Methodology and Data Presentation: Pamantasan NG Lungsod NG Maynila

PAMANTASAN NG LUNGSOD NG MAYNILA
College of Engineering and Technology

Chemical Engineering Department
CHAPTER 3
METHODOLOGY AND
DATA PRESENTATION
Production of Viscose Film via Xanthation of Alkali Hydrolyzed Pineapple

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(Ananas comosus) Crown Leaves and Corn (Zea mays) Cobs
METHODS OF RESEARCH
The researchers gathered the data regarding the properties of the raw material
and its availability, product’s characteristics and specifications in the market, its market
viability, and the experimental procedures and manufacturing processes involved.
Descriptive and experimental methods are used as the methodology.
Descriptive Method
The researchers gathered the data from different government institutions for the
recent information and statistical data available for the raw material and the product,
Viscose Film.
 Science Direct
Books, theses, and other studies helped the researchers to come up with
the idea of producing Viscose Film from Pineapple Crown Leaves and Corncobs.
 Philippine Statistics Authority (PSA)– Quezon Avenue

Provided the data on the production of Pineapple Crown Leaves and
Corncobs and the amount of importation, exportation and local production of
Viscose Film including its substitute products in the Philippines.

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Experimental Method
The experimental method is the scientific undertaking of the research. In here,

laboratory setup for experimentations is done. Different parameters are considered to
come up with the best quality of our product.
 Pamantasan ng Lungsod ng Maynila (PLM) Medicine Laboratory

Experiments were carried out in this laboratory.
 Adamson University Technology Research and Development Center

(AUTRDC)
Properties (such as moisture content and alpha-cellulose) of raw materials
were carried out in this testing center.
 De La Salle University (DLSU) Chemistry Instrument and Research

FTIR of alkali cellulose, alkali cellulose xanthate, viscose solution and
viscose film were carried out in this university testing center. Also, UV-VIS of alkali
cellulose, alkali cellulose xanthate, and viscose solution are also performed.
 Department of Science and Technology – Industrial Technology

Development Institute (DOST – ITDI)
Physical Properties of Viscose Film were carried out in this testing center.

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CONCEPTUAL FRAMEWORK
Figure 3.1: Conceptual Framework of the Study

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ANALYSIS OF CONCEPTUAL FRAMEWORK
The conceptual framework structures the research scope. It presents the overview
of the research study and it includes the methods applied to provide direction in achieving
the research objectives.
The first step is the collection of data needed for the research study. Data are
gathered from different government institutions, journals, researches, books, and internet
to get the most recent studies and information available locally and internationally. Such
information serves as the foundation and basis of the literature used in the study.
In the market study, the proponents investigate regarding the marketability of the
product which includes an analysis of the demand and supply. These help the
researchers in determining the market feasibility of the said product by projecting the
demand and supply using different statistical projections. The projected demand and
supply are used in determining the market share and plant rated capacity. Furthermore,
various marketing, promotional strategies, and distribution channels are developed to
determine how the product would penetrate the market. As the project was proven to be
feasible, the proponents proceeded to the experimental study.
Set of experiments for parameter variations are considered in fulfilling this study.
Experimentation is conducted on a laboratory scale and the values acquired during the
actual experimentation are scaled-up to design a manufacturing plant which includes the
design of equipment, storage and transport utilities, piping system, and instrumentation
and process control. These constitute the technical part of the study.
The completion of the market study, experimental study, and technical study would
establish the feasibility of the study.

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THEORETICAL FRAMEWORK
Figure 3.2: Theoretical Framework of the Study

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ANALYSIS OF THEORETICAL FRAMEWORK
In this study, there are four major parts that were processed and distinguished the
independent and dependent (experimental variations) variables. The parts are the
production of alkali cellulose, production of cellulose xanthate, production viscose
solution, and film forming.
For the extraction of the cellulose, called alkali cellulose, alkaline hydrolysis is the
ideal process based from related literature. The size of raw materials was the first
variation for the hydrolysis process. The pineapple crown leaves and corn cobs were cut.
The cutting time for the size reduction is the independent variable that yield homogeneous
particle size and length, which is the dependent variable. This is followed by the ratio of
raw materials. Since pineapple crown leaves and corncobs have different alpha-cellulose
content, it is necessary to determine the appropriate ratio for the process. This is followed
by type of the alkali. The common bases used are sodium hydroxide (NaOH) and
potassium hydroxide (KOH). After determining the type of alkali solution; the next
variation for the process were the: the concentration of the alkali solution, ratio of raw
material to alkali solution, temperature ranging from 30 to 50C, and time from 60 to 180
minutes. The parameters that are chosen based on the percent alkali cellulose yield and
percent impurities removed.
After producing the alkali cellulose, it is converted to cellulose xanthate through

xanthation. Carbon Disulfide will be used as the reagent based on the related literature.
The optimum parameters for the ratio of raw material to that of the carbon disulfide,
temperature and time are to be found using One-factor-at-a-time setup.
The obtained cellulose xanthate is the converted to viscose solution by alkalization.

One-factor-at-a-time setup is used as the choice of optimization for time, and
concentration of reagent. The type of reagent will be based from the related literature.
Lastly, the viscose solution is formed and plasticized. Some parameters are
optimized. These are the concentration of the acid used, time of plasticizing and,
temperature and time in drying the sheet. The type of plasticizer and bleaching agent to
be used is based from the related literature.

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SUMMARY OF VARIATION PARAMETERS
Table 3.1: Summary of Variation Parameters
OPTIMUM (BASED
PROCESS PARAMETER VARIATIONS
ON STUDIES)
5, 10, 20, 30, 40
PCL Length 30 mm
mm.
Corncobs Particle 1.18, 2.36, 4.75,
< 10 mm
Diameter 9.5 mm.
30, 60, 90, 120,
Alkaline Time 60 mins.
150, 180 min
Hydrolysis
30, 40, 50, 60,
Temperature 30 C
70C
NaOH, KOH,
Reagent NaOH
Ca(OH)2
Concentration 18 wt% 15, 18, 21%
30, 60, 90, 120,
Time 120 mins.
150, 180 min
Xanthation
Ratio to Raw 25, 30, 35, 40, 45%
25-35 %
Material grams of sample
Concentration 5% 3, 5, 7, 9, 11%
Alkalization 30, 60, 90, 120,
Time 120-180 mins.
150, 180 min
30, 60, 90, 120,
960 – 1440 mins.
Ageing Time 150, 180, 210, 240
(16-24 hrs.)
min
12, 16, 20, 24, 28%
Casting Concentration 12 %
H2SO4
Table 3.1 shows the parameters that were extracted from various studies
that will be used and evaluated in the experimental process for the production of
Viscose Film from Pineapple Crown Leaves and Corncobs.

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EXPERIMENTAL
STUDY

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EXPERIMENTAL METHOD
The researchers devised an experimental method to obtain Viscose Film from

Pineapple Crown Leaves and Corncobs. Laboratory set-up for experimentations was
prepared and various parameters were considered to come up with the most suitable
operating conditions and best quality of the product. Several principles and findings from
various literatures and studies were incorporated in the experimental method to suit the
properties of the raw material and the working environment.
The analysis of Pineapple Crown Leaves and Corncobs to determine its chemical
composition was carried out in Adamson University Technology Research and
Development Center (AUTRDC). The experimental method consists of four major parts:
(1) preparation/conditioning of raw materials which involves size reduction, and alkaline
hydrolysis; (2) Xanthation which forms the alkali cellulose xanthate; (3) Alkalization which
forms the viscose solution and involves ripening to prepare the viscose solution for
casting; and (4) Casting. The best trial will be chosen from the results that will be obtained
in each part of the experiment. The results will be supported by either qualitative or
quantitative testing, or analysis to ensure their validity. Furthermore, the obtained
experimental results will be used for the upscale production of Viscose Film.

