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Pamantasan ng Lungsod ng Maynila

College of Engineering and Technology


Department of Chemical Engineering

Nitration of Pineapple
(Ananascomosus)Leaves for the
Production of Pyroxylin Lacquer

Submitted by:
Madrial, Andrea Coleen E.
Mendoza, Marian D.
Raguini, Jasmin Fatima D.
Saya, Diana Jane S.

Submitted to:
Engr. Milagros R. Cabangon

Date of Submission:
APRIL 4, 2016

Nitration of Pineapple Leaves for the Production of Pyroxylin Lacquer 1


Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

TABLE OF CONTENTS

Introduction 3

Statement of the Problem 4

Objectives of the study 5

Significance of the study 6

Scope and limitations 7

Review of Related Literature 8

Review of Related Study 16

Methods of Reseach 17

Experimental Method 20

Process Flowchart 40

Process Diagram 41

Conclusion 42

Recommendation 43

Referecences 44

Nitration of Pineapple Leaves for the Production of Pyroxylin Lacquer 2


Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

INTRODUCTION

Pineapple leaves, though already being employed in the textile (Fitzgerald, B., 2015) and

animal feed industry in the country (Tran, 2006),are still being burned for disposal by majority of

the farmers here in the Philippines (Baconguis, S. 2014) and this method contributes to the air

pollution (Wan &Zainuddin, 2013).The outer peel or skin and core from the pineapple canning

industries, called bran, and the leaves are being utilized as feed for ruminants. However, some

researchers have reported that the leaf bracts are not considered attractive as an animal feed

because of high fiber content and soluble carbohydrates with low protein content (Correia et al.,

2004). Tagaytay City produces 4,788.70 metric tons of pineapple for the year 2009 with which

generates 383 to 478 metric tons pineapple leaf bracts (Cavite Government). One excellent way

to dispose pineapple leaf bracts, which has a cellulose content of 57.75% (The Philippines

Recommends for Pineapple, 2010), while avoiding the method of burning for disposal is to use

them as a raw material for the production of a coating material called lacquer.

Lacquer is a protective coating primarily based on nitrocellulose (cellulose nitrate) that

dries primarily by evaporation of solvent rather than oxidation of polymerization (Department of

Trade and Industry).The estimated total capacity of the lacquer manufacturers is approximately

equivalent to 250 million liter per annum. Demand for this product increased by 40 million liters

from 2013 to 2014 and is anticipated to have a continuous increase on the coming years (PAPM,

2014). However, the local supply in the market could not satisfy the mere 11% of the total

demand for 2014 and the rest of these are satisfied by importation (PAPM, 2015).

Nitration of Pineapple Leaves for the Production of Pyroxylin Lacquer 3


Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

STATEMENT OF THE PROBLEM

In 2009, Tagaytay City was able to produce 4,788.70 MT of Pineapple which

generates large amount of agricultural wastes such as pineapple leaves that is still has no proper

waste disposal management. Waste disposal is a major problem, because of very high lignin and

cellulose content of the leaves which is difficult to be degraded, thus resulting in pollution and

affecting the environment.Often times, pineapple leaves are utilized as animal feed (Tran,

2006).However, some researchers have reported that by-product of pineapple processing industry

is not considered attractive as an animal feed because of low protein content (Correiaet al.,

2004).Another way of disposal is burning the residues in an open field; however these methods

are not only ineffective but also contribute to air pollution (Wan &Zainuddin, 2013).

Burning of the pineapple leaves produces 40% of carbon dioxide (CO2), 32% of

carbon monoxide (CO), 20 % particulate matter (PM) and 50% of polycyclic aromatic

hydrocarbons. These leaves contain 57.75% cellulose (The Philippines Recommends for

Pineapple, 2010), which is important in producing lacquer that can solve the growing

demand for this product.

The demand for lacquer increased immensely by 16 percent from 2013 to 2014 and is

expected to increase in the following years (PAPM, 2014). However, local supplies cannot match

the 11 percent of the total demand that results to importation of the product (PAPM, 2015).

Nitration of Pineapple Leaves for the Production of Pyroxylin Lacquer 4


Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

OBJECTIVES OF THE STUDY

General:

To produce pyroxilin lacquer through nitration of cellulose from pineapple leaves

Specific:

To determine optimum qualities of the product by comparing the physical and chemical
properties of the standard pyroxylin lacquer
Properties Existing Proposed
Boiling Point/Range 77 C < 77%
Appearance and color Colored viscous liquid with Colored viscous liquid
strong ester odor with strong ester odor
FTIR Spectrum
Solubility Insoluble in water Insoluble in water
Table 1. Standard and Proposed PropertiesofPyroxylin Lacquer

To find out the best pre-conditioning parameters of the pineapple leaves before
undergoing chemical reaction to achieve the proposed property of pyroxylin lacquer
To determine the best operating conditions like particular alkali reagent, concentration of
reagent and most effective ratio of solution in pineapple leaves which will provide best
yield of the product
To identify the equivalent unit equipment of every laboratory process and apparatus

Nitration of Pineapple Leaves for the Production of Pyroxylin Lacquer 5


Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

SIGNIFICANCE OF THE STUDY

To the Pineapple Plantation Proprietors of Lagusan Drive, Tagaytay City

The consumption of pineapple leaves as the main raw material for lacquer production

would provide the pineapple plantation proprietors of Barangay Lagusan Drive another option

for maximizing the use of pineapple leaves instead of burning it.

To the Chemical Engineering Undergraduates and Researchers

This study can be used as a reference for undergraduate subjects related to industrial

research by chemical engineering students who will make use of pineapple leaves as their main

raw material to manufacture products related to lacquer.

To the Philippine Paint Manufacturers

Through this study, the Philippine paint manufacturers would benefit by producing

pyroxylin lacquer from pineapple leaves instead of making use of synthetic resins.In addition to

that, the manufacturers would be able to help reduce the pineapple leaf wastes.

