e
fiber hydrolysis. This can result in weight and strength loss.

Scouring of Nylon:

Nylon is used mostly in knit goods. The signs are generally not used but
coning oils may be present. These may be self emulsifiable formulations.
Since nylon acidic and basic sites present in its structure, anionic
surfactants are avoided for scouring, as they can occupy dye sites and may
be difficult to remove. The scouring conditions are generally mild alkaline
with presence of non-ionic surfactants. The conditions are:

Non-ionic
- 2-3 gpl
surfactant

Anionic - 1-2 gpl

Soda ash - 1-3 gpl

Temperature - 70 °C

Time - 20-30 min

Heat set fabrics can be treated at a higher temperature (95-100°C)


compared to unset fabrics (70-80°C).

Scouring of acrylic (PAN) Fiber:

PAN fibers are sensitive to alkaline conditions, hence strong alkalis are
generally avoided for scouring.

Conditions

99 | P a g e
Non-ionic
- 1-2 gpl
detergent

Tri sodium
- 1 gpl
phosphate

Time - 30 sec

Temperature - boil

It is important to cool the goods below 60°C before rinsing. Sudden drop
in temperature may result in formulation of creases which may be difficult
to remove later.

Scouring of Viscose:

Viscose fiber also does not contain any natural impurity. It can be scoured
by:

Non-ionic or ionic surfactant - 1-1.5 gpl

Temperature - near boil

Time - 20-30 min

Soda ash or tri sodium


- 1 gpl
phosphate

Goods should be rinsed in tension less state as the wet strength of regular
viscose is poor.

100 | P a g e
9.2 Bleaching of synthetic fibers

Regenerated cellulosic fibers


Regenerated cellulosic fibers like viscose are similar to cotton in respect of
chemical composition. They are free from naturally occurring colouring
matter. The bleaching that sense may be required to get rid of the
coloration caused due to greases, lubricants, rust, stains adventitious dirt
etc. The degree of polymerisation is much less than cotton and the degree
of crystallinity is also lower. Hence the bleaching process for viscose and
other regenerated fibers should be milder than that for cotton to limit the
possible chemical degradation. Since viscose is chemically purified
cellulose, bleaching agent used for cotton can also be used for viscose.

Bleaching with NaOCl

Bleaching with NaOCl can be carried out with 1.5 gpl available chlorine
concentration. The pH is adjusted to 10-11 with soda ash at room
temperature and bleaching carried out for upto 1 hr.

Bleaching with H2O2 :

The presence of heavy metals arising from xanthation stage makes this
fiber prone to degradation during H2O2 bleaching. Bleaching can be carried
out with 1 volume H2O2 solution at 70°C for 1 hr. pH can be adjusted to 9
with soda ash/caustic soda and sodium silicate can be used as a stabiliser.

Bleaching of Nylon:
Nylon is a sufficiently white fiber but heat setting can cause some

101 | P a g e
discoloration which may require bleaching. Nylon should be preferably
bleached in acidic conditions due to its sensitivity to basic ph. Hence both
hypochlorite and H2O2 are not recommended. Bleaching with hypochlorite
can reduced the tensile strength of nylon fiber. Sodium chlorite is the most
suitable agent for nylon. Following recipe can be used.

NaClO2 (80%) - 1-2 gpl

Sodium Nitrate - 1-3 gpl

Formic acid
- 2 ml/l (pH-3.5-4)
(85%)

Time - 1 hrs

Temperature - 80-85 °C

Bleaching of acrylic fibre:


PAN can also be bleached with sodium chlorite in acidic ph. It is not
recommended to bleach PAN with either H2O2 or NaOCl in alkaline ph.
Acidic pH of sodium chlorite is safer for PAN. The recipe is

Sodium
- 0.4-0.7% (owf)
chlorite

pH - 3-4

Temperature - 70-80°C

Time - 30-40 minute

102 | P a g e
Bleaching of polyester:
For bleaching of PET also, sodium chlorite is preferred as it is used in
acidic ph. The recipe is:

NaClO2 (50%) - 3-5 gpl

Formic acid - for pH to 3

Time - 1-2 hrs

Temperature - 95°C

9.3 Scouring of blends

Polyester- cotton
Since polyester is sensitive to alkaline conditions at higher temperature,
milder alkaline condition is used while scouring polyester/cotton blends.

Following recipe may be used

Na2CO3 - 5-10 gpl

Emulsifier - 2-5 gpl

Polyester-wool blend
The blend of polyester and wool may contain spin finishes, lubricants,

103 | P a g e
sizes etc. These can be removed under relatively milder conditions.

The scouring is carried out with following recipe:

Non ionic recipe - 0.5-1 %

Soda ash/ NH4OH 0.25-0.5


-
(25%) ml/litre

pH - 8-9

Time - 20-30 min

Temperature - 40-50 °C

Acrylic/wool blends
Scouring can be carried out as follows:

Time - 30 min

Temperature - 100 °C

Non-ionic
- 1 gpl
detergent

Acetic acid
- 0.5 ml/litre
(80%)

9.4 Bleaching of blends

Polyester/cotton

104 | P a g e
In general, the cotton component of such blends requires bleaching. For
bleaching of cotton hypochlorite, chlorite and hydrogen peroxide can be
employed. If both cotton & polyester need to be bleached, sodium chlorite
bleaching is preferred.

For blends, hydrogen peroxide is the preferred route for bleaching.

The following recipe can be used for bleaching P/C blends-

30-40
H2O2 (35%) -
ml/litre

Sodium 10-12
-
silicate ml/litre

NaOH
- 2-4 gpl
(100%)

The fabric is padded with the liquor, steamed and stored in a J-box at 95
°C for 75 min. After the bleaching, the fabric is washed with hot water and
dried.

