Pretreatment of Textile
Pretreatment of Textile
Pretreatment of Textile
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Pretreatment of Textile
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Preparation for Dyeing and Printing
4/13/2022
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Abel Taye
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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
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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
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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
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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.
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1. Introduction
1.1 Introduction to Pretreatment
Need for preparation/ pretreatment
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.
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.
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Sodium perborate Lithium hypochlorite
Peracetic acid
Sulphur dioxide
Sodium
hydrosulphite
Sulphoxylates
Acidic sodium
sulphite
Sodium bisulphites
thioureadioxide
increases
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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.
HOCl →HCl + [O] ↑
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HOCl →HCl + [O] ↑
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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.
H2O −
ClO− + 2I− + 2 H+ → I2 + Cl
+
Similarly
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chlorine.
Effect of pH
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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.
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Figure 2 Rate of oxidation of cellulose in terms of the consumption
of half the total available chlorine.
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for bleaching.
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
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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
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pH 6-7 (bleaching time 1 min.)
pH 9-11.5
It is economical
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due to which its use is on the wane. These are:
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acids or acid liberating agents to bring down the pH when
bleaching takes place.
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.
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Figure 4 Effect of pH on the composition of sodium
chlorite liquors.
Reactions:
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HClO2 → 4ClO2 + HCl +2H2O at lower pH
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Suitable pH for bleaching – 3-4.5(4+-0.2)
Effect of Temperature:
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for several hours.
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.
It can give good white colour with excellent mote removal even
without kier boiling.
Disadvantages
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coloration ).
Antichlor Treatment
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bottles. It is quite stable in acidic pH and can decompose in
presence of alkalis or UV light.
Mechanism
Activator
Stabilizer
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Sequestering agents
Activators:
Stabilizers:
Buffering action
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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.
Sequestering Agents
Poly phophonates
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Phosphonic acids
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EDTA (Ethylene Di-Amine Tetra
Acetic Acid)
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Figure 5 A simplified
representation of EDTA-metal
complex
Effect of pH:
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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.
Effect of temperature:
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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.
Disadvantages
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into high, uniform whiteness, the most important assessment of
textile goods is assessment of whiteness. This is done by:
W(Harisson)= 100-(R670–R430)
2. Calorimetric method
W= L-3b
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parameters. Thus
W(Stansby)= L-3b+3a
W(Burger)= 0.333Y+1.060Z-1.277X
5. Mercerization
1844 - John mercer observed the effect.
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Improving Elasticity or Stretch material (in slack mercerization
only).
MECHANISM-
NaOH
Composition of
Conc. (% Type of hydrate
hydrate
by Wt.)
Solvated dipole
NaOH.10H2O 18
hydrate
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A°)
Composition of Hydrodynamic
hydrate volume (dia Å)
Solvated dipole
8-10
hydrate
Separated Hydrated
15-20
ion pair
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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.
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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.
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C6H10O5 , NaOH, 3H2O
NaOH. 5H2O
NaOH. 7H2O
Na-Cell I
NaOH. 10H2O
(C6H10O5)2 , NaOH. 2H2O
NaOH. 12H2O
(C6H10O5)2 , NaOH. 1.5H2O
NaOH. 2H2O
C6H10O5 , H2O
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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.
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Swelling of cellulose fibres in Alkali solutions
This will be clear from the figure shown below which shows
swelling of cotton fibres with different alkali concentrations at
different temperatures.
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Kontturi, Tekla Tammelin, Monika Osterberg
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
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solution at 0 °C, it will dissolve!
Structural Modification
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treatment, temperature and tension employed in the process.
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crystallinity of cotton also goes down slightly on mercerization.
Effect of temperature
Enhancement in lustre
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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:
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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.
Mechanical properties
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after mercerization
Effect of tension
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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.
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Effect of NaOH conc. on Mechanical
Properties of Cotton Yarn Mercerized at
Constant Length
Dyeing Properties
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content)
Rate of dyeing
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Effect of Mercerization on Dyeing
Properties of Cotton Yarn at constant length
(dye- CI Direct blue 1)
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K – Light absorption factor, S – light scattering factor, C is
concentration and a is a constant
R - reflectance
Upon mercerization
In general, the increased dye absorption and the optical effect may
contribute roughly equally towards increased Visual colour yield
after mercerization.