Nitration of Pineapple Leaves for the Production of Pyroxylin Lacquer 6


Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

SCOPE AND LIMITATIONS

The study titled Nitration of Pineapple Leaves for the Production of Pyroxylin

Lacquer focuses on the use of pineapple leaves in order to produce nitrocellulose lacquer. The

digestion process in order to obtain the cellulose from the leaves was also the existing

manufacturing process which is modified to produce the same quality lacquer. The study only

covers the determination of size of the pineapple leaves, alkali to be used in the digestion

process, ratio of the solvent to the solute and the concentration of the alkali.

The researchers were able to use only limited quantities of chemicals and raw materials in

conducting the experiment; hence, the trials were only limited up to 3. It is also due to the finite

resources why the parameters in the nitration process i.e the variation of catalyst, the ratio of the

catalyst to the nitric acid and the ratio of alcohol to ether were not identified. Also, difficulty in

access to different research materials related to the study has really turned out to be a factor in

incorporating reliable sources and data. In addition, technical grade chemicals were used during

the nitration process.

The pineapple leaves prior to the experiment was not tested for its cellulose content;

hence the researchers relied to the gathered data and studies. The product was tested using the

Fourier Transform Infrared Spectroscopy (FTIR) and only the physical properties of the existing

were compared to the outcome of the research.

Nitration of Pineapple Leaves for the Production of Pyroxylin Lacquer 7


Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

REVIEW OF RELATED LITERATURE

A. RAW MATERIALS
A.1Cellulose content of Pineapple Leaves. Plant materials used for the production of

cellulose contain three main components besides from water are cellulose fibers, lignin, and

hemicellulose. The cellulose is the component needed for this research. Lignin, is a three-

dimensional polymer that binds the cellulose fibres together. Moreover, hemicelluloses are the

shorter branched carbohydrate polymers than the cellulose (Holik H., 2006).

Table2.Chemical Composition of Pineapple Fiber


Variety Moisture (%) Lignin (%) Cellulose (%) Hemicellulose (%) Others (%)
Queen 11.24 6.82 57.75 19.02 5.17
Source: (Department of Science and Technology, 2010)

According to the The Philippine recommends Pineapple of the Depart of Science and

Technology, pineapple leaves has the following chemical composition. The researchers used the

Queen type of pineapple which according to Table 2 has 11. 24% of moisture. With this

information, drying of the leaves was bypassed. The pineapple leaves having high cellulose

content, 57.75%, would be efficient for producing pyroxylin.

Based from the article, A Review on Pineapple Leaves Fibre and Its Composites (Asim et. al..,

2015), pineapple leaf consist of 11.8% of moisture. Its cellulose content is ranging from 60-72%

and a lignin content of 5-11%. This information acquired from an international journal, though

having small increments, supports the above citation of chemical composition of pineapple leaf.

Nitration of Pineapple Leaves for the Production of Pyroxylin Lacquer 8


Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

A.2Cellulose content of Pineapple Leaves compared to other Agricultural waste.

Table3. Comparison of Cellulose Content


Type Moisture (%) Lignin (%) Cellulose (%) Hemicellulose (%) Others (%)
Pineapple 11.24 6.82 57.75 19.02 5.17
leaf [1]
Sugar Cane 10.32 20.50 28.75 12.28 28.15
Bagasse [2]
Coconut 15.00 24.93 20.29 7.23 32.55
Husk [3]
Sources: [1] Department of Science and Technology, 2010 [2] Manalo, et. al.., 1992 [3]
Tejano, E.A, 1985 [4]

Philippines being an agricultural country produces tons of agricultural crops. Most of the

common are coconut husk and sugar cane bagasse. Philippines is also one of the top producers of

tropical fruits and plants such as pineapple. The waste from this plants and crops can be

converted into a useful product. Cellulose can be extracted from this agricultural waste. Table 3

shows the composition of cellulose in the fibers of sugar cane bagasse, coconut husk and

pineapple leaf.

The researchers made use of pineapple leaves among the two top leading agricultural waste in

the country because of its high cellulose content.

A. 2 Production of Pineaappine in Tagaytay. Pineapple is considered one of the

commercially important plants in the province since it has helped increase the income of most

municipalities in the province like Silang, Indang, Alfonso and Tagaytay City, its major

producers. Tagaytay alone produces 4,778.70 MT of pineapple.

Nitration of Pineapple Leaves for the Production of Pyroxylin Lacquer 9


Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

Table 4: Pineapple Production by City/Municipality, Province of Cavite: 2009

City / Municipality Production (Metric Tons)


District VII
Tagaytay City 4,778.70

Source: Office of the Provincial Agriculturist, TreceMartires City (2009)

A. 3. Utilization of Pineapple leaves

Frequently, pineapple leaves are utilized as animal feed (Tran, 2006).However, some

researchers have reported that by-product of pineapple processing industry is not considered

attractive as an animal feed because of low protein content (Correiaet al., 2004).Another way of

disposal is burning the residues in an open field; however these methods are not only ineffective

but also contribute to air pollution (Wan &Zainuddin, 2013).

A. 4. Effects of Pineapple leaf burning

According to the Commission for Environmental Cooperation,It is estimated that burning

biomass, such as wood, leaves, trees and grassesincluding agricultural wasteproduces 40%

of carbon dioxide (CO2), 32% of carbon monoxide (CO), 20% of particulate matter (PM), and

50% of polycyclic aromatic hydrocarbons (PAHs) released into the environment around the

globe. Although agricultural waste burning is not an environmentally acceptable form of

agricultural management, it is a frequent practice and is worrisome from a public health

viewpoint for a number of reasons.

Nitration of Pineapple Leaves for the Production of Pyroxylin Lacquer 10


Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

A. 4. Pineapple Leaf Related

According to Benjamin Fitzgerald, as couture bites into fruit as a source of natural fiber, the

amount of pia used in textiles is steadily growing across North America. Pia importer Ecossar,

is just one textile firm working directly with local artisans in The Philippines, to spread pia's

reach. More designers need to experience the luxury of this fruit-based thread, completely

derived from pineapple leaves.