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OBJECTIVES OF THE EXPERIMENTAL STUDY
General Objective
The main objective of the experimental study is to produce a high yield of viscose
film with properties that will conform to the following commercial standards:
Table 3.2: Properties of the Standard, and Existing Properties Viscose Film
Property Standard(a) Existing(b) Produced

Tensile Strength 8 - 20 MPa(i) 10 MPa (g) 10.263
(MPa)
Elongation at Break 10-50 (f) 18 (g) 22.99
(%)
Water Absorption for 50% (equilibrium) 45-115%(c) 114.60%
24 hours
Thickness 21.0 – 42.0 27.7 – 34.7 0.0358 mm = 35.8
microns (g) microns microns
Density 1.50 – 1.55 g/cm3 1.50 – 1.52 g/cm3 1.52 g/ cm3
(d) (c)
Appearance Transparent Transparent to Translucent

Translucent
FT-IR Analysis C-C Ring Breathing Band at 1155cm-1Wavelength peak
C-O-C Glycoside Ether at 1105 cm-1 (h)
at 1155 cm-1 and
1105 cm-1
UV-VIS Analysis Alkali cellulose xanthate below 250 Wavelength peak
nm; and between 280 and 370 nm at 236 nm and
wavelength (e) 305 nm
Source: (a) Film Properties of Plastics and Elastomers, 2nd Edition. Laurence W.
McKeen, Liesl K. Maey, (b) Uncoated Regenerated Cellulose Film, (c) Cellulose
(Regenerated Cellulose) Material Information, (d) Physico-mechanical properties of
materials (cellophane), (e) “A Real-Time Technique for Monitoring Cellulose Dissolution
during the Xanthation Process” by He, L. et al, (f) Polymer Chemistry, 2000. Mechanical
Property. Dr. Whisnant, D., (g) MatWeb LLC Material Property Data. Goodfellow
Cellophane, Rayophane Regenerated Cellulose Film, and (h) “Fourier Transform Infrared
Spectroscopy for Natural Fibres”, by Fan,M. et al.

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Specific Objectives
 To determine the optimum operating conditions in the alkaline hydrolysis,

xanthation, alkalization and casting using One-Factor-at-a-Time Method which
would result to the highest significant percent conversion of viscose film from
pineapple crown leaves and corncobs
 To determine the properties of the chemical intermediates using physical,

chemical, or mechanical tests, ATR-FTIR spectroscopy, UV-Visible Spectroscopy,
and gravimetric analysis that would verify whether the target substances were
produced along the process
 To calculate the percent yield in each laboratory process in order to determine the
overall process yield
 To identify the equivalent unit operations or unit processes and industrial

equipment for every laboratory procedures and apparatuses applied in the
experiment

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EXPERIMENTAL PROCESS FLOW DIAGRAM
The experimental process flow diagram depicting the involved unit operations and
unit processes in the study is presented in the figure below:
Figure 3.3: Experimental Process Flow Diagram of the Study

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LIST OF REQUIRED REAGENTS AND LABORATORY APPARATUSES
The reagents to be used, as well as the laboratory apparatuses necessary for each
experimental process, were summarized in Table 3.2. The chemicals were purchased
from Patagonian Enterprises in Sta. Cruz, Manila and from Alysons’ Chemical
Enterprises, Inc. in Araneta Avenue, Quezon City.
Table 3.3: List of Required Reagents and Laboratory Apparatuses
Process Required Reagents Laboratory

Reagent Function Apparatuses
Shears, Beaker, Tyler Mesh, and
Cutting - -
Analytical Balance
Sodium Hydroxide Alkali Reactant Beaker, Hot Plate, Cheesecloth,
Alkaline Strainer, Thermometer,
Potassium Hydroxide Alkali Reactant
Hydrolysis Analytical Balance, and
Calcium Hydroxide Alkali Reactant Stopwatch
Beaker, Hot Plate, Stirring Rod,
Xanthating
Xanthation Carbon Disulfide Thermometer, Analytical
Agent
Balance, and Stopwatch
Beaker, Thermometer, Analytical
Alkalization Sodium Hydroxide Alkali Reactant
Balance, and Stopwatch
Glass Slide, Glass Tray, Tongs,
Casting Sulfuric Acid Acid Reactant Stopwatch, Beaker and
Analytical Balance
Beaker, Hot plate, Tongs,
Hot water Washing
Water Analytical Balance, and
Washing Medium
Stopwatch
Ceramic Tray, Beaker, Tongs,
Bleaching Sodium Hypochlorite Bleaching Agent Analytical Balance and
Stopwatch
Washing
Washing Water Analytical Balance, and
Medium
Stopwatch
Plasticizing
Plasticizing Glycerol Analytical Balance, and
Agent
Stopwatch
Drying - - Oven and Stopwatch

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PREPARATION OF RAW MATERIALS AND REAGENTS
I. RAW MATERIAL
The pineapple crown leaves were collected from Silang, Cavite while the
corncobs were collected from Carmona, Cavite.
Xanthation
Figure 3.4: Pineapple Crown Leaves and Corncobs to Viscose Film via Xanthation
Prior to the experimentation of the pineapple crown leaves and corncobs,

the cellulose content, and bulk density were determined. These properties are
important in the determination of the optimum parameters in the pretreatment
process and alkaline hydrolysis.
A. Cellulose Content
The researchers went to the Adamson University Technology Research and

Development Center (AUTRDC) for the testing of the cellulose content of the
raw materials. Titration (dry weight) for the determination of alpha-cellulose
content.

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Table 3.4: Alpha-Cellulose Content of the Raw Materials
Raw Material %α-cellulose

Pineapple Crown Leaves 83.77%
Corncobs 48.79%
Source: Adamson University Technology Research and Development Center
(AUTRDC), 2017
Analysis: The results of the testing showed that the alpha-cellulose content is
83.77% which falls within the range of 70-85% reported by Carus (2011) and
Verma et al. (2013). On the other hand, the alpha-cellulose content is 48.79%
which is slightly higher than the 38-44% as suggested by different literatures.
B. Determination of the Bulk Density
Bulk density is the mass of the particles divided by the volume they occupy
that includes the space between the particles (ASTM D5004, 2001). In solving
for the bulk density, use the equation:
𝑚𝑎𝑠𝑠 𝑜𝑓 𝑠𝑎𝑚𝑝𝑙𝑒 (𝑔) 𝑊𝑠
𝜌𝑏 = =
𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑐𝑜𝑛𝑡𝑎𝑖𝑛𝑒𝑟 (𝑚𝐿) 𝑉
1. Materials and Apparatuses

Pineapple Crown Leaves Corncobs
1000mL Graduated Cylinder Analytical Balance 1000ml Beaker
2. Objective
To obtain the average bulk density of pineapple crown leaves and
corncobs.
3. Procedure
3.1 For Pineapple Crown Leaves
3.1.1 Prepare 5 sets of 10 pieces pineapple crown leaves.