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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.
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Certain alkylarylsulphonates
Hot mercerization
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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.
Advantages:
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The fabric can be stretched to greater degree as the fabric
becomes more plastic
The sequence
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in one operation.
Washing
Washing of fabric at 95 °C
Impregnation in NaOH at 20 °C
Impregnation in NaOH at 30 °C
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Washing
Uniform dyeability
Mercerization of blends
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Hank Mercerizing Machine
Yarn mercerization
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in lower tensile strength.
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of fabric getting torn near the edges where it is held by clips.
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Where B = Volume of HCl (ml) required for blank titration
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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.
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goods with a blue tinge to it, making it appear much brighter.
Aesculetin-6-glucoside
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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.
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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
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appear coloured. This is shown in figure (page-479) below.
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
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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.
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.
The most common OBAs for cellulosic fibres are based on triazine
derivatives of diaminostilbene disulphonic acid (DAST) with
following chemical structure.
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Where M is alkali metal like Na or K, or ammonium cation
However, it is expensive.
Nylon –
OBA generally used for Nylon are anionic in nature like acid dyes.
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These are generally applied from an acidic bath pH – (4-5).
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.
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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.
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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
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combined pre-treatment processes will be discussed.
(Pad -steam)
Potassium per
- 3 gpl
sulphate
70
Sodium hydroxide -
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.
The options available for cotton scouring are alkaline scouring with
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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 %
Time - 2 hrs
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
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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.
The attempts to combine all three sequences are again based on alkaline
scoring and bleaching.
Scouring agent - 4 %
Hydrogen per
- 1-2 %
oxide
Temperature - 95 °C
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Sodium silicate - 2 %
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.
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ROCO yet bleaching system
Be –Impacta – Impregnation
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Steam passage
through the fabric
in a narrow casing,
Ben Injecta
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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.
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without
intermediate
squeeze
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.
Sequences-
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Acidification → Drying/Baking →
rushing → Dusting → Neutralization
Processing Stages:
Treatment with (5-7% w/v) sulphuric acid & acid stable wetting agent.
Hydro extraction
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)
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to metallic machine parts may lead to
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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)
III
0.25 0.1 43-46 2
BOWL
IV Water
- 40-43 1.5
BOWL only
Oxidative bleaching-
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.
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obtained.
Reductive bleaching
Thiourea dioxide
Sodium dithionite
Bleaching with thio urea oxide is 3 times cheaper in cost and also has the
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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.
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 .
b) Boil-off in soap.
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c) Degumming with alkalies.
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:
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Try 0.19 0.20 0.25 0.23 0.21
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.
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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
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
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correlation is apparent.
Degree of
Kind of Degumming
hydrolysi
soap loss (%)
s (%)
Coconut
28.8 16.77
oil
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
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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
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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. Bicarbonate
4.2 gpl
(0.05M)
Non-ionic
3 gpl
Surfactant
Temperature 96 °C
Time 20 min
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Degumming with Organic Acids
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):
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The mechanism of acid attack on silk peptide bonds is shown below:
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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
Papain
Bacterial enzymes
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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.
Trimethyl
0.25 mol/L
Amine
N.I.D. 3 gpl
Temperature 80 °C
Time 45 min
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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
Carbonate + Bicarbonate
100 82.2
buffer
ASSESSMENT OF DEGUMMING
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
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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.
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)
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pH 8.5-9 8.5-9
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
d ) Sighting colours/dirt
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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:
Alkali (NaOH,
- 2 gpl
Na2CO3, NH4OH)
Temperature - 70-80 °C
Scouring can also be carried out with anionic surfactant. Conditions are:
Anionic
- 1-2 gpl
surfactant
Temperature - 80-95 °C
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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
Temperature - 70 °C
PAN fibers are sensitive to alkaline conditions, hence strong alkalis are
generally avoided for scouring.
Conditions
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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:
Goods should be rinsed in tension less state as the wet strength of regular
viscose is poor.
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9.2 Bleaching of synthetic fibers
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.