B. Processes

B.1 Alkali Digestion

Alkali digestion is a process that extracts fibrous material, cellulose. The purpose of

alkali digestion is to liberate cellulose fibers from other chemicals and impurities in the fibrous

source. Alkali digestion uses lye (a caustic soda) to remove lignin from fibrous source. (Sixta&

Herbert, 2006)

B.2 Nitration Process. Nitration is a broad class of chemical process for the introduction

of a nitro group into an organic chemical compound (Booth, 2012) For this process, nitric acid is

the main reagent used the addition of a nitro group, usually to an organic molecule. Also

commonly used as a strong oxidizing agent (Zumdahl, S., 2009). Usual nitration syntheses apply

so-called "mixed acid", a mixture of concentrated nitric acid and sulfuric acids. Sulfuric acid is

not required to nitrate the cellulose but acts as a catalyst to produce nitronium ion, NO2+, and

acts as an absorbent for water (McMurry, J., 2007)

Nitration of Pineapple Leaves for the Production of Pyroxylin Lacquer 11


Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

The first step of nitration is to activate nitric acid with sulfuric acid to produce a stronger

electrophile, the nitronium ion. Because the nitronium ion is a good electrophile, it is attacked by

cellulose to produce Nitrocellulose. (Clark, 2000)

Nitrocellulose is a highly flammable compound formed by nitrating cellulose through

exposure to nitric acid or another powerful nitrating agent. (Merck Index, 2013)

Two parts of concentrated sulfuric acid and one part of concentrated nitric acid is needed.

When acids are mixed, a lot of heat is produced, and the mixture needs to be cooled. The mixture

of these two acids is called a nitrating acid mixture. After acids are mixed, add there cellulose.

After 15 minutes, cellulose is nitrated. It should then be rinsed with water to get rid of the acid

residues and baking soda will be added for neutralization. (Thoisoi, 2014)

10% concentration of sodium bicarbonate solution is suggested. (TAPPI Standards)

3HNO3 +C6H10O5C6H8(NO2)2O5+ 3H2O

Fig. 1.The actual nitrating agent in nitration of aromatic compounds is the nitronium ion, NO2 +
derived from nitric acid by the action of sulfuric acid

Nitration of Pineapple Leaves for the Production of Pyroxylin Lacquer 12


Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

According to Prof. Steve Dessens of Houston Community College, when you mix pure

sulfuric acid with concentrated nitric acid (about 70% HNO3 in water), you are diluting the

H2SO4 just as if you were mixing it with water, which, you'll recall, is a very exothermic

process in which a weakly-held hydogen ion from H2SO4 is transferred to a water molecule,

forming hydronium ion, H3O+. Thus the old rule, "Add Acid" for sulfuric acid, meaning you

should slowly add the acid to the water instead of the water to the acid, to help prevent the

danger of sudden boiling and splattering of hot acid. Keeping things cool helps prevent this

overheating.

If you are mixing only a few milliliters of concentrated H2SO4 and HNO3, the amount of

heat released will not be so great, so a water bath at room temperature is normally adequate to

ensure that overheating does not occur. You can even do the mixing in a small graduated

cylinder with no water bath. But larger volumes are often mixed at ice bath temperatures just to

be on the safe side.

Aromatic nitrations easily result in "over-nitration" to form dinitrated products and/or

decomposition products if the reaction gets out of hand. This problem is lessened if the reaction

is done at lower temperature. Nitrations are also exothermic reactions, so in the absence of a

cold water bath, the increase in temperature could cause the reaction to get out of control.

Nitration of Pineapple Leaves for the Production of Pyroxylin Lacquer 13


Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

B.3 Neutralization

The reaction of acids with sodium bicarbonate is a common method for neutralizing acid

spills. The advantage to this method is that one can use excess sodium carbonate, which is

relatively innocuous. The neutralization process is signaled by the release of gaseous CO2The

sodium bicarbonate is an alkali and will neutralize much of the acid remaining (Powell, 2009)

NaHCO3 is a salt which consists of the ions Na+ and the bicarbonate anion, HCO3-. In

aqueous solution, these ions are separated. Furthermore the bicarbonate anion forms some

hydroxide, which results in its solutions being mildly alkaline (Robert, 2007)

(HCO3-)CO2+OH-

CO2 + 2NaOH Na2CO3 + H2O

B.4 Dissolutionof Nitrocellulose.

In a book, Practical Herbs 2 by Henriette Kress (an active online book since 1995).

Pyroxylin consists of dinitro-cellulose, C6H8(NO2)2O5 which is soluble in a mixture of alcohol

and ether. Alcohol is commonly used in the dissolving nitrocellulose.

For this research study, ethanol and petroleum ether which are forms of alcohol and ether

were used to dissolve the dinitro-cellulose.

C. Lacquer

C.1 Definition. According to the Department of Trade and Industry, lacquer is defined as

a coating that dries primarily by evaporation rather than by oxidation or polymerization. Because

Nitration of Pineapple Leaves for the Production of Pyroxylin Lacquer 14


Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

the solvents or water used in lacquers are relatively volatile and no chemical change is required

for formation of the film, lacquers dry very rapidly.

According to PHARMACOPEIA, pyroxylin lacquer contains not less than 5.0% and not
more than 14%, by weight, of pyroxylin. Ether to alcohol ratio is 3:1.

C.2 Pyroxylin manufacture and applications

According to Walter Field, the term pyroxylin is understood the soluble nitric ethers of
cellulose, namely the di, tri, tetra, and penta-nitrates. From the date of the use of pyroxylin in
photography by Scott Archer in 1851, the number of its uses has increased until, at present time,
tons of the lower nitrates of cellulose are produced yearly.

In the form of celluloid it is before us constantly. As a varnish it is used on penholders,


pencils, silver and brass ware. Articles are bronzed with it as a medium. An artificial leather has
been produced with it. These applications are all made, with the exception of celluloid, by the
use of a solution of pyroxylin.