3.1.2 Weigh and record the mass of each set of pineapple crown leaves.
3.1.3 Fill the graduated cylinder with 600 mL of water.
3.1.4 Submerge one set of pineapple crown leaves in the graduated
cylinder, and record the change in water volume.

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3.1.5 Repeat step 3.1.4 for the other four sets then calculate the average
bulk density.
3.2 For Corncobs

3.2.1 Prepare 5 sets of 2 pieces corncobs.
3.2.2 Weigh and record the mass of each set corncobs.
3.2.3 Fill the graduated cylinder with 500 mL of water.
3.2.4 Submerge one set of corncobs in the graduated cylinder, and
record the change in water volume.
3.2.5 Repeat step 3.2.4 for the other four sets then calculate the
average bulk density.
4. Data and Calculation
Table 3.5: Bulk Density of Pineapple Crown Leaves
Trial Mass (g) Change in Volume (mL) Bulk Density (g/mL)

1 16.88 20 0.844
2 16.78 16 1.049
3 12.81 15 0.854
4 16.63 18 0.924
5 18.34 23 0.797
Average Bulk Density 0.894
Sample Calculation:
𝑀𝑎𝑠𝑠 𝑜𝑓 𝑃𝐶𝐿 (𝑔)

𝜌𝑏 =
𝐶ℎ𝑎𝑛𝑔𝑒 𝑖𝑛 𝑊𝑎𝑡𝑒𝑟 𝑉𝑜𝑙𝑢𝑚𝑒 (𝑚𝐿)
16.88 𝑔𝑟𝑎𝑚𝑠 𝐠
𝜌𝑏 = = 𝟎. 𝟖𝟒𝟒
20 𝑚𝐿 𝐦𝐋
(0.844 + 1.049 + 0.854 + 0.924 + 0.797) 𝑔/𝑚𝐿

𝐴𝑣𝑒. 𝜌𝑏 =
5
𝐴𝑣𝑒. 𝜌𝑏 = 𝟎. 𝟖𝟗𝟒 𝒈/𝒎𝑳

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Table 3.6: Bulk Density of Corncobs

1 72.52 119 0.609
2 55.30 90 0.614
3 53.63 95 0.565
4 58.58 95 0.617
5 51.43 95 0.541
Average Bulk Density 0.589
Sample Calculation:
For Trial 1:
𝑀𝑎𝑠𝑠 𝑜𝑓 𝐶𝑜𝑟𝑛𝑐𝑜𝑏𝑠 (𝑔)

𝜌𝑏 =
𝐶ℎ𝑎𝑛𝑔𝑒 𝑖𝑛 𝑊𝑎𝑡𝑒𝑟 𝑉𝑜𝑙𝑢𝑚𝑒 (𝑚𝐿)
72.52 𝑔𝑟𝑎𝑚𝑠 𝒈
𝜌𝑏 = = 𝟎. 𝟔𝟎𝟗
119 𝑚𝐿 𝒎𝑳
(0.609 + 0.614 + 0.565 + 0.617 + 0.541) 𝑔/𝑚𝐿

𝐴𝑣𝑒. 𝜌𝑏 =
5
𝐴𝑣𝑒. 𝜌𝑏 = 𝟎. 𝟓𝟖𝟗 𝒈/𝒎𝑳
5. Conclusion
The average bulk density of pineapple crown leaves and corncobs are
0.894 g/mL and 0.589 g/mL, respectively.

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II. MINOR RAW MATERIALS
In order for the experiment to proceed, below are the list of reagents that are
needed along the process.
Table 3.7: List of Minor Raw Materials
REAGENT PURPOSE
Sodium Hydroxide Reactant for Alkali Hydrolysis and
Alkalization
Potassium Hydroxide Reactant for Alkali Hydrolysis
Calcium Hydroxide Reactant for Alkali Hydrolysis
Carbon Disulfide Reactant for Xanthation
Sulfuric Acid Acid for Casting
Sodium Hypochlorite Reagent for Bleaching
Glycerol Reagent for Plasticizing

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EXPERIMENTAL PROCEDURE
I. ALKALINE HYDROLYSIS
Alkaline hydrolysis has been used to separate cellular components with
high lignin solubilization, hemicellulose removal and effective cellulose swelling
(Lee et al., 2014). It uses strong alkali solvent.
The figure below depicts the chemical reaction involved during the alkaline
hydrolysis:
𝐶𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒 + 𝐴𝑙𝑘𝑎𝑙𝑖 → 𝐴𝑙𝑘𝑎𝑙𝑖 𝐶𝑒𝑙𝑙𝑢𝑜𝑠𝑒 + 𝐻2 𝑂

𝐶6 𝐻9 𝑂4 𝑂𝐻 + 𝑋𝑂𝐻 → 𝐶6 𝐻9 𝑂4 𝑂𝑋 + 𝐻2 𝑂
Where X = Na+, K+, or Ca2+
Figure 3.5: Separation of Lignocellulosic Components
The maximum theoretical amount of alkali cellulose that can be obtained was
computed as follows:
For Pineapple Crown Leaves (PCL):
𝒎𝒕𝒉𝒆𝒐𝒓𝒆𝒕𝒊𝒄𝒂𝒍 𝒂𝒍𝒌𝒂𝒍𝒊 𝒄𝒆𝒍𝒍𝒖𝒍𝒐𝒔𝒆
𝟏 𝟏 𝒎𝒐𝒍𝒆 𝒂𝒍𝒌𝒂𝒍𝒊 𝒄𝒆𝒍𝒍𝒖𝒍𝒐𝒔𝒆
= 𝒎𝒕𝒉𝒆𝒐𝒓𝒆𝒕𝒊𝒄𝒂𝒍 ∝−𝒄𝒆𝒍𝒍𝒖𝒍𝒐𝒔𝒆 ( )( ) (𝑴𝑾𝒂𝒍𝒌𝒂𝒍𝒊 𝒄𝒆𝒍𝒍𝒖𝒍𝒐𝒔𝒆)
𝑴𝑾𝜶−𝒄𝒆𝒍𝒍𝒖𝒍𝒐𝒔𝒆 𝟏 𝒎𝒐𝒍𝒆 ∝ −𝒄𝒆𝒍𝒍𝒖𝒍𝒐𝒔𝒆
𝑚𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 ∝−𝑐𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒 = % 𝛼 − 𝑐𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒 𝑖𝑛 𝑃𝐶𝐿 ∗ 𝑚𝑃𝐶𝐿
𝑚𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 ∝−𝑐𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒 = 0.8377 ∗ 500 𝑔 = 𝟒𝟏𝟖. 𝟖𝟓 𝒈
𝑚𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑎𝑙𝑘𝑎𝑙𝑖 𝑐𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒 = 418.85 𝑔 𝑥
1 𝑚𝑜𝑙𝑒 ∝ −𝑐𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒
∝ −𝑐𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒 ×
162.16 𝑔 ∝ −𝑐𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒
1 𝑚𝑜𝑙𝑒 𝑎𝑙𝑘𝑎𝑙𝑖 𝑐𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒 184.14 𝑔 𝑎𝑙𝑘𝑎𝑙𝑖 𝑐𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒
× ×
1 𝑚𝑜𝑙𝑒 ∝ −𝑐𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒 1 𝑚𝑜𝑙𝑒 𝑜𝑓 𝑎𝑙𝑘𝑎𝑙𝑖 𝑐𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒
𝒎𝒕𝒉𝒆𝒐𝒓𝒆𝒕𝒊𝒄𝒂𝒍 𝒂𝒍𝒌𝒂𝒍𝒊 𝒄𝒆𝒍𝒍𝒖𝒍𝒐𝒔𝒆 = 𝟒𝟕𝟓. 𝟔𝟐 𝒈
For Corncobs (CC):
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𝑚𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 ∝−𝑐𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒 = % 𝛼 − 𝑐𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒 𝑖𝑛 𝐶𝐶 ∗ 𝑚 𝐶𝐶