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
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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.
Formic acid
- 2 ml/l (pH-3.5-4)
(85%)
Time - 1 hrs
Temperature - 80-85 °C
Sodium
- 0.4-0.7% (owf)
chlorite
pH - 3-4
Temperature - 70-80°C
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Bleaching of polyester:
For bleaching of PET also, sodium chlorite is preferred as it is used in
acidic ph. The recipe is:
Temperature - 95°C
Polyester- cotton
Since polyester is sensitive to alkaline conditions at higher temperature,
milder alkaline condition is used while scouring polyester/cotton blends.
Polyester-wool blend
The blend of polyester and wool may contain spin finishes, lubricants,
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sizes etc. These can be removed under relatively milder conditions.
pH - 8-9
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%)
Polyester/cotton
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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.
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.
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pyrophosphate
To maintain pH
NH4OH -
at 8.5-9.0
Temperature - 40 °C
12-15
H2O2 (35%) -
ml/litre
Organic
- 2-4 gpl
stabilizer
for pH (5.5-
Acetic acid -
6)
Temperature - 65°C
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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
TEGEWA SCALE
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complexing agents, antimicrobial agents, polymeric flocculants, cosmetic
raw materials, pharmaceutical excipients and allied products.
Reagent preparation
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
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No Colour Change = No starch is present
Acid desizing
If fabric dries before acid is removed completely, cotton degrades as per the
following equations
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This results in lowering of DP of cellulose (M. Wt.)
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10.3 Scouring
Shrinkage
Measurements of
Weight loss
Protein content
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Practical tests of absorbency
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.
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%.
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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%.
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1. Copper number
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.
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cuprous oxide by 100 g of cellulose under standard treatment conditions.
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.
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.
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is shown below:
3. Cuprammonium fluidity
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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
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.
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
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nitrate solution.
BAN of
11. Heat Setting
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11.1 Heat Setting
Polymers in the form of Textiles of various shapes and types
have been used by mankind for centuries
Crystals Amorphous
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forces.
Objective
Conditions
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Tensionless or under tension
Temperature
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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
Thermal transitions
Tg Tm
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Glass transition Melting temperature
temperature
When cooled below Tg– the structure becomes frozen and a setting
is obtained
Temporary Set
But the material is not able to reach the equilibrium state and hence
the set obtained is only temporary
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It can easily be lost by moisture or a little heating
Perfection of Crystals
Thickening of Crystals
In heat setting the material is led from its existing state to a new
state of lower minimum energy by modification of its internal
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structure (crystalline and amorphous state and orientation)
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Effect of heat setting temperature on shrinkage and elongation in
slack, unrestrained state is shown in figure 3 and 4.
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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.
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Shrinkage – two stage process
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Figure 5 : Model of a (a) drawn and (b) annealed yarn with
folded chain structure
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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.
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Figure 6. Effect of heat setting tension on tenacity of
annealed polyester yarn
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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
Acrylics 140 °C
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Tricel 190–210 °C
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.
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accurately.
Figure 1 Dependence of
CDT on Density of
polyester fibre
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In figure 2 a), fibre C is more variable than fibre B.
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number of turns are measured. The set is calculated from the
equation
EQUATION
Figure 3 Setting
apparatus
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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.
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is a function of overall crystallinity, it can also be affected.
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Figure 5 Hot air
shrinkage of PET yarn
2) Crease recover
3) Dyeing
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Figure 6 The effect of heat-setting temperature on
dye uptake when polyester is dyed with C. I.
Disperse Red 1
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absorption increases.
Pilling
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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
KIER
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The capacity of a kier is generally 2 tons but may vary from 0.5 to
5 tons.
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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
Trough
- 750 l
capacity
Fabric - ~5000
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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.
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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.
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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.
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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.
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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
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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
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J-box
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Desizing in a J-Box
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Dupont two stage continuous scouring and bleaching range
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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
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time is only 90-120 sec. The capacity of the machine is around 200 m which allows fabric speed of about 120 m/min.
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.
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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.
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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.
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.
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.
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Slack rope washing machine
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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.
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Aquatex unit
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Benninger Becoflex washing compartment
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.
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Horizontal washer
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