C.1 INDUSTRY PROFILE

According to the Philippine Association of Paint Manufacturers, the estimated total

capacity of the lacquer manufacturers is approximately equivalent to 250 million liter per annum.

With a volume forecast that expected to expand a modest 8-9% annual rate. In addition, a 16%

annual rate growth is forecast for demand in architectural coatings as building activity expands

and the economy grows at a modest rate from 2013 to 2014.

Nitration of Pineapple Leaves for the Production of Pyroxylin Lacquer 15


Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

REVIEW OF RELATED STUDIES

1. Non-wood fibers for Rayon Grade High Alpha Pulp

Author: P.C. Francia, L.D. Belen, E.U. Escolano, and E.P. Villanueva

Fresh solution of pulping liquor with known concentration of active alkali was added. Abaca and
bagasse were cooked for 90 min; pineapple 60 min. Rise in temperature from 100 C to 170 C

Table 5: Cellulose components of Abaca, Bagasse and Pineapple leaves

Raw Material %Holocellulose %Alphacellulose %ash %lignin


ABACA
Grade S2 S3 88.1 64.1 0.6 8.8
Grade I, G, H 86.4 58.6 0.9 10.2
Bagasse 74.6 42.4 1.2 9.8
Depithed
Bagasse 71.5 - 2.39 20.5
Whole
Pineapple leaves 25.2 23.7 6 2.6
Source: FPRDI DOST

For the trial testing of the soda pulping, the researchers used 60 minutes as the base pulping time
for the experiment with a maximum temperature of 150 C.

2. Pulp and Paper Production from Nigerian Pineapple Leaves and Corn Straw as

Substitute to Wood Source

Author: Aremu, M., Rafiu, M., &Adedeji, K

Pulping of chipped pineapple leaves and corn straw was achieved using chemical pulping

method (soda pulping). About 200g of the raw material (oven-dry weight) was loaded into a

1000ml conical flask which was then placed in a pressure pot containing sufficient amount of

water. 42 g of pulping chemical (caustic soda) was dissolved in 600 ml of water (7% sodium

Nitration of Pineapple Leaves for the Production of Pyroxylin Lacquer 16


Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

hydroxide) and the solution was poured into the conical flask. The ratio of volume of water to the

weight of raw material was 3:1. Pulping time was 180 mins (3hrs).

Similarly, the ratio of the solvent to solute was adapted and the lower range is 2:1.

However, it is not possible because the pineapple leaves will not be submerged in the solution

thats why 2.5:1 is chosen instead.

METHODS OF RESEARCH

The experimenters conducted extensive research in order to have a comprehensive study


through experimentation for the analysis of the properties and characteristics of raw materials
and product. Different methods of research were used to obtain vital information and data for the
study. The methods are the following:

I. Descriptive Method

This method consists of the collection of qualitative and quantitative information


about the study such as related literatures and studies from different books, articles, and
journals. Local and international articles from different institutional and organizational
websites in relation to production and processing of lacquers from pineapple leaves were
collected by the researchers.The gathered data undergone intense analysis and was
summarized to be included in the review of related literature.

The researchers gathered the information for the availability and demand of pineapple
leaves and lacquer from different government institutions and electronic sources. As well
as the factual information for the description and properties of the raw materials. The
following are:

National Statistics Office (NSO) Ramon Magsaysay, Sta. Mesa, Manila


- Provided the data for the availability and demand of pineapple and
lacquer.

Nitration of Pineapple Leaves for the Production of Pyroxylin Lacquer 17


Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

Department of Science and Technology (DOST) Bicutan, Taguig City


- Science and Technology Information Institute Library of DOST
provided factual information of the raw materials and desired product.
Also, journals for the pulping and nitration process was gathered from
here.
National Library of the Philippines Kalaw, Ermita, Manila
- Information from books and articles about the raw material was
gathered.
Pamantasan ng Lungsod ng Maynila Library Intramuros, Manila
- Provided information for some terms used in the research.
Chemical Engineering Websites
- The researchers made used of internet for international and local
studies which include journal websites and portable document format
(PDF). Some of these websites are Science Direct, EBSCO, ScoPus,
and other academic sites.

II. Experimental Method

This method includes the detailed information and processes for the production of
nitrocellulose lacquer based from the gathered data in the review of related literature.
This method of research scientific undertaking was done through laboratory set-up for
experimentations. Various parameters were considered to come up the best quality of the
product which were anchored by the related studies and literature that was analyzed by
the researchers.

The experimental method was done at through the following:

Adamson University Laboratory San Marcelino St., Ermita, Manila


- Provided the laboratory space and apparatus for the experiment. They
also provided the product testing through FT-IR Spectroscopy.
Sta. Cruz, Manila
Nitration of Pineapple Leaves for the Production of Pyroxylin Lacquer 18
Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

- One of the researchers home provided further observation and


improvement of the product.

Nitration of Pineapple Leaves for the Production of Pyroxylin Lacquer 19


Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

EXPERIMENTAL METHOD
The experimentation was done in a laboratory scale. In order to produce the desired product,
variation of parameters such as size, alkali reagent, concentration of alkali reagent, and ratio of
liquor to raw material were observed.

A. Collection and Preparation of Raw Material


The raw material used which is the pineapple leaves are gathered and collected from
Barangay Lagusan Drive, Tagaytay City.
In this process, the pineapple leaves will undergo size reduction. From the study

Chemical Analysis and Pulping Study of Pineapple Crown Leaves, the leaf samples were cut into

pieces of 5 cm in length. This study was used by the researchers to set the parameter in the size

reduction of the pineapple leaves.

A.1 Size Reduction of Pineapple Leaves


a. Apparatus and Materials

scissors

Pineapple
leaves

Figure 9.1 Size Reduction of Pineapple Leaves

b. Objective
To determine the optimum size of pineapple leaves that will give a best yield for
alkali digestion process
c. Hypothesis
The smaller the size of the pineapple leaves, the faster the rate of reaction.