𝑚𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 ∝−𝑐𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒 = 0.4879 ∗ 500 𝑔 = 𝟐𝟒𝟑. 𝟗𝟓 𝒈
× ×
𝒎𝒕𝒉𝒆𝒐𝒓𝒆𝒕𝒊𝒄𝒂𝒍 𝒂𝒍𝒌𝒂𝒍𝒊 𝒄𝒆𝒍𝒍𝒖𝒍𝒐𝒔𝒆 = 𝟐𝟕𝟕. 𝟎𝟐 𝒈
For combination of Corncobs (CC) with Pineapple Crown Leaves (PCL):
𝑚𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 ∝−𝑐𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒
= % 𝛼 − ((𝑐𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒 𝑖𝑛 𝐶𝐶 ∗ 𝑚 𝐶𝐶 ) + (𝑐𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒 𝑖𝑛 𝑃𝐶𝐿 ∗ 𝑚𝑃𝐶𝐿))
𝑚𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 ∝−𝑐𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒 = ( 0.4879 ∗ 125 𝑔) + (0.8377 ∗ 375 𝑔) = 𝟑𝟕𝟓. 𝟏𝟐𝟓 𝒈
× ×
𝒎𝒕𝒉𝒆𝒐𝒓𝒆𝒕𝒊𝒄𝒂𝒍 𝒂𝒍𝒌𝒂𝒍𝒊 𝒄𝒆𝒍𝒍𝒖𝒍𝒐𝒔𝒆 = 𝟒𝟐𝟓. 𝟗𝟕 𝒈
The theoretical mass of alkali cellulose was used in the determination of the
optimum operating conditions for alkaline hydrolysis. When the mass of the
extracted alkali cellulose is higher than the theoretical amount, it means that
hemicellulose and lignin are still attached to the corncobs and pineapple crown
leaves. But, there is also a possibility that the excess value accounts for the
remaining alkali solvent since the process used to separate the reagent from the
raw material is only by manual pressing. On the other hand, when it is lower than
the expected theoretical amount, it means that degradation of α-cellulose already
occurred. The selection of optimum operating conditions was based from % alkali
cellulose yield and % impurities removed which were computed as follows:
% 𝑨𝒍𝒌𝒂𝒍𝒊 𝑪𝒆𝒍𝒍𝒖𝒍𝒐𝒔𝒆 𝒀𝒊𝒆𝒍𝒅

|𝒎𝒆𝒙𝒕𝒓𝒂𝒄𝒕𝒆𝒅 𝒂𝒍𝒌𝒂𝒍𝒊 𝒄𝒆𝒍𝒍𝒖𝒍𝒐𝒔𝒆 − 𝒎𝒕𝒉𝒆𝒐𝒓𝒆𝒕𝒊𝒄𝒂𝒍 𝒂𝒍𝒌𝒂𝒍𝒊 𝒄𝒆𝒍𝒍𝒖𝒍𝒐𝒔𝒆 |
= (𝟏 − ) × 𝟏𝟎𝟎
𝒎𝒕𝒐𝒕𝒂𝒍 − 𝒎𝒓𝒆𝒄𝒐𝒗𝒆𝒓𝒆𝒅 𝜶−𝒄𝒆𝒍𝒍𝒖𝒍𝒐𝒔𝒆
% 𝑰𝒎𝒑𝒖𝒓𝒊𝒕𝒊𝒆𝒔 𝑹𝒆𝒎𝒐𝒗𝒆𝒅 = × 𝟏𝟎𝟎
𝒎𝒕𝒐𝒕𝒂𝒍 − 𝒎𝒕𝒉𝒆𝒐𝒓𝒆𝒕𝒊𝒄𝒂𝒍 𝜶−𝒄𝒆𝒍𝒍𝒖𝒍𝒐𝒔𝒆

Project Study 50
𝒎𝒓𝒆𝒄𝒐𝒗𝒆𝒓𝒆𝒅 𝜶−𝒄𝒆𝒍𝒍𝒖𝒍𝒐𝒔𝒆
𝒎𝒆𝒙𝒕𝒓𝒂𝒄𝒕𝒆𝒅 𝒂𝒍𝒌𝒂𝒍𝒊 𝒄𝒆𝒍𝒍𝒖𝒍𝒐𝒔𝒆 𝟏 𝒎𝒐𝒍𝒆 𝒐𝒇 ∝ −𝒄𝒆𝒍𝒍𝒖𝒍𝒐𝒔𝒆
= ×
𝑴𝑾 𝒂𝒍𝒌𝒂𝒍𝒊 𝒄𝒆𝒍𝒍𝒖𝒍𝒐𝒔𝒆 𝟏 𝒎𝒐𝒍𝒆 𝒐𝒇 𝒂𝒍𝒌𝒂𝒍𝒊 𝒄𝒆𝒍𝒍𝒖𝒍𝒐𝒔𝒆
× 𝑴𝑾𝜶−𝒄𝒆𝒍𝒍𝒖𝒍𝒐𝒔𝒆
The higher the percent alkali cellulose yield and percent impurities removed,
the more desirable the operating condition is. However, percent impurities
removed should not exceed 100% as it would entail degradation and conversion
of the desired α-cellulose to byproducts.
Laboratory Setup:
Alkaline
Hydrolysis
Figure 3.6: Alkaline Hydrolysis Setup
1. Determination of the Optimum Length for Pineapple Crown Leaves
According to a study of Devi (2014), a length of 30 mm is needed to effectively

extract cellulose and convert it to alkali cellulose.
Figure 3.7 Determination of the Optimum Length for Pineapple Crown Leaves Setu
Project Study 51
1.1 Materials and Apparatuses
Pineapple Crown Leaves Shears Strainer

Hot Plate Ruler Graduated Cylinder
Thermometer Beaker Cheesecloth
1.2 Objective
To determine the optimum length that will result to the highest significant
percent alkali cellulose yield without degrading the cellulose content of
pineapple crown leaves
1.3 Hypothesis
The length of 30 mm will provide the highest % alkali cellulose yield and
impurities removal.
1.4 Procedure
1.4.1 Using shears, cut the pineapple crown leaves with a length of 5
mm.
1.4.2 Place 500 g of cut 5 mm-pineapple crown leaves in a beaker.
1.4.3 Add 1500 g of 18 %w/w NaOH solution.
1.4.4 Heat the mixture to 40C for 1 hour.
1.4.5 Separate the cake from the filtrate by manual pressing using a
cheesecloth.
1.4.6 Weigh the cake and record.
1.4.7 Repeat steps 1.4.1 to 1.4.6 using 10mm, 20mm, 30mm, and 40mm
length.