Polyester/wool blends
Since wool cannot be bleached with hypochlorite and chlorite, blends of
wool can only be bleached with H2O2.

Following recipe may be used-

H2O2 (35%) - 30-40 ml/litre

Sodium - 2-4 gpl

105 | P a g e
pyrophosphate

To maintain pH
NH4OH -
at 8.5-9.0

Time - 2-4 hrs

Temperature - 40 °C

Nylon/ Wool blends


The only safe bleaching methods to bleach such blends is either reduction
bleaching or bleaching with acidic H2O2 with following recipe:

12-15
H2O2 (35%) -
ml/litre

Organic
- 2-4 gpl
stabilizer

Wetting agent - 0.25 gpl

for pH (5.5-
Acetic acid -
6)

Time - 2-2.5 hrs

Temperature - 65°C

106 | P a g e
10. Assessment of various pretreatment processes

10.1 Desizing
Assessment of desizing efficiency

The weight loss can be used as criteria for assessment of desizing efficiency

The weight loss is of the order of 7-10%

The more scientific method, which is used industrially also, is TEGEWA


rating test

(Applicable for starch based sizes only)

It is a scale, which consists of colours ranging from violet to white as


given below.

TEGEWA SCALE

The TEGEWA Association comprises of manufacturers of the following:


Textile, paper, leather and fur auxiliaries and colourants, surfactants,

107 | P a g e
complexing agents, antimicrobial agents, polymeric flocculants, cosmetic
raw materials, pharmaceutical excipients and allied products.

TEGEWA was established in 1951 in Wiesbaden as an association of the


manufacturers of chemicals, the name being an amalgam of these key
activities: TExtilhilfsmittel” (textile auxiliaries), “GErbstoffe” (tanning
agents) and “WAschrohstoffe” (detergent raw materials).

Reagent preparation

Ten gram (10 g) potassium iodide (KI,100%) is dissolved in 100 ml of


water

To the solution, 0.6358 g of iodine (100%) is added

The mixture is stirred well until iodine is completely dissolved in the KI


solution.

To the solution, 800 ml of ethanol is added

The volume is to 1000 ml by adding water

Method of testing

One or two drops of the above solution are put on the desized fabric and
rubbed gently. The fabric should be cold and free from any residual
alkalinity. In a short time the color of the spotted area changes. The change
in color is assessed with TEGEWA scale visually.

Assessment

108 | P a g e
No Colour Change = No starch is present

Pale blue to bluish violet = Presence of starch size or a blend of starch +


synthetic size

Brown = Presence of modified starch or a blend of starch/PVA size

10.2 Degradation of Cotton during Desizing


Degradation can occur with acid or oxidative desizing if proper care is not
taken during the desizing process

Acid desizing

Insignificant degradation of cotton with dilute sulphuric acid (upto 10 gpl) at


R.T.

Degradation of cellulose can take place if the temperature increases beyond 40


oC or the concentration increases beyond 10 gpl

Fluidity increases from 4 to 5.8 rhes in 4 h

About 70% of the starch is removed

The fabric should be washed thoroughly and traces of acid neutralized

If fabric dries before acid is removed completely, cotton degrades as per the
following equations

109 | P a g e
This results in lowering of DP of cellulose (M. Wt.)

The end –OH groups undergo tautomeric change to CHO

This –CHO (aldehyde) group has reducing power

Most organic acids in dilute solution have little effect on cotton

In case of enzymatic desizing, the degradation of cotton is minimal.

110 | P a g e
10.3 Scouring

On scouring cotton, following changes take place:

Loss in weight (5-10%)

Significant increase in absorbency (1-3 seconds)

Further improvement is TEGEWA rating

Slight increase in average DP (due to removal of low mol. wt. components)

Shrinkage

Assessment of scouring efficiency

Practical tests of absorbency

Measurements of

Weight loss

Protein content

Residual wax content

Methylene blue absorption (removal of pectic substances)

111 | P a g e
Practical tests of absorbency

Sinking time test (AATCC Test Method 17-1994).

The scoured yarn is converted to a hank (18 in periphery, 5 g wt). The hank is
connected with the help of a hook (3 g) to a sinker which is a flat cylindrical plate
(25 mm diameter, 15-40 g wt). The assembly is put on 500 ml water in a glass
measuring cylinder. Initially the air entrapped in the hank causes the hank to float
but as wetting starts and the air is replaced with water, the hank starts to sink due
to attached sinker. The time required by the hank to go inside water from floating
state is known as sinking time.

Drop test

The fabric is placed flat on a table and creases are removed. A burette is placed at
a certain height from the fabric surface. Distilled water drops are allowed to fall on
the fabric. The time required for the drops to be absorbed completely is noted as
wetting time.

Measurements of Weight loss

The weight of dried cotton sample before and after scouring may be used as an
indicator of scouring efficiency. This difference when expressed in % (% wt loss)
should be in the range 6-9%.

Measurements of Protein content

The protein content is determined indirectly by analysing nitrogen content after


scouring.

Measurement of residual wax content

112 | P a g e
A dry cotton sample is refluxed for 3 h in chloroform in the Soxhlet extractor and
(solvent). After extraction the sample is reweight and the wt. loss is determined
which is indicative of removal of fat and wax. For well scoured cotton, it should be
~0.2%.

Methylene blue absorption (removal of pectic substances)

The details of this are given in next section.