Nitration of Pineapple Leaves for the Production of Pyroxylin Lacquer 20


Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

d. Procedure
1. Measure and cut the pineapple leaves into 5 cm in length.
2. Weigh 150 grams of pineapple leaves and place it in 1-L beaker.
3. Pour450g of 10% NaOH solution to the 1-L beaker containing the
pineapple leaves.
4. Heat the pineapple leaves until it reaches 100C and digest for 60 minutes
after boiling.
5. After digesting, let it cool for 10 minutes.
6. Separate the pulp from black liquor and wash the pulp with 1-L water.
7. Dry the washed pulp for 15 minutes at 100C.
8. Weigh the obtained pulp and record.
9. Repeat steps 2-9 using 7 cm and 9 cm in length pineapple leaves.

Figure 9.2 Alkali digestion of size reduced pineapple leaves

e. Data and Results


Table 9.1 Determination of the Optimum Size of Pineapple Leaves

Parameter Trial 1 Trial 2 Trial 3


Mass of Pineapple Leaves (g) 150.00 150.00 150.00
Size 5 cm 7 cm 9cm
Amount of White Liquor (g) 450 450 450
Temperature () 100 100 100
Time (min) 60 60 60

Nitration of Pineapple Leaves for the Production of Pyroxylin Lacquer 21


Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

Mass of Dried Pulp (g) 75.05 85.52 80.49


Percent Yield (%) 65.17 74.27 69.90
Percent Mass Removed (%) 34.83 25.73 30.10

f. Calculations:
PERCENT YIELD:
150 g leaves (0.5775+0.1902) = 115.155 g of cellulose

=

Trial 1: 5cm
.
= .
.

Trial 2: 7cm

.
= .
.

Trial 3: 9cm

.
= .
.
g. Analysis
The optimum size for the pineapple leaves was determined through alkali
digestion. Based on the Table 9.1, more mass is removed when the size is shorter because
the leaves are completely soaked and exposed to the solution compared to the leaves with
longer length. Thus, the size of 5 centimeter was chosen to be the optimum size for
pineapple leaves.

Nitration of Pineapple Leaves for the Production of Pyroxylin Lacquer 22


Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

h. Conclusion

The optimum size for the pineapple leaves is 5 cm in length since it is completely
immersed in the liquor thus, yielding the highest percent of mass removed of 34.83%.

i. Equivalent Equipment
Laboratory Scale Plant Scale

Scissors Rotary Knife Cutter

B. Alkali Digestion Process of Pineapple Leaves


Pineapple leaves are digested in an alkali solution in order to obtain the cellulose which is
needed for the production of pyroxylin lacquer. The parameters such as the alkali reagent,
concentration of alkali reagent and ratio of alkali reagent to pineapple leaves are tested and the
remaining parameters and held constant.

B.1 Determination of the Optimum Alkali Reagent for Pulping


a. Apparatus and Materials

Pineapple Leaves Sodium Hydroxide


Vials Calcium Hydroxide
Thermometer Potassium Hydroxide
Stirring Rod Analytical Balance
Pipette Aspirator
1-L Beakers Hot Plate

b. Objective
To determine the optimum alkali reagent for alkali digestion

Nitration of Pineapple Leaves for the Production of Pyroxylin Lacquer 23


Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

c. Procedure
1. Weigh 150 g of pineapple leaves and place it in a 1-L beaker.
2. Pour10% concentration of NaOH solution in the beaker containing
pineapple leaves.
3. Heat the pineapple leaves until it reaches 100C and digest for 60 minutes
after boiling.
4. After digesting, let it cool for 10 minutes.
5. Separate the pulp from black liquor and wash the pulp with 1-L water.
6. Dry the washed pulp for 15 minutes at 100C.
7. Weigh the obtained pulp and record.
8. Repeat steps using saturated Ca(OH)2 solution and 13% KOH.

d. Data and Results


Table 9.2. Determination of the Optimum Alkali Reagent

Parameter Trial 1 Trial 2 Trial 3


Mass of Pineapple Leaves (g) 150 150 150
Alkali Reagent NaOH Ca(OH)2 KOH
Amount of White Liquor (g) 450 450 450
Temperature () 100 100 100
Time (min) 60 60 60
Mass of Dried Pulp (g) 75.05 Using calcium 74.37
hydroxide as
Percent Yield (%) 65.17 an alkali 64.58
reagent did not
digest the
pineapple
leaves. After
30 minutes of
Percent Mass Removed (%) 34.83 35.42
digesting, the
leaves are still
in its
rectangular
shape.

Nitration of Pineapple Leaves for the Production of Pyroxylin Lacquer 24


Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

Figure 9.3 Determination of Alkali Reagent. (L-R) KOH, NaOH, Ca(OH)2

e. Calculations:
150 g leaves (0.5775+0.1902) = 115.155 g of cellulose
PERCENT YIELD:

=

Trial 1: NaOH
.
= .
.

Trial 3: KOH
.
= .
.

f. Analysis
Table 9.2 shows that using Ca(OH)2 as an alkali reagent for alkali digesting is
ineffective. The pineapple leaves does not react well with Ca(OH)2 compared to the other
two being used and as a result, it does not change its rectangular shape as shown in
Figure 9.3. Between NaOH and KOH, the former is chosen because the difference in
percent mass removed between the two alkali reagents is 0.59 which is insignificant.