Project Study 52
1.5 Data and Results
Table 3.8: Determination of the Optimum Length for Pineapple Crown Leaves
Mass
Mass
Pineapple % Alkali %
Length of
Setup Crown Cellulose Impurities Observation
(mm) cake
Leaves Yield Removed
(g)
(g)
The recovered alkali
1 500 5 490.92 96.78 83.40 cellulose is mushy
with green color.
The physical
observation in setup
2 500 10 480.17 99.04 95.07
1 is similar to that of
setup 2.
The recovered
alkali cellulose is
soft but quite firm
3 500 20 479.37 99.21 95.93 to still maintain its
fibrous
characteristics. It is
dark green in color.
cellulose is firm with
4 500 30 483.79 98.28 91.14 traces of its original
form. It is dark green
in color.
cellulose is soft but it
5 500 40 484.02 98.23 90.89 almost retained its
original appearance.
It is green in color.
Note: The theoretical amount of α-cellulose and alkali cellulose for PCL is 418.85 and
475.62 grams, respectively.

Project Study 53
1.6 Sample Calculation

For Setup 3:
% 𝐴𝑙𝑘𝑎𝑙𝑖 𝐶𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒 𝑌𝑖𝑒𝑙𝑑
|𝑚𝑒𝑥𝑡𝑟𝑎𝑐𝑡𝑒𝑑 𝑎𝑙𝑘𝑎𝑙𝑖 𝑐𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒 − 𝑚𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑎𝑙𝑘𝑎𝑙𝑖 𝑐𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒 |
= (1 − )
𝑚𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑎𝑙𝑘𝑎𝑙𝑖 𝑐𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒
× 100
|479.37 𝑔 − 475.62 𝑔|
% 𝐴𝑙𝑘𝑎𝑙𝑖 𝐶𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒 𝑌𝑖𝑒𝑙𝑑 = (1 − ) × 100
475.62 𝑔
% 𝑨𝒍𝒌𝒂𝒍𝒊 𝑪𝒆𝒍𝒍𝒖𝒍𝒐𝒔𝒆 𝒀𝒊𝒆𝒍𝒅 = 𝟗𝟗. 𝟐𝟏%
𝑚𝑃𝐶𝐿 − 𝑚𝑟𝑒𝑐𝑜𝑣𝑒𝑟𝑒𝑑 𝛼−𝑐𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒

% 𝐼𝑚𝑝𝑢𝑟𝑖𝑡𝑖𝑒𝑠 𝑅𝑒𝑚𝑜𝑣𝑒𝑑 = × 100
𝑚𝑃𝐶𝐿 − 𝑚𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝛼−𝑐𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒
𝑚𝑟𝑒𝑐𝑜𝑣𝑒𝑟𝑒𝑑 𝛼−𝑐𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒
𝑚𝑒𝑥𝑡𝑟𝑎𝑐𝑡𝑒𝑑 𝑎𝑙𝑘𝑎𝑙𝑖 𝑐𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒 1 𝑚𝑜𝑙𝑒 𝑜𝑓 ∝ −𝑐𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒
= ×
𝑀𝑊 𝑎𝑙𝑘𝑎𝑙𝑖 𝑐𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒 1 𝑚𝑜𝑙𝑒 𝑜𝑓 𝑎𝑙𝑘𝑎𝑙𝑖 𝑐𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒
× 𝑀𝑊𝛼−𝑐𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒
479.37 𝑔 1 𝑚𝑜𝑙𝑒 ∝ −𝑐𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒
= ×
184.14 𝑔/𝑚𝑜𝑙 1 𝑚𝑜𝑙𝑒 𝑎𝑙𝑘𝑎𝑙𝑖 𝑐𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒
×
𝑚𝑟𝑒𝑐𝑜𝑣𝑒𝑟𝑒𝑑 𝛼−𝑐𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒 = 422.15 𝑔
500 𝑔 − 422.15 𝑔
500 𝑔 − 418.85 𝑔
% 𝑰𝒎𝒑𝒖𝒓𝒊𝒕𝒊𝒆𝒔 𝑹𝒆𝒎𝒐𝒗𝒆𝒅 = 𝟗𝟓. 𝟗𝟑 %
Comparing Setups 2 and 3:

|∆| |𝑥 − 𝑦|
𝑃𝑒𝑟𝑐𝑒𝑛𝑡 𝐷𝑖𝑓𝑓𝑒𝑟𝑒𝑛𝑐𝑒 = × 100 = × 100
𝑓(𝑥, 𝑦) min(𝑥, 𝑦)
|479.37 − 480.17|
𝑃𝑒𝑟𝑐𝑒𝑛𝑡 𝐷𝑖𝑓𝑓𝑒𝑟𝑒𝑛𝑐𝑒 = × 100
480.17
𝑷𝒆𝒓𝒄𝒆𝒏𝒕 𝑫𝒊𝒇𝒇𝒆𝒓𝒆𝒏𝒄𝒆 = 𝟎. 𝟏𝟕%
(Setups 2 and 3 are not significantly different.)

Project Study 54
|483.79 − 479.37|
479.37
𝑷𝒆𝒓𝒄𝒆𝒏𝒕 𝑫𝒊𝒇𝒇𝒆𝒓𝒆𝒏𝒄𝒆 = 𝟎. 𝟗𝟐%
1.7 Analysis
The selection of the optimum length for pineapple crown leaves is
dictated by the color, texture and appearance of the resulting alkali
cellulose, %alkali cellulose, and % impurities removed. Among the setups
presented in Table 3.7, it was found out that setup 3 with length of 20mm
resulted to an alkali cellulose with dark green in color. Also, as compared to
other setups, setup 3 yielded the highest percentage of alkali cellulose
(99.21%) and impurities removed (95.93%). This observation is due to the
fact that setup 3 provided more contact surface area, leading to higher
percentage conversion. Since there is no significant difference between
this setup and setup 2 (10 mm), then the optimum length was selected to
be 20 mm.
1.8 Conclusion
The optimum length for alkaline hydrolysis of pineapple crown leaves
is 20 mm, having 99.21% alkali cellulose yield and 95.93% impurities
removal with no occurrence of cellulose degradation.
2. Determination of the Optimum Particle Size Diameter for Corn Cobs

According to Neata (2015) and Pointner (2014), a particle size diameter of less
than 10 mm is needed to effectively extract cellulose and convert it to alkali
cellulose.
Figure 3.8 Determination of the Optimum Particle Size Diameter for Corn Cobs Setup

Project Study 55

Corn Cobs Beaker Thermometer
Hot Plate Graduated Cylinder Strainer
Tyler Mesh Cheesecloth
2.2 Objective
To determine the optimum particle size that will result to the highest
significant percent alkali cellulose yield and percent impurities removal
without degrading the cellulose content of corn cobs.
2.3 Hypothesis
The particle size of 1.18mm will provide the highest % alkali cellulose yield
and % impurities removal.
2.4 Procedure
2.4.1 Using shears, cut the corncobs with a diameter of 1.18 mm.
2.4.2 Place 500 g of cut 1.18 mm-corncobs in a beaker.
2.4.3 Add 1500 g of 18 %w/w NaOH solution.
cheesecloth.
2.4.7 Repeat steps 2.4.1 to 2.4.6 using 2.36mm, 4.75mm, and 9.5mm
particle size diameter.