10.4 Degradation of cotton during alkaline scouring


Although cotton is stable in dilute alkalis at high temperatures in absence
of air, presence of air causes serious degradation. This mainly results in
oxy-cellulose formation, during which some hydroxyl groups on
glucosidic units get oxidized to keto and carboxylic groups.

Assessment of the degradation can be done by either assessing the


aldehyde/carboxylic group content of cellulose, measurement of fluidity or
loss in tensile strength.

Following are some of the methods for assessment of cotton cellulose


degradation:

1. Copper number, a measure of the reducing groups present in cellulose.

2. Carboxyl group content by methylene blue absorption

3. C uprammonium fluidity, which is a measure of molecular chain length


of cellulose.

4. Tensile strength of the cotton material before and after scouring.

113 | P a g e
1. Copper number

The first stage of cellulose oxidation during cotton souring results in


formation of –CHO groups from –OH groups. These aldehyde groups have
a reducing tendency and can reduce alkaline solution of copper sulphate,
resulting in formation of insoluble cuprous oxide which precipitates on the
cotton cellulose. The amount of cuprous oxide formed is proportional to
the amount of reducing groups which is expressed as Copper Number.

The test is carried out as under-

A solution is prepared by dissolving 100g copper sulphate in 1 litre of


water. Another solution is prepared by dissolving 350 g sodium carbonate
and 50 g sodium bi carbonate in another 1 litre of water. These two
solutions are mixed just before use to form Fehling’s solution.

Three groups of cotton cellulose is boiled in a solution containing 100 ml


of Fehling’s solution and 200 ml of water under reflux for 15 min. during
the boiling process some copper sulphate is reduced to cuprous oxide
which gets deposited on cellulose.

This mass of cellulose is filtered & washed with water. The cellulose is
then transferred to a beaker containing 1-2 gm fabric alum dissolved in
dilute sulphuric acid. The cuprous oxide present in cellulose reduces ferric
sulphate and forms equivalent amount of ferrous sulphate. This is titrated
against N/100 ceric sulphate solution by dissolving the ferrous sulphate in
sulphuric acid. Ortho ferrous phenathroline is used as an indicator.

Thus copper number is defined as grams of cupric copper reduced to

114 | P a g e
cuprous oxide by 100 g of cellulose under standard treatment conditions.

The copper number is determined by the following formula:

Where V = ml of ceric solution - blank reading

N is the normality of ceric sulphate solution

W is the weight of the bone dry cellulose sample (it depends on type of
sample; for normal samples it is 0.25 g and for highly degraded samples
0.1 g is taken

Copper number for pure cellulose is 0.5, for scoured & bleached cotton
below 0.3 & for viscose less than 1.2.

2. Methylene blue absorption method

Normal cellulose generally has no affinity for methylene blue, a basic dye.
When cellulose in oxidized, -OH groups convert to aldehyde group. But
when the oxidation is more severe, these aldehyde groups can oxidize to
carboxylic groups. In degraded cellulose, both –CHO & -COOH groups
may be present. Hence there is a need to determine the degree of cellulose
oxidation in terms of –COOH groups content.

Methylene blue absorption method is based on the principle that the


carboxyl groups present in cellulose are able to absorb methylene blue dye
cations quantitatively from a solution of methylene blue dye. The scheme

115 | P a g e
is shown below:

The amount of dye absorbed can be determined by analyzing the drop in


concentration of methylene blue in treatment solution using calorimetric
methods.

3. Cuprammonium fluidity

The degradation of a polymer results in reduction of degree of


polymerization. At same concentration, the degree of polymerization is
related to the viscosity of its solution. Fluidity (ease of flow) is a property
inversely related to viscosity (resistance to flow). Thus the degradation
resulting in reduction of the DP can also be assessed by measuring fluidity.
In case of cotton the fluidity measurements are made on solution of cotton

116 | P a g e
material in cuprammonium hydroxide solution. In the table given below,
fluidity values of various forms of cellulosic textiles are given.

Fluidity
Type of cellulose
values

Unbleached cotton ~2

Bleached cotton <5

Degraded cotton showing loss in


>10
tensile strength

standard unbleached viscose ~10

Physical testing

Tensile strength, bursting strength and abrasion resistance, Tear strength can
be measured

The results are influenced by both fabric structure and chemical damage.

Tear strength is also influenced by residual natural lubricants.

Staining tests

Carboxyl groups in oxidized cellulose resist staining with C.I. Direct Blue
1 or give increased uptake of C.I. Basic Blue 9.

Harrison test

The oxycellulose test sample is immersed in a boiling alkaline silver

117 | P a g e
nitrate solution.

Brown to black deposits of silver are produced on the substrate where


there are reducing aldehyde groups.

Barium Activity Number

Mercerized cotton fibre is highly absorptive. It absorbs more iodine, dyes,


moisture and alkalis and undergoes oxidation or hydrolysis at increased
rates compared to unmercerized cotton.

BAN method is based on preferential absorption of barium hydroxide from


its dilute solution by mercerized cotton as compared to unmercerized
cotton under the same conditions.

Barium activity number is determined by expressing this ratio as


percentage.

BAN of

Unmercerized cotton - 100

Semi-mercerized cotton - 115 to 130

Completely mercerized cotton ~ 155 .

11. Heat Setting

118 | P a g e
11.1 Heat Setting
Polymers in the form of Textiles of various shapes and types
have been used by mankind for centuries

Certain properties – strength, comfort, thermal


conductivity/insulation, dyeability are important

The structural/molecular basis of the properties – only ~ 100


year old

What we know today:

Polymers consist of amorphous and crystalline zones

Crystals Amorphous

Stability, strength, Extensibility, pliability,


durability, cohesion etc toughness, diffusion, etc

Recovery – an important property in which both crystalline and


amorphous parts and their interaction contributes

Most textile polymers are partially oriented semi-crystalline in


nature

After manufacture – they are rarely in equilibrium (low energy


relaxed state)

This may be due to the manufacturing method

Stresses are generated duringdrawing, spinning, weaving or


knitting and finishing processes by extension, twisting and bending

119 | P a g e
forces.