Nitration of Pineapple Leaves for the Production of Pyroxylin Lacquer 25


Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

g. Conclusion
The optimum alkali reagent for the alkali digestion process of pineapple leaves is
NaOH having the significant percent mass removed of 34.83%.

h. Equivalent Equipment

Laboratory Scale Plant Scale

Beaker Batch Reactor

B.2 Determination of the Concentration of Sodium Hydroxide Reagent (NaOH)


According to the Technical Association of the Pulp and Paper Industry (TAPPI),
the standard concentration of sodium hydroxide for alkali digestion is 10% w/w. From here,
the researchers varied the determination of concentration of sodium hydroxide to 7%, 10%
and 13% w/w.

a. Apparatus and Materials

Thermometer
1-L beaker

Sodium
hydroxide
Pineapple solution
leaves

Figure 9.4 Determination of Concentration of Sodium Hydroxide

Nitration of Pineapple Leaves for the Production of Pyroxylin Lacquer 26


Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

b. Objective
To determine the optimum concentration of sodium hydroxide

c. Hypothesis
The concentration of sodium hydroxide must be low in order to avoid cellulose
degradation

d. Procedure
1. Weigh 150 g of 5 cm in length pineapple leaves and place it in a 1-L
beaker.
2. On a separate beaker, dissolve 100 g of NaOH pellets in 1-L water to
produce 7% concentration. Carefully stir to dilute.
3. Mix the NaOH solution in the 1-L beaker containing pineapple leaves.
4. Heat the pineapple leaves until it reaches 100C. Cook it for 60 minutes
after boiling.
5. After digesting, let it cool for 10 minutes.
6. Separate the pulp from black liquor and wash the pulp with 1-L water.
7. Dry the washed pulp for 15 minutes at 100C.
8. Weigh the obtained pulp and record.
9. Repeat steps using 10% and 13% concentration of NaOH.

e. Data and Results


Table 9.3Determination of the Concentration of Sodium Hydroxide Reagent (NaOH)

Parameter Trial 1 Trial 2 Trial 3


Mass of Pineapple Leaves (g) 150 150 150
Concentration of NaOH (% w/w) 7 10 13
Amount of White Liquor (g) 450 450 450
Temperature () 100 100 100
Time (min) 60 60 60

Nitration of Pineapple Leaves for the Production of Pyroxylin Lacquer 27


Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

Mass of Dried Pulp (g) 79.70 75.05 68.67


Percent Yield (%) 69.21 65.17 59.63
Percent Mass Removed (%) 30.79 34.83 40.37

f. Calculations:
PERCENT YIELD:

Trial 1: 7%
.
= .
.

Trial 2: 10%
.
= .
.

Trial 3: 13%
.
= .
.

g.Analysis
After the alkali digestion process, the optimum alkali reagent concentration is
identified to be 10%. Table 9.3 shows that as the concentration of the alkali reagent
increases, the percentage of mass removed also increases. However, the mass of dried
pulp obtained in 13% concentration is much lower than 10%. Thus, the 10%
concentration which yield a percent mass removed of 34.83% and which is considered.

h. Conclusion
The optimum concentration of NaOH is 10% by weight which yield the second to
the highest percentage of mass removed of 34.83%.

Nitration of Pineapple Leaves for the Production of Pyroxylin Lacquer 28


Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

i. Equivalent Equipment

Laboratory Scale Plant Scale

Beaker Batch Reactor

B.3 Determination of the Ratio of Alkali Reagent to Raw Material

The determination of ratio of alkali reagent to pineapple leaves is set to be 2.5:1, 3:1,
and 4:1. The researchers based the variation of ratio from the study Pulp and Paper
Production from Nigerian Pineapple Leaves and Corn Straw as Substitute to Wood
Source(Aremu et al., 2015)wherein the ratio of the alkali reagent to pineapple leaves is 3:1.
The lower range must be 2:1 for consistency. However, the use of such ratio do not fully
immerse the pineapple leaves into the solution, thus, having 2.5:1 as an option.

a. Apparatus and Materials

thermometer

1-L beaker

Figure 9.5 Determination of the Ratio of Liquor to Raw Material

b. Objective
To determine to appropriate ratio of the liquor to the pineapple leaves
c. Procedure
1. Weigh 150 g of 5 cm in length pineapple leaves and place it in a 1-L
beaker.

Nitration of Pineapple Leaves for the Production of Pyroxylin Lacquer 29


Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

2. Mix 375 g of 10% NaOH solution in the 1-L beaker containing pineapple
leaves.
3. Heat the pineapple leaves until it reaches 100C. Cook it for 60 minutes
after boiling.
4. After digesting, let it cool for 10 minutes.
5. Separate the pulp from black liquor and wash the pulp with 1-L water.
6. Dry the washed pulp for 15 minutes at 100C.
7. Weigh the obtained pulp and record.
8. Repeat steps using 450 g and 600 g amount of 10% NaOH solution.

d. Data and Results


Table 9.4 Determination of the Ratio of Liquor to Raw Material

Ratio of NaOH to Pineapple Leaves


Parameter 2.5:1 3:1 4:1
Mass of Pineapple Leaves (g) 150 150 150
Concentration of NaOH (% w/w) 10 10 10
Amount of White Liquor (g) 375 450 600
Temperature () 100 100 100
Time (min) 60 60 60
Mass of Dried Pulp (g) 75.24 75.05 53.50
Percent Yield (%) 65.34 65.17 46.46
Percent Mass Removed (%) 34.66 34.82 53.54

e. Calculations:

PERCENT YIELD:

=

Trial 1: 7%

Nitration of Pineapple Leaves for the Production of Pyroxylin Lacquer 30


Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

.
= .
.

Trial 2: 10%
.
= .
.