Project Study 56
Table 3.9: Determination of the Optimum Particle Size Diameter for Corncobs
Mass Particle Mass of % Alkali %
Setup Corncobs Size Residue Cellulose Impurities Observation
(g) (mm) (g) Yield Removed
The extracted alkali
cellulose is too
1 500 1.18 296.81 92.86 93.19
mushy. It has light
yellow color.
The resulting alkali
2 500 2.36 293.00 94.23 94.50 cellulose is too soft.
It has yellow color.
The alkali cellulose
extracted is soft
but still firm
enough to
3 500 4.75 283.80 97.55 97.67
maintained its
characteristics. It
has a deep yellow
color.
The resulting alkali
cellulose is still firm
4 500 9.5 300.35 91.58 91.97 and quite maintained
its original form. It is
yellow in color.
Note: The theoretical amount of α-cellulose and alkali cellulose for CC is 243.95 and
277.02 grams, respectively.
For Setup 3:
= (1 − )
× 100
|283.80 𝑔 − 277.02 𝑔|
277.02 𝑔
% 𝑨𝒍𝒌𝒂𝒍𝒊 𝑪𝒆𝒍𝒍𝒖𝒍𝒐𝒔𝒆 𝒀𝒊𝒆𝒍𝒅 = 𝟗𝟕. 𝟓𝟓%

Project Study 57
𝑚𝐶𝐶 − 𝑚𝑟𝑒𝑐𝑜𝑣𝑒𝑟𝑒𝑑 𝛼−𝑐𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒

𝑚𝐶𝐶 − 𝑚𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝛼−𝑐𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒
= ×
= ×
×
500 𝑔 − 381.31 𝑔
500 𝑔 − 243.95 𝑔
% 𝑰𝒎𝒑𝒖𝒓𝒊𝒕𝒊𝒆𝒔 𝑹𝒆𝒎𝒐𝒗𝒆𝒅 = 𝟗𝟕. 𝟔𝟕 %

|∆| |𝑥 − 𝑦|
|283.80 − 293.00|
293.00
𝑷𝒆𝒓𝒄𝒆𝒏𝒕 𝑫𝒊𝒇𝒇𝒆𝒓𝒆𝒏𝒄𝒆 = 𝟑. 𝟏𝟒%

|300.35 − 283.80|
283.80
𝑷𝒆𝒓𝒄𝒆𝒏𝒕 𝑫𝒊𝒇𝒇𝒆𝒓𝒆𝒏𝒄𝒆 = 𝟓. 𝟖𝟑%
(Setups 3 and 4 are significantly different.)
2.7 Analysis
The selection of the optimum particle size for corncobs is dictated by the
color, texture and appearance of the resulting alkali cellulose, %alkali
cellulose, and % impurities removed. Among the setups presented in Table
3.8, it was found out that setup 3 with particle size diameter of 4.75 mm
resulted to an alkali cellulose with deep yellow in color. Also, as compared
to other setups, setup 3 yielded the highest percentage of alkali cellulose

Project Study 58
(97.55%) and impurities removed (97.67%). This observation is due to the

fact that setup 3 provided more contact surface area, leading to higher
percentage conversion. The optimum particle size was selected to be 4.75
mm.
2.8 Conclusion
The optimum particle size for alkaline hydrolysis of corncobs is 4.75 mm,
having 97.55% alkali cellulose yield and 97.67% impurities removal with no
occurrence of cellulose degradation.
3. Determination of the Optimum Ratio of Corncobs to Pineapple Crown Leaves

20 mm-Pineapple Crown
Cheesecloth Strainer
Leaves
4.75 mm-Corn cobs Thermometer Graduated Cylinder
Beaker Cheesecloth
3.2 Objective
To determine the optimum ratio of corncobs to pineapple crown leaves that
will result to the highest significant percent alkali cellulose yield and percent
impurities removal without degrading the cellulose content of corn cobs and
pineapple crown leaves.
3.3 Hypothesis
The ratio 25:75 of corncobs to pineapple crown leaves will yield the highest
percent alkali cellulose yield and percent impurities.
3.4 Procedure
3.4.1 Place 500 g of corncobs and pineapple crown leaves with a ratio of
25:75 in a beaker.
3.4.2. Add 1500 g of 18 %w/w NaOH solution.
cheesecloth.
3.4.6 Repeat steps 3.4.1 to 3.4.5 using 50:50, and 75:25 ratio.

Project Study 59
Table 3.10: Determination of the Optimum Ratio of Corncobs to

Pineapple crown leaves
Mass Ratio of
Corncobs Corncobs %
Mass of % Alkali
and to Impuritie
Setup Residue Cellulose Observation
Pineapple Pineapple s
(g) Yield
Crown Crown Removal
Leaves (g) Leaves
The mixture
1 500 25:75 431.57 98.69 96.05 turns into green
color.
The mixture has a
2 500 50:50 449.18 94.55 83.63 yellow green
color.
The mixture turns
3 500 75:25 463.10 91.28 73.82
to yellow color.
Note: The theoretical amount of α-cellulose and alkali cellulose is 375.125 and 425.97
grams, respectively.

For Setup 1:
= (1 − )
× 100
|431.57 𝑔 − 425.97 𝑔|
425.97 𝑔
% 𝑨𝒍𝒌𝒂𝒍𝒊 𝑪𝒆𝒍𝒍𝒖𝒍𝒐𝒔𝒆 𝒀𝒊𝒆𝒍𝒅 = 𝟗𝟖. 𝟔𝟗%
𝑚𝑖𝑛 − 𝑚𝑟𝑒𝑐𝑜𝑣𝑒𝑟𝑒𝑑 𝛼−𝑐𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒

𝑚𝑖𝑛 − 𝑚𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝛼−𝑐𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒
= ×
Project Study 60
= ×
×
500 𝑔 − 380.06 𝑔
500 𝑔 − 375.125 𝑔
% 𝑰𝒎𝒑𝒖𝒓𝒊𝒕𝒊𝒆𝒔 𝑹𝒆𝒎𝒐𝒗𝒆𝒅 = 𝟗𝟔. 𝟎𝟓 %

|∆| |𝑥 − 𝑦|
|449.18 − 431.57|
431.57
𝑷𝒆𝒓𝒄𝒆𝒏𝒕 𝑫𝒊𝒇𝒇𝒆𝒓𝒆𝒏𝒄𝒆 = 𝟒. 𝟎𝟖%

|463.10 − 431.57|
431.57
𝑷𝒆𝒓𝒄𝒆𝒏𝒕 𝑫𝒊𝒇𝒇𝒆𝒓𝒆𝒏𝒄𝒆 = 𝟕. 𝟑𝟏%
(Setups 1 and 3 are significantly different.)
3.7 Analysis
The selection of the optimum ratio of corncobs to pineapple crown
leaves is dictated by the color, %alkali cellulose, and % impurities
removed. Among the setups presented in Table 3.9, it was found out that
setup 1 with ratio of 25:75 resulted to an alkali cellulose with green in color.
Also, as compared to other setups, setup 1 yielded the highest percentage
of alkali cellulose (98.69%) and impurities removed (96.05%). The higher
portion of pineapple crown leaves over corncobs provided the highest %
alkali cellulose yield as pineapple crown leaves contains higher alpha-
cellulose content over corncobs. The optimum ratio was selected to be
25:75.