Any subsequent heat treatment or washing produces stress


relieving that shows up as shrinkage or change of shape.

Hence they become susceptible to dimensional instabilities

Fibre ------> Yarn -------> Fabric --------> Garment manufacture


introduce more instabilities

(This can result in high thermal shrinkage, permanent deformation


etc.)

Hence there is a need to get rid of these instabilities

This is called setting

Objective

To achieve the dimensional stability of a yarn or fabric containing


thermoplastic fibres by achievement of a desired stress-free form of
the fibres making up a textile product.

For thermoplastic fibres – this is mostly done by heat energy aided


by moisture and tension

For natural fibres – this is generally done by chemical treatment


aided by tension and moisture

Type of heat treatments

Dry hot air, steam, liquid baths etc.

Conditions

120 | P a g e
Tensionless or under tension

Temperature

Higher than maximum application temperature expected in


downstream processing

Example of heat setting by a hypothetical experiment of stress


relaxation:

Figure 1 : Load–deformation diagram with stress relaxation


and recovery

Suppose a textile fibre or yarn is stretched along OA and held in

121 | P a g e
the extended form. If heat is applied to the fibre for some time, the
load drops to CB from CA. If yarn is now allowed to recover by
slowly removing the stress, it does not return to its original state. A
permanent residual deformation equal to OD is retained. In other
words, heat was used to relieve the stresses the yarn had built-up
during stretching. The heat applied allows the yarn to relieve
stresses; the longer the treatment the better is stress relaxation and
poorer the recovery.

Origin of instability

Polymers cab be divided in the following category depending on


their structure and behavior towards thermal treatment

Category I – whose molecules are synthesized in chain extended


form (biopolymers), or by stress and flow induced polymerization

Category II – whose structure is developed by solid stste drawing


or rolling (As it is difficult for the chains to fully relax in solid
state, the systems develop locked in stresses)

Category III – Highly crystalline and oriented structure like gel


spun UHMWHDPE fibres

The residual stresses reside in

Amorphous state or defective crystalline phase

Thermal transitions

Tg Tm

122 | P a g e
Glass transition Melting temperature
temperature

Characteristics of Characteristics of crystalline


Amorphous phase phase

Tg (Glass transition temperature)

Above Tg– segmental mobility starts

This happens due to breaking of Van der Waals forces, H-bonds


etc.

Enough free volume becomes available for rotation of molecular


segments

When cooled below Tg– the structure becomes frozen and a setting
is obtained

Temporary Set

By heating the material above Tg

Breaking of existing Van der Waals forces/H-bonds and allowing


the material to obtain equilibrium state

Cooling the material below Tg and freezing the structure in the


relaxed state

But the material is not able to reach the equilibrium state and hence
the set obtained is only temporary

123 | P a g e
It can easily be lost by moisture or a little heating

Example – wrinkles in a washed garments

Mechanism of permanent set

Permanent setting effects are associated with a change in


crystalline morphology

Modification of crystalline morphology can be done by

Partial melting and recrystallization

The most common route

Involves partial melting of small, imperfect, or irregular crystallites


at a temperature much below the real melting point, and a growth
of larger, more perfect crystals.

Crystallization of Oriented Amorphous Phase

Crystallization of molecules in the amorphous regions that are well


parallelized but not in register

Perfection of Crystals

By expelling the defects out of the crystal

Thickening of Crystals

Localized axial movement of fold stems can lead to refolding

In heat setting the material is led from its existing state to a new
state of lower minimum energy by modification of its internal

124 | P a g e
structure (crystalline and amorphous state and orientation)

11.2 Heat setting behavior of different fibres


Mechanical properties are affected by heat setting.

(Tenacity, elongation, modulus, recovery, shrinkage, swelling,


dyeing behavior, lustre etc.)

The effect of heat setting temperature on tensile strength of a


nylon 6,6 fibre in slack unrestrained state is given in figure 2. It is
easy to notice a sharp drop in tensile strength at ver high annealing
temperatures (close to melting point).

Figure 2 : Change in Breaking Strength of a Nylon 6,6 fibre


with increasing annealing temperature

125 | P a g e
Effect of heat setting temperature on shrinkage and elongation in
slack, unrestrained state is shown in figure 3 and 4.

Figure 3 : Shrinkage as a function of annealing temperature


for nylon 6,6 fibre

It can be seen that shrinkage is increasing with increasing heat


setting temperature. One possibility for this observation could be
increasing disorientation with increasing treatment temperature.
However, one look at the figure 4 reveals that increasing shrinkage
is not really due to increasing disorientation. Figure 4 shows
breaking elongation with increasing heat setting temperature. It is

126 | P a g e
easy to see that elongation initially increases but then falls off
rapidly at higher temperature. Increasing disorientation would
have resulted in increasing breaking elongation of nylon filaments.
But since s hrinkage is not recoverable in the form of elongation, it
is not simply a disorientation process.

Figure 4 : Effect of heat setting on elongation of a nylon 66


fibre (slack unrestrained)

Hence it can be inferred that shrinkage involves changes other


than disorientation especially at high heat setting temperatures.