Trial 3: 13%
.
= .
.
f. Analysis
150 grams of feed is digested using different ratio of alkali reagent specifically
2.5:1, 3:1, and 4:1. Setting all other parameters constant except for the ratio of the alkali
reagent, the best ratio is determined. As shown in Table 9.4, there is a small increment
between 2.5:1 and 3:1 ratios that is why the former is considered to be the optimum ratio.
g. Conclusion
The optimum ratio of the alkali reagent to the pineapple leaves is determined to be
2.5:1.
h. Equivalent Equipment

Laboratory Scale Plant Scale

Beaker Batch Reactor

Table 9.6Summary of Parameter for Alkali Digestion

SUMMARY OF PARAMETERS FOR ALKALI DIGESTION


Amount of Initial Mass 150 g
Size of Pineapple Leaves 5 cm
Concentration of NaOH 10%
Ratio of NaOH Soln. to Pineapple leaves 2.5:1
Amount of White Liquor 375g
Temperature for Digesting 100
Time for Digesting 60 min

Nitration of Pineapple Leaves for the Production of Pyroxylin Lacquer 31


Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

C. Nitration
Nitration is a broad class of chemical process for the introduction of a nitro group into an

organic chemical compound (Booth, 2012). As reported by Pharmacopeia, pyroxylin lacquer

contains not less than 5.0% and not more than 14%, by weight, of pyroxylin. Ether to alcohol

ratio is 3:1. Moreover, according to Professor Steve Dessens of Houston Community College,

mixing only a few milliliters of concentratedH2SO4and HNO3, the amount of heat released will

not be so great, so a water bath at room temperature is normally adequate to ensure that

overheating does not occur. You can even do the mixing in a small graduated cylinder with no

water bath. But larger volumes are often mixed at ice bath temperatures just to be on the safe

side.

a. Apparatus and Materials

b. Procedure
1. Mix 40 ml of 63% Nitric Acid and 120 ml of 94% Sulfuric Acid in a
beaker.
2. Place the beaker in a water bath full of ice. Stir the mixture until it reaches
0C.
3. Weigh 40 g of cellulose pulp and mix it with the nitric and sulfuric acid
solution in the beaker.

Nitration of Pineapple Leaves for the Production of Pyroxylin Lacquer 32


Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

4. Stir the slurry for 10 minutes to provide time for the reaction to produce
nitrocellulose.
5. Separate the filter cake containing the nitrocellulose from the mixture.
6. Soak the filter cake with 500 mL of water for 5 minutes.
7. Neutralize the nitrocellulose pulp by soaking the washed pulp to a 10%
sodium bicarbonate solution for 5 minutes. Gradually stir.
8. Filter the pulp from the solution then, flatten it in a filter paper pressing it
with another filter paper above to remove excess moisture.
9. Blow dry it with cool air for 10 minutes.
10. Using the flammability test, ignite the pulp with fire to prove if it is a
nitrocellulose. If the pulp ignites rapidly and leaves no residue, then it is a
nitrocellulose.
11. Another testing is to dissolve the solution with petroleum ether and
ethanol. Dissolve the 10 g of nitrocellulose with 10g of petroleum ether
and 30g of ethanol.
12. Repeat steps except procedure no. 2.

c. Data and Results


Table 9.7 Nitration Process

Parameter Trial 1 Trial 2


Pulp (g) 40 40
Ratio of Sulfuric Acid to Nitric Acid 3:1 3:1
Temperature () 80 0
Time (min) 30 30
Mass of Dried Pulp (g) 2 27
Percent Yield (%) 5.00 67.5

Nitration of Pineapple Leaves for the Production of Pyroxylin Lacquer 33


Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

d. Calculations:

PERCENT YIELD:

=

Trial 1: 7%

= %

Trial 2: 10%

= . %

e. Analysis
On table 9.7, trial 2 was chosen against trial 1 since the percent yield is much higher
which amounts to 67.5 percent. Also, the yielded dried pulp is higher compared to trial 1
which has only 2 grams of dried pulp. Temperature difference also plays an effect on the
yielded pulp, the lower the temperature the higher the percent yield.

f. Conclusion
The optimum parameter for the Nitration process is 3:1 of sulfuric to nitric acid at 0 C.

D. Neutralization
The reaction of acids with sodium bicarbonate is a common method for neutralizing
acid spills. The advantage to this method is that one can use excess sodium carbonate, which
is relatively innocuous. The neutralization process is signaled by the release of gaseous
CO2The sodium bicarbonate is an alkali and will neutralize much of the acid remaining
(Powell, 2009).
a. Apparatus and Materials
Cellulose Pulp Nitric Acid
Ice Beakers

Nitration of Pineapple Leaves for the Production of Pyroxylin Lacquer 34


Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

Thermometer Vials
Stirring Rod Analytical Balance
Pipette Aspirator
pH paper Sodium Bicarbonate
Sulfuric Acid Water Bath

b. Procedure
1. Mix 40 ml of 63% Nitric Acid and 120 ml of 94% Sulfuric Acid in a beaker.
2. Place the beaker in a water bath full of ice. Stir the mixture until it reaches 0C.
3. Weigh 40 g of cellulose pulp and mix it with the nitric and sulfuric acid solution
in the beaker.
4. Stir the slurry for 10 minutes to provide time for the reaction to produce
nitrocellulose.
5. Separate the filter cake containing the nitrocellulose from the mixture.
6. Soak the filter cake with 500 mL of water for 5 minutes.
7. Neutralize the nitrocellulose pulp by soaking the washed pulp to a 10% sodium
bicarbonate solution for 5 minutes. Gradually stir.
8. Test the pH of the solution using pH paper. The result should have a pH of 7.
9. Filter the pulp from the solution then, flatten it in a filter paper pressing it with
another filter paper above to remove excess moisture.
10. Blow dry it with cool air for 10 minutes.
11. Using the flammability test, ignite the pulp with fire to prove if it is a
nitrocellulose. If the pulp ignites rapidly and leaves no residue, then it is a
nitrocellulose.
12. Another testing is to dissolve the solution with petroleum ether and ethanol.
Dissolve the 10 g of nitrocellulose with 10g of petroleum ether and 30g of
ethanol.

Nitration of Pineapple Leaves for the Production of Pyroxylin Lacquer 35


Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

c. Data and Results


Table 9.8 Neutralization Process

Parameter Trial 2
Pulp (g) 40
Ratio of Sulfuric Acid to Nitric Acid 3:1
NaHCO3 Concentration(%w/w) 10
pH 7
Temperature () 0
Time (min) 30
Mass of Dried Pulp (g) 27
Percent Yield (%) 67.5

d. Calculations:

PERCENT YIELD:

=

Trial 1: 7%

= . %

e. Conclusion
After the nitration process, the cellulose obtained must undergo a neutralization
process. The cellulose is emerged in a bicarbonate solution which will neutralize the
remaining acid.