Project Study 61
3.8 Conclusion
The optimum ratio for alkalization of corncobs to pineapple crown leaves
is 25:75, having 98.69% alkali cellulose yield and 96.05% impurities
removed with no occurrence of cellulose degradation.
4. Determination of the Optimum Alkalization Agent

For alkalization, sodium hydroxide, potassium hydroxide, and calcium hydroxide
were used as alkalization agents.
Figure 3.9 Determination of the Optimum Alkalization Agent Setup

Corncobs and Pineapple Crown Leaves NaOH KOH Ca(OH)2
Thermometer Beaker Hot Plate Strainer
4.2 Objective
To determine the appropriate alkalization agent that will provide the
highest significant percent alkali cellulose yield without degrading the
cellulose content of Corncobs and Pineapple Crown Leaves
4.3 Hypothesis
NaOH will provide the highest yield of alkali cellulose.
4.4 Procedure
4.4.1 Place 500 g of 25:75 corncobs and pineapple crown leaves in a
beaker.

Project Study 62

cheesecloth.
4.4.6 Repeat steps 4.4.1 to 4.4.5 using KOH and Ca(OH)2 as alkali agents.

Table 3.11: Determination of Alkali Type for Alkaline Hydrolysis
Mass
25:75
Corncobs Mass of % Alkali %
Type of
Setup to Cake Cellulose Impurities Observation
Alkali
Pineapple (g) Yield Removed
Crown
Leaves (g)
Particles of Ca(OH)2
forms a milky white
suspension-
1 500 Ca(OH)2 520.11 77.90 33.61 consistency filtrate
which the undissolved
Ca(OH)2 adheres on
the biomass
obtained is soft but
2 500 KOH 441.59 96.33 88.99 lumpy indicating there
is removal of non-
cellulosic material
obtained is soft and
crumbly showing
3 500 NaOH 433.15 98.31 94.94
the effective
removal of non-
cellulosic material.

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For Setup 3:
= (1 − ) × 100
|433.15 𝑔 − 425.97 𝑔|
425.97 𝑔
% 𝑨𝒍𝒌𝒂𝒍𝒊 𝑪𝒆𝒍𝒍𝒖𝒍𝒐𝒔𝒆 𝒀𝒊𝒆𝒍𝒅 = 𝟗𝟖. 𝟑𝟏%
𝑚𝑐𝑎𝑠𝑠𝑎𝑣𝑎 𝑝𝑒𝑒𝑙𝑠 − 𝑚𝑟𝑒𝑐𝑜𝑣𝑒𝑟𝑒𝑑 𝛼−𝑐𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒
𝑚𝑐𝑎𝑠𝑠𝑎𝑣𝑎 𝑝𝑒𝑒𝑙𝑠 − 𝑚𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝛼−𝑐𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒
= × × 𝑀𝑊𝛼−𝑐𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒
433.15 𝑔 1 𝑚𝑜𝑙𝑒 ∝ −𝑐𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒 162.16 𝑔 ∝ −𝑐𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒
= × ×
184.14 𝑔/𝑚𝑜𝑙 1 𝑚𝑜𝑙𝑒 𝑎𝑙𝑘𝑎𝑙𝑖 𝑐𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒 1 𝑚𝑜𝑙𝑒 ∝ −𝑐𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒
500.00 𝑔 − 381.45 𝑔
500.00 𝑔 − 375.125 𝑔
% 𝑰𝒎𝒑𝒖𝒓𝒊𝒕𝒊𝒆𝒔 𝑹𝒆𝒎𝒐𝒗𝒆𝒅 = 𝟗𝟒. 𝟗𝟒 %
4.7 Analysis
Among the type of alkali used in extraction of cellulose, NaOH
provides the highest percent cellulose (98.31%) yield and percent impurities
removed (94.94%). Moreover, KOH also able to extract alkali cellulose and
remove non-cellulosic impurities but not as much as NaOH do but Ca(OH)2
has not able to obtain alkali cellulose because Ca(OH)2 does not dissolve
in water. Therefore, of the three-alkali used, NaOH is the strongest making
it more effective as swelling agent to remove the non-cellulosic
components.
4.8 Conclusion
The optimum alkalization agent is NaOH, having 98.31% alkali cellulose
and 94.94% impurities removed with no occurrence of cellulose
degradation.

Project Study 64
5. Determination of the Optimum Alkali Concentration

In alkaline hydrolysis, according to Kumar et al. (2007), the cellulose pulp is
immersed in 17-20% strong alkali solvent to swell the cellulose fibers and to
convert cellulose to alkali cellulose.
Figure 3.10 Determination of the Optimum Alkalization Concentration Setup

25:75 Corncobs to Pineapple Crown Leaves NaOH
Beaker
Hot Plate Strainer Graduated Cylinder
Thermometer
5.2 Objective
To determine the optimum alkali concentration that will provide the highest
significant percent alkali cellulose yield and percent impurities removal
without degrading the cellulose content of corncobs and pineapple crown
leaves.
5.3 Hypothesis
The optimum alkali concentration for alkaline hydrolysis is 18wt%.

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5.4. Procedure
beaker.
cheesecloth.
5.4.6 Repeat steps 5.4.1 to 5.4.5 using 15% w/w and 21% w/w NaOH
soution.
5.5. Data and Results
Table 3.12: Determination of the Optimum Alkali Concentration for Alkaline

Hydrolysis
Mass
25:75
Corncobs Mass
Alkali % Alkali %
to of
Setup Conc. Cellulose Impurities Observation
Pineapple cake
(wt%) Yield Removed
Crown (g)
Leaves
(g)
The alkali cellulose is
soft but lumpy with little
1 500 15 533.64 74.72 24.07
change in color from the
original biomass
The alkali cellulose is
darker in color, soft,
crumbly and the
2 500 18 438.84 96.98 90.92
undesired components
were substantially
removed.
The impurities removal
exceeded which means
3 500 21 344.96 119.02 157.13
the degraded cellulose
is 57.13%

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5.6. Sample Computation

For Setup 3:
= (1 − )
× 100
|344.96 𝑔 − 425.97 𝑔|
% 𝐴𝑙𝑘𝑎𝑙𝑖 𝐶𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒 𝑌𝑖𝑒𝑙𝑑 = (1 − ) × 100 = 𝟏𝟏𝟗. 𝟎𝟐%
425.97 𝑔
= ×
= ×
×
500.00 𝑔 − 303.78 𝑔
% 𝐼𝑚𝑝𝑢𝑟𝑖𝑡𝑖𝑒𝑠 𝑅𝑒𝑚𝑜𝑣𝑒𝑑 = × 100 = 𝟏𝟓𝟕. 𝟏𝟑%
500.00 𝑔 − 375.125 𝑔
157.13% of cellulose was degraded.
5.7. Analysis
As shown in Table 3.11, among the three concentrations of NaOH solution,
18% has the highest alkali cellulose yield (96.98%) and impurities removed
(90.92%) without degrading cellulose content. Although set-up 3 is viable,
occurrence of cellulose degradation makes the set-up two more
economical. Such degradation must be avoided as further alkalization might
result to unwanted side reactions such as the production of other chemicals
derived from cellulose.