127 | P a g e
Shrinkage – two stage process

1. Disorientation (mostly in amorphous phase)

2. Chain folded structure

At lower setting temperatures, disorientation in amorphous regions


prevails resulting in shrinkage. But at high setting temperatures,
the disoriented chain segment start forming crystal structures by
folding (figure 2b).

128 | P a g e
Figure 5 : Model of a (a) drawn and (b) annealed yarn with
folded chain structure

Crystallinity increases – by local melting and recrystallization


through chain folding

129 | P a g e
Increase in folded chain fold segments. Such folding can
occur if heat setting is done under unrestrained condition (no
tension). Folding results in high shrinkage which is not
recoverable in the form of high elongation. Crystallinity may
still increase as folded chain may fit into a crystal register.

Effect of tension on Properties

Free annealing (tensionless) – reduces molecular orientation and


tenacity, increases fibre diameter and denier

Tension annealing – increase in tenacity, crystallinity, no change


in diameter/denier

130 | P a g e
Figure 6. Effect of heat setting tension on tenacity of
annealed polyester yarn

This is clearly seen in figure 6. Annealing under tension does not


allow significant disorientation and hence the tenacity is
maintained. However, with reducing tension, the tendency to
disorient decreases, resulting in a concomitant decrease in
tenacity, especially at high temperatures.

Recommended setting temperatures

131 | P a g e
Different fibre types require different setting temperatures. Even
within a given polymer, the specific fibre type may require
different setting temperature. For example, bulked or textured
polyester filaments are generally heat set at lower temperatures to
maintain the bulk. Setting temperatures used in the industry for
various fibre types are given in the table below:

Setting
Fabric
Temperatures

Woven and knit goods of


170–195 °C.
textured polyester filament:

Fabrics of polyester filament: 185–220 °C.

Polyester (bulked yarn) 150 °C

Blends of polyester and cellulose


180–210 °C.
fibres:

Wool blends 170 °C

Nylon 6.6 (filament) – woven 200–210 °C

Nylon 6,6 (filament) – knitted 220–225 °C

Nylon 6 (filament) 180–190 °C

Acrylics 140 °C

132 | P a g e
Tricel 190–210 °C

11.3 Effect of setting on Properties: Dyeing, handle,


pilling, shrinkage
Measurement of the degree of Set

The main objective of the heat setting is to eliminate hidden


stresses and strains in the fibre structure to enable it to achieve a
more relaxed and lower energy stable state. The effectiveness of
the treatment can be judged from the following methods.

Critical Dissolution Time (CDT)

The basic premise of CDT lies in the fact that heat setting process
results in larger and more crystalline phase. The dissolution time of
a crystal in a given solvent will be related to its size. In CDT
method, the dissolution time of a loop of filament is measured and
recorded as a plot between CDT and density of the filament.

The CDT value increases with increasing crystallinity as a more


crystalline filament takes longer to dissolve.

In the figure shown below, CDT is plotted against the density of


the filament. As can be seen, small changes in crystallinity (from
1.375 to 1.405) result in large changes in CDT (~10 to 1000).
Hence it can be said that CDT is a very sensitive technique which
can detect even small changes in the fibre structure sufficiently

133 | P a g e
accurately.

Figure 1 Dependence of
CDT on Density of
polyester fibre

Because of its sensitivity CDT can also be used to analyze the


variations between and within bobbins.

In figures shown below, the CDT is plotted against the sample


taken from various positions within a bobbin. It can be seen that
some variations, however small, exists even within a bobbin.

134 | P a g e
In figure 2 a), fibre C is more variable than fibre B.

Figure 2 a) Variation in CDT with


position of bobbins for two different
fibres b) variation within the same
bobbin

Recovery from bending strains

This is an important assessment since in case of apparel fabrics,


crease and wrinkle recovery are important attributes of the overall
usefulness of a garment. In this method the fibres are wound on a
rod for a given number of turns under constant tension. The wound
fibres are heat set for 10 minutes and the rod is allowed to cool.
The tension is removed from the fibres and recovery is allowed.

After 10 minutes of recovery the length of the helix and the

135 | P a g e
number of turns are measured. The set is calculated from the
equation

EQUATION

L1 = Initial length of the helix

L2 = Length of the recovered helix

N1= Initial number of helix turns

N2= Number of turns after recovery

The schematic of the apparatus is given in the figure below.

Figure 3 Setting
apparatus

In the figure below, set is plotted for PET, nylon 6 and nylon 66 as


a function of temperature. It can be seen that for nylon the degree

136 | P a g e
of set is low below Tg (45°). The set increases sharply above Tg and
levels off at a value ~ 80% for higher heat setting temperatures. For
PET it increases near Tg and reaches a high value (~90%) at higher
setting temperatures.

Figure 4 Dependence of Set on


setting temperature for PET,
nylon 6 and 6,6

Effect of heat setting on fibre properties

As has been discussed earlier, heat setting can result in changes in


fibre structure. Thus crystallinty, crystal properties, orientation, etc.
can be affected. These changes can affect certain fibre properties
like modulus, bending rigidity, shrinkage, etc. Since the dye uptake

137 | P a g e
is a function of overall crystallinity, it can also be affected.

1) Dimensional stability (Shrinkage)

Heat setting is essentially a disorientation process and results in the


shrinkage of fiber/yarn. The shrinkage is higher for higher
heatsetting temperature. In the figure given below the shrinkage of
a medium tenacity PET yarn is plotted as a function of heat setting
temperature in hot air. The shrinkage results in increase in
elongation and lowering in breaking load. However the residual
shrinkage after the heat setting process drops significantly. Thus ,
heat set fabrics have much better dimentional stability as compared
to unheat set fabrics. For this reason synthetic fabrics like PET are
heatset in grey state as shrinkage can take place during
pretreatment and dyeing. Not only unheatset fabrics tend to shrink
by large amounts during dyeing, they also tend to crease
uncontrollably and the creases are very difficult to remove later.