Nitration of Pineapple Leaves for the Production of Pyroxylin Lacquer 36


Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

h. Equivalent Equipment

Laboratory Scale Plant Scale

Beaker with stirrer Neutralization (Mixing) Tank

E. Dissolution
According to Henriette Kress on her online book called Practical Herbs 2, Pyroxylin

consists of dinitro-cellulose, C6H8(NO2)2O5 which is soluble in a mixture of alcohol and

ether. Alcohol is commonly used in the dissolving nitrocellulose. Ethanol and Petroleum

ether were used as solvents which are forms of alcohol and ether.

a. Apparatus and Materials


Nitrocellulose Pulp Petroleum Ether
Vials Beakers
Stirring Rod Analytical Balance
Pipette Aspirator
Ethanol

b. Procedure
1. Weigh 10 g of nitrocellulose pulp.
2. Mix 10 g of petroleum ether to 30 g of ethanol. Stir.
3. Dissolve the nitrocellulose pulp to the mixture of petroleum ether and ethanol.
Stir the mixture for 30 min.
4. Filter the unreacted pulp.

Nitration of Pineapple Leaves for the Production of Pyroxylin Lacquer 37


Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

c. Data and Results


Table 9.9 Dissolution Process

Parameter Trial 2
Nitrocellulose Pulp (g) 10
Ratio of Alcohol to Ether 1:3
Unreacted pulp (g) 2
Time (min) 30

e. Analysis
After the neutralization process, the neutralized nitro cellulose will now be
dissolved in a 3:1 ratio of alcohol to ether.

Table 9.10. Summary of Parameters for Nitration, Neutralization and Dissolution

Nitration of Pineapple Leaves for the Production of Pyroxylin Lacquer 38


Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

PROCESS FLOWCHART

Nitration of Pineapple Leaves for the Production of Pyroxylin Lacquer 39


Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

Nitration of Pineapple Leaves for the Production of Pyroxylin Lacquer 40


Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

CONCLUSION

Nitration of Pineapple Leaves for the Production of Pyroxylin Lacquer 41


Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

RECOMMENDATION

The researchers recommend the future scholars to vary the other parameters in the

experimental method specifically, the time and temperature which is essential in the alkali

digestion. Also, vary the parameters for the nitration, neutralization and dissolution process. The

future researchers may also use analytical grade of chemicals to provide best results of the

experiment.

Moreover, other regions having vast pineapple production may become a source of raw

material. Varieties of pineapple plant may be tested to determine the best raw material to acquire

cellulose. Other agriculture products having high cellulose content may be utilized to produce

pyroxylin lacquer.

Besides comparing the cellulose content with other studies, testing of the properties of the

pineapple leaves may be done for the verification of the cellulose content. The researchers also

recommend the testing for the cellulose, nitrocellulose and pyroxylin lacquer.

Additionally, find and test other properties of pyroxylin lacquer. FTIR spectrum analysis

may be replaced with other kind of spectrum analysis. A thorough research is recommended for

the gathering of local standard and existing properties of pyroxylin lacquer.

Lastly, cautiousness and alertness should be embodied by the future researchers because

of the nature of the chemicals used in the experiment. Usage of personal protective gears should

be used because high corrosive chemicals and toxic fumes are concerned. Proper waste disposal

of the by-products should be applied.

Nitration of Pineapple Leaves for the Production of Pyroxylin Lacquer 42


Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

REFERENCES

[1] McMurry, J. (2007). Organic Chemistry 2nd. Edition

[2] Wiley, VCH (2012). Ullmann's Encyclopedia of Industrial Chemistry

[3] Hassam, D.M. (2013). Role of TFNet in Promoting Global Pineapple


Industries:Sarawak Perspective. Retrieved March 20, 2016 from
http://www.mpib.gov.my/documents/10124/531591/ROLE+OF+TFNET+IN+PROMOTI
NG+GLOBAL+PINEAPPLE+INDUSTRIES+SARAWAK+PRESPECTIVE+(TFNET+-
+DR+MOHD+DESA+BIN+HJ.+HASSIM).pdf
[4] Zumdahl, S.S. (2009). Chemical Principles 6th Ed. Houghton Mifflin Company. p.
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[5]("sulfuric acid". The Columbia Encyclopedia (6th ed.). 2009. Retrieved 2010-03-16.)

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[8] Fitzgerald, B. Pia Couture: Pineapple Fiber Fabric in the Philippines retrieved
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couture-pineapple-fiber-makes-fabric-in-the-philippines)

[9] Lacquer, Department of Trade and Industry, retrieved February 30, 2016 from
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[10] Manalo, J. B., Boyles, A., Ambal, W. O., & Estrella, R. R. (1992). PRODUCTION

OF XYLITOLFROM SUGAR CANE BAGASSE. The Philippine Journal of Science,

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Nitration of Pineapple Leaves for the Production of Pyroxylin Lacquer 43


Pamantasan ng Lungsod ng Maynila
College of Engineering and Technology
Department of Chemical Engineering

[11]Department of Science and Technology. (2010). The Philippine recommends for

pineapple (2nd ed., Vol. XXI, p. 143). Los Baos, Laguna: PCARRD-DOST.

M. Asim, KhalinaAbdan, M. Jawaid, et al., A Review on Pineapple Leaves Fibre

and Its Composites,International Journal of Polymer Science, vol. 2015, Article

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[12] Tejano, E. A. (december 1985). State of the Art of Coconut Coir Dust and

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[14] Aremu, M., Rafiu, M., &Adedeji, K., (2015).Pulp and paper production from
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[16] Powell, W., (2009). Sodium Bicarbonate Solution retrieved April 4, 2016 from
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Nitration of Pineapple Leaves for the Production of Pyroxylin Lacquer 44

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