The shrinkage of unheatesetpolyester yarn is ~15% at 175° as


compared to 1% for heatset fibres at 220°C.

138 | P a g e
Figure 5 Hot air
shrinkage of PET yarn

2) Crease recover

One of the important objectives of heat setting is to reduce creasing


of synthetic fabrics during wet operations (wet creasing). Wet
creasing reduces with increasing setting temperature.

3) Dyeing

Figure 6 shows typical dyeing behavior of a polyester fibre dyed


without carrier and heat sett at various temperatures. It is
interesting to note that initially the

139 | P a g e
Figure 6 The effect of heat-setting temperature on
dye uptake when polyester is dyed with C. I.
Disperse Red 1

Dyeuptake of the fibre decreases with increasing setting


temperature, reaches a lowest value around 160 to 180°C, and then
starts rising. At very high temperatures, it becomes higher than
unheatset fibre. The initial decrease occurs due to increase in
crystallinity of fibre. At high setting temperatures, crystallites grow
at the expense of smaller/imperfect crystals and become more
perfect. This results in increase in the amorphous volume per
crystal. The path for dye diffusion becomes less tortuous and dye

140 | P a g e
absorption increases.

However, the practice of using very high setting temperatures for


improving polyester dyeuptake is not followed. The setting
temperatures used for polyester generally result in a little drop in
dyeuptake as compared to unheatset fibre. However, heatsetting
results in a uniform dyeuptake, whereas non heatset polyester
fabric absorbs dye in a non uniform way and chances of obtaining
unlevel dyeings increase. In table 1 below, typical temperatures
used for heat setting various fibres are given.

Pilling

The problem of pilling occurs due to entanglement of protruding


fibres in a yarn. These loose fibre convert to small fuzzy balls due
to rubbing or abrasion. Generally singeing is a way of dealing with
this problem. In case of synthetic fibres heat setting can reduce pill
formation. During heat setting, the loose end of the protruding
fibres shrink and get embedded more firmly in the yarn structure.
Reduction in the length of loose ends reduces the chance of pill
formation.

141 | P a g e
12. Machinery for preparation of textiles
Textile machinery can be classified as batch, semi continuous and
continuous one. While semi continuous and continuous machinery
generally is used for textile fabrics, batch machines are available
for fibre, yarn as well as fabrics & garments.

Batch machines

Pre-treatment is carried out mainly on kier, winch and jigger


machines.

KIER

Kiers are cylindrical vessels especially designed to carry out


scouring of cotton in rope form. Kiers may be open where
scouring is carried out at boil at atmosphere pressure or may be
closed to carry out scouring at high temperature and pressure. The
material of construction is generally steel or cast-iron in which
case the inner side is rendered passive by a coat of sodium silicate,
cement and magnesium sulphate.

The kier has a perforated false bottom, located about 18 inches


above the base. The fabric is piled on it either manually or by a
mechanical plier. It is important to lay the fabric in an even
manner otherwise channels of least resistance may form leading to
uneven scouring. The movement of fabric during boiling may be
avoided by putting heavy weights over the fabric pile.

142 | P a g e
The capacity of a kier is generally 2 tons but may vary from 0.5 to
5 tons.

The circulation of the liquor is maintained by passing stream in the


kier through a central piper (puffer) through a hole in the
perforated bottom. The steam draws liquor with it which hits a
curved baffle plate above the goods & is distributed over the
surface of the fabric. The liquor gradually percolates down the pile
below the perforated bottom from where it is again forced through
the buffer pipe by the steam pressure. Use of steam to circulate
liquor as well as heat it is not very efficient and economical.
Moreover, steam condensation may result in an increase in M: L
ratio which is generally maintained at ~1:3. Hence many modern
kiers use external heat exchangers and the circulation is
maintained by a powerful centrifugal pump.

For scouring of cotton in kiers, it is important that all air is forced


out from the system as cotton can be oxidized into oxycellulose in
presence of air in hot alkaline liquors. This is ensured by heating
the liquor to 90°C & then stopping heating and circulation for 10-
15 min. the steam and air is allowed to escape from a valve. The
liquor is heated again & air is allowed to escape periodically till
only steam emerges out from the valve. After this the valve may
be closed & scouring continued for desired time.

143 | P a g e
144 | P a g e
Jigger

Jigger is one of the oldest fabric processing machines and can be used for pre-treatment and dyeing of textile fabrics. It is used for processing of
fabrics in open width, tensioned form. Hence those fabrics which can be withstand tension and must not be creased during processing can be
processed on jigger.

Jigger consists of a V-shaped trough. Two steel or ebonite rollers are fitted above the trough over which the fabric to be treated is wound in roll
form. Fabric passes from one roller trough guide rollers in the trough to the other roller. Since most the fabric in roll form remains out of the
trough, a low ML ratio (3-4) can be maintained.

During the process, the fabric in open width form unwinds from one roller, passes through guide rollers in the trough & winds on the other roller.
When all the fabric from first roller is transferred to the second roller, a reversal mechanism is activated & the direction of the fabric movement
is changed from second roller to the first. This process continuous till the treatment is over. Complete transfer of the entire fabric length from one
roller to the other is known as one end or turn. For a given process, the no. of turn depends on the residence time required for the process. Each
end may take 10-15 min.

The liquor in the trough may be heated by steam running through pipes in trough & having perforations. Early jiggers were open but now a days
they come equipped with top covers to minimize heat loss through evaporation.

Old jiggers

Trough
- 200 l
capacity

Fabric - 500-
length 1000 m

Modern high capacity jiggers-

Trough
- 750 l
capacity

Fabric - ~5000

145 | P a g e
length m

An additional roller is placed on fabric wound roller such that it squeezes out liquor from the fabric into the trough.

Jiggers can be used for desizing, scouring or even bleaching of textile fabrics.

Winch

It is another old processing equipment which processes fabrics in rope form. It is suitable for all those fabric which can withstand creasing during
rope form processing. One of the major differences a winch has with a jigger is lower amount of tension working on fabrics during processing.
During processing, most of the fabric remains submersed in a deep trough which increases M:L ratio (1:20 or 25) as compared to a jigger. Due to
much lower lengthwise tension imposed on the fabric, winches are better suited for processing of delicate fabrics like knits & woollens.

146 | P a g e
In winch the fabric is processed in the form of an endless loop. The fabric is piled over the sloping bottom of a deep trough (figure below). At the
deeper end of the trough, the fabric rises & passes over a 15 cm diameter reel known as jockey or flyer and then over a much larger elliptical
winch reel. The rotation of the winch reel provides the motion to the fabric. There is no positive grip between the fabric and the reel. The fabric
movement takes place due to the friction and the weight of wet fabric.

At a time one and more ropes can be dyed. When dyeing multiple ropes, separation is maintained by a peg rail. The peg rail runs through the
width of machine and is located at about 20 cm above liquor level.

147 | P a g e
The main chamber of winch is divided into two parts by a perforated stainless steel sheet. The smaller chamber situated towards the front of the
machine is used for making additions of dyes & auxiliaries as well as for housing the steam pipes.

The M:L ratio in winches is high, generally around 1:25. Winch provides little sideways movement of the fabric, as it can result in entanglement.
Most of the fabric remains in the form of a slowly moving pile at the machine bottom. This can result in uneven dyeing. The high M:L ratio also
results in poor dye exhaustion of low substantivity dyes.

Winches can be used for desizing, scouring, bleaching or even washing of textile fabrics.

Semi-continuous or continuous machines

148 | P a g e
Padding Mangle:

It is one of the most familiar machines for use in dyeing, pre-treatment or finishing. It is used for application of chemicals or even dyes to the
fabric in a uniform manner in open width form. The completion of the reaction or dye fixing is carried out by batching, steaming, curing etc.

This machine is used in continuous and semi-continuous methods of chemical/dye application to fabrics. It is suitable for application of low
substantivity dyes or chemicals to fabrics.

Hence, padding mangle is only one part of a process in which chemicals or dyes are transferred to the fabric uniformly. The reaction or dye
fixation is carried out separately by a suitable combination of time and temperature in another machine (batching device, steamer, curing
chamber etc.)

The mangle consists of two cylindrical rubber bowls with a stainless steel mandrel. The diameter of bowls is equal with 55-70° shore hardness.
The bowls should be perfect cylinders with smooth surface. The size is generally 170-200 cm in length and 30-40 cm in diameter.

In general the lower bowl is fixed and is driven by an electric motor. The top bowl is mounted on arms pivoted at the side in such a way that
there is a gap (~2 cm) between the two bowls when the machine is not in operation. The upper bowl moves by contact friction generated by the
pneumatic pressure.

For operation, pneumatic pressure is applied on the top bowl which may be as high as 50 kg/cm [10 tons for a 2 meter bowl].

The fabric to be padded is passed through a padding bowl or trough which is situated below and in front of the mangle. The bowl is filled with
padding liquor. As the fabric passes through the trough guided by guide rolls, it gets saturated by the liquor. The stage is known as dip. Since the
passage time in the liquor is very small, the fabric should be well –prepared and be highly absorbent. In the next step the fabric passes through
the bowls in such a way that the squeezing pressure is applied on the saturated fabric, which is known as nip. While the bowls under pressure
move in opposite directions in such a way that the fabric is transported forward. The squeezing action of the bowls allows air in the interstices of
the fabric to be expelled which in turn is replaced with padding liquor. The liquor is distributed over the entire fabric surface uniformly and the
excess squeezed liquor flows back to the trough.

Since the liquor is continuously taken out by the fabric, it needs to be replenished continuously. The level in the trough is maintained by
overflow.

149 | P a g e
Sometimes due to tight construction of some fabrics, application of liquor may not be uniform in two bowl padding mangles which operate in
one dip one nip mode. Such fabrics may be handled by 3 bowl padding mangles by two dip two nip sequences.

Two Bowl Padding Mangles with Varying Troughs and Bowl Arrangements

150 | P a g e
Three-Bowl Padding Mangles with Varying Bowl Arrangements

J-Box:

After application of liquor by padding, the required time for chemicals to act on impurities is provided in a J-box or batching tray or steamer. J-
Box is one of the popular machines generally used in scouring of cotton fabrics. J-box is essentially a J-letter shaped stainless steel chute with
large fabrics holding capacity. The fabric is fed from one end & taken out of the other (First in first out) in contrast to a keir where it is first in
last out. The J-box has a polished inner side and it is insulated to minimise heat losses.

The fabric after saturation with liquor (from a saturator located just in front of J-box) is fed from the top and taken out from the lower end.
Depending on fabric speed (150-300 m/min) and the capacity (10,000 m) a residence time of 60-90 min may be provided. Fabric may be heated
at the entry to the J-box and may retain the temperature due to insulation inside the chamber. M:L ratio 1:1.

After coming out from the J-box, the fabric is sent to a washer. In the schematic below, the flow of material for desizing in a J-box is shown.

In continuous processing, it makes sense to combine various processes to save time, water, energy manpower etc. Combining desizing and
scouring in case of cotton is possible by using oxidative desizing agents which can work in alkaline medium. Similarly, scoring and bleaching
can be carried out in two continuous stages in one operation. This is shown in the schematic shown below.

Steamer:

Alternately, after saturating the fabric with the liquor, it may be sent to a steamer. The speed is about 60 m/min, temperature 100-110°C and
residence time 30 sec to 5 min. The J-boxes

151 | P a g e
J-box

152 | P a g e
Desizing in a J-Box

153 | P a g e
Dupont two stage continuous scouring and bleaching range

154 | P a g e
Steamer

have large capacity as the fabric is stored in rope form and moves down due to gravity. In steamers the capacity is much lower as fabric is
processed in open width form.

Continuous machines generally do not operate at high pressure. However, there is one high pressure reaction chamber that can operate at high
pressures and hence can reduce reaction time significantly. This is known as Vapor-Loc unit.

Vapor-loc

In vapour lock unit, which is essentially a high pressure steamer, fabric entry and exit is through hydraulic sealing heads. These heads consists of
PTFE diaphragms where pressure is higher than the chamber pressure. The pressure in the unit may be 2 atm, temperature 134°C. The reaction

155 | P a g e
time is only 90-120 sec. The capacity of the machine is around 200 m which allows fabric speed of about 120 m/min.

Mather & Platt continous open-width pressure reaction chamber

Washing-

Washing an important stage in all stages of pre-treatment. The aim of washing is to remove the added or natural impurities, residual auxiliaries
etc. Since washing is done with water, the impurities must be either water soluble or emulsifiable.

Modern washing practise aim to improve washing efficiency by utilising minimum water to remove impurities, at present it is about 4-6 litre
water/kg goods.

Rope washing machine:

156 | P a g e
Tight rope washing machine-

This machine maintains high tension on the fabric during washing & hence is used for medium of heavy fabrics.

The fabric in rope form passes through the nip of squeezing rolls in to the water trough and again into the nip. Thus many loops of the fabrics are
made which are separated by the pegs below the bowls & allow the rope to move in a spiral fashion. Fresh water is continuously fed to the tank.

The rollers are heavy, with a wooden lower roller and the upper ones are made from highly compressed cotton. Squeezing is provided by levers
& weights.

157 | P a g e
158 | P a g e
Tight rope washing machine

One disadvantage of tight rope washing machine is fast contamination of the water in the box. Feeding fresh water and removing soiled water
helps to some extent.

However, the problem has been tackled to a large extent by placing a small trough below the squeeze rollers. Fresh water is fed at the exit end
and the soiled squeezed water is collected in the smaller trough which is then directed to a drain. This reduces contamination of the water in the
bigger trough considerably.

Slack rope washing machine

This is a machine similar to the previous machine in that it relies on squeezing action for liquor inter-change. The difference lies in the low
tension exercised in this one. It also consists of two hard wooden rollers with lower roller driven & the upper one friction driven. Beneath these
rollers is situated a large wooden tank with slanting bottom.

The fabric enters the nip of the rollers, into the tank where it slides down the bottom of the tank. From the deeper section of the tank, the rope is
led over a freely rotating roller, into the nip and finally to the exit. A small wooden box is situated just below the bowls to collect soiled water
squeezed out from the bowls to minimize the contamination of the tank.

Open width continuous washing machine

These are used whenever the fabric is being processed on a continuous machine in open width crease free form. Generally the liquor is stationary
and the fabric movement through the liquor provides some mechanical agitation and liquor interchange.

159 | P a g e
Slack rope washing machine

160 | P a g e
Mostly the washing machines are a series of washing boxes/chambers working on the principle of counter current flow of fresh washing liquor.
The fabric and the liquor movement from one box to the other is designed to maximize interchange of liquor & minimize the contamination of
subsequent chamber. The process is aided by frequent squeezing of fabric. The basic processes involved are squeezing, diluting and diffusing.

One of the machines working on this concept is Mather & Platt Aquatex unit. The fabric passes between a set of top & bottom parallel rollers
such that the bottom rollers are immersed in liquor. Each compartment or chamber may consist of five or six such top/bottom rollers. As the
fabric moves from the bottom rollers upwards to the upper roller some carry over liquor flows down back. Additionally pressure rollers above
the top rollers help to squeeze more contaminated liquor back. The bottom rollers are separated by metal plates to avoid mixing of liquor as
fabric moves forward. Counter current flow of wash liquor is used which ensures that as the fabric moves forward it comes in contact with
fresher liquor. As the liquor moves against the fabric it gets dirtier & finally exits from the fabric entry point.

The need to save space has led to double threading with additional rollers in vertical direction. This increases fabric capacity and number of
immersions at a given speed. However threading becomes complicated & costs also go up.

The temperature of washing liquor affects washing efficiency at higher temperature, the viscosity of liquor goes down, the solubility of
impurities goes up and the rate of diffusion also increases. In general, a temperature of 95°C seems to be optimum.

A continuous washing range often consists of a number of compartments or chambers. The fabric movement from one to the next is facilitated
by a carryover roller or nip mangle to reduce liquor carryover.

161 | P a g e
Aquatex unit

162 | P a g e
Benninger Becoflex washing compartment

Horizontal washing machines:

Here the fabric moves horizontally between two sets of vertical rollers & gradually moves up. The fresh liquor is fed from the top & moves
down. The water coming in contact of the fabric may either pass through it or spill over the selvedge.

163 | P a g e
Horizontal washer

164 | P a g e

You might also like