Project Study 67
5.8. Conclusion
The optimum alkali concentration for alkaline hydrolysis is 18 wt% NaOH
having 96.98% alkali cellulose yield and 90.92% impurities removal with no
occurrence of cellulose degradation.
6. Determination of the Optimum Reaction Temperature
6.1. Materials and Apparatuses

Beaker
Hot Plate Strainer Graduated Cylinder Cheesecloth
6.2 Objective
To determine the optimum reaction temperature that will provide the highest
significant percent alkali cellulose yield and impurities removed without
degrading the cellulose content of corncobs and pineapple leaves.
6.3 Hypothesis
The temperature that will give the optimum result is expected to be 40°C.
6.4. Procedure
beaker.
cheesecloth.
6.4.6 Repeat steps 6.4.1 to 6.4.5 using 40C, 50C, 60C, and 70C
reaction temperature.

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Table 3.13: Determination of the Optimum Temperature for Alkaline Hydrolysis

Mass
25:75
Corncobs Mass of % Alkali %
Temp
Setup to Cake Cellulose Impurities Observation
°C
Pineapple (g) Yield Removed
Crown
Leaves (g)
was soft and lumpy
1 500 30°C 468.97 89.91 69.68 and little darker
than the original
feed
The alkali
cellulose is softer
2 500 40°C 436.02 97.64 92.91 than the previous
set-up, crumbly,
has darker color.
is even darker with
3 500 50°C 411.35 96.57 110.31
impurities removal
exceeds by 10.31%
is very dark with
4 500 60°C 394.54 92.62 122.17
impurities removal
exceeds by 22.17%
is very dark with
5 500 70°C 379.27 89.04 132.93
impurities removal
exceeds by 32.93%

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For Setup 3:
= (1 − ) × 100
|411.35 𝑔 − 425.97 𝑔|
% 𝐴𝑙𝑘𝑎𝑙𝑖 𝐶𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒 𝑌𝑖𝑒𝑙𝑑 = (1 − ) × 100 = 𝟗𝟔. 𝟓𝟕%
425.97 𝑔
= × × 𝑀𝑊𝛼−𝑐𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒
411.35 𝑔 1 𝑚𝑜𝑙𝑒 ∝ −𝑐𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒 162.16 𝑔 ∝ −𝑐𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒
= × ×
184.14 𝑔/𝑚𝑜𝑙 1 𝑚𝑜𝑙𝑒 𝑎𝑙𝑘𝑎𝑙𝑖 𝑐𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒 1 𝑚𝑜𝑙𝑒 ∝ −𝑐𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒
500.00 𝑔 − 362.25 𝑔
500.00 𝑔 − 375.125 𝑔
% 𝑰𝒎𝒑𝒖𝒓𝒊𝒕𝒊𝒆𝒔 𝑹𝒆𝒎𝒐𝒗𝒆𝒅 = 𝟏𝟏𝟎. 𝟑𝟏%
10.31% of cellulose was degraded.
6.7. Analysis
The set of data shows that as the temperature of alkali digestion increases,
the amount of impurities removed also increases. However, at temperatures
50OC, 60OC, and 70OC was observed removal of impurities exceed from
100% which signifies occurrence of cellulose degradation. Among the
temperatures used, 40OC shows the highest alkali cellulose yield (97.64%)
and impurities removal (92.91%) without degrading the cellulose content,
hence it is chosen as the optimum temperature.
6.8. Conclusion
The optimum operating temperature for alkalization is 40°C having 97.64%
alkali cellulose yield and 92.91% impurities removed with no occurrence of
cellulose degradation.

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7. Determination of the Optimum Reaction Time

Beaker Hot Plate
Cheesecloth Graduated Cylinder Timer
7.2 Objective
To determine the optimum reaction time that will provide the highest
significant percent alkali cellulose yield without degrading the cellulose
content of corncobs and pineapple crown leaves
7.3 Hypothesis
The optimum reaction time for alkaline hydrolysis is expected to be 1 hour.
7.4. Procedure
beaker.
7.4.3 Heat the mixture to 40C for 30 minutes.
cheesecloth.
7.4.6 Repeat steps 7.4.1 to 7.4.5 using 60mins, 90mins, 120mins,
150mins, and 180 mins reaction time.

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Table 3.14: Determination of Optimum Reaction Time for Alkaline Hydrolysis
Mass
25:75
Corncobs
Mass of % Alkali %
to Time
Setup Cake Cellulose Impurities Observation
Pineapple (minutes)
(g) Yield Removed
Crown
Leaves
(g)
1 500 30 458.86 92.28 76.81 changes is soft and
crumbly
The alkali cellulose s
softer relative to the
previous step. The
2 500 60 433.76 98.17 94.51 alkali cellulose yield
and the percent
impurities removed in
closest to 100%
The percent removal of
impurities exceeds
3 500 90 410.12 96.28 111.18 100% which means
cellulose was degraded
during the process is
impurities exceeds
100% which means
4 500 120 406. 06 95.33 114.04
14.04%
impurities exceeds
100% which means
5 500 150 377.49 88.62 134.19
34.19%
impurities exceeds
100% which means
6 500 180 359.52 84.40 146.92
46.92%

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For Setup 3:
= (1 − )
× 100
|410.12 𝑔 − 425.97 𝑔|
% 𝐴𝑙𝑘𝑎𝑙𝑖 𝐶𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒 𝑌𝑖𝑒𝑙𝑑 = (1 − ) × 100 = 𝟗𝟔. 𝟐𝟖%
425.97 𝑔
𝑚𝑐𝑎𝑠𝑠𝑎𝑣𝑎 𝑝𝑒𝑒𝑙𝑠 − 𝑚𝑟𝑒𝑐𝑜𝑣𝑒𝑟𝑒𝑑 𝛼−𝑐𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒
𝑚𝑐𝑎𝑠𝑠𝑎𝑣𝑎 𝑝𝑒𝑒𝑙𝑠 − 𝑚𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝛼−𝑐𝑒𝑙𝑙𝑢𝑙𝑜𝑠𝑒
= ×
= ×
×
500.00 𝑔 − 361.17 𝑔
% 𝐼𝑚𝑝𝑢𝑟𝑖𝑡𝑖𝑒𝑠 𝑅𝑒𝑚𝑜𝑣𝑒𝑑 = × 100 = 𝟏𝟏𝟏. 𝟏𝟖%
500.00 𝑔 − 375.125 𝑔
11.18% cellulose is degraded.
7.7. Analysis
The preceding steps shows that as the reaction time successively
increases, amount of impurities removed from the product. However, only
degradation of alpha cellulose was observed at 60 minutes onwards
wherein removal exceeded 100%. This degradation of cellulose may lead
to dissolution of cellulose in sodium hydroxide solvent, thus may lead to
lower percentage yield. This condition must be avoided in further
alkalization might result to unwarranted side reactions cause by immersion
in an acid slide.

Project Study 73
7.8. Conclusion
The optimum reaction time for acid hydrolysis of pineapple crown leaves
and corn cobs is 60 minutes yielding 98.17% alkali cellulose and removed
94.51% of impurities present with no removal of cellulose through
degradation.
II. XANTHATION
The alkali cellulose is allowed to react with carbon disulfide. The carbon
disulfide weighing between 30-40% of the dry recoverable cellulose is slowly
added under controlled temperature (about 20-30C) during 2 hours of churning,
during which time the crumbs gradually turn yellow and finally deep orange, and
coagulate into small balls called cellulose xanthate (Dua, 2017).
Figure 3.11: Xanthation Reaction
Laboratory Setup:
Figure 3.12: Xanthation Setup

Project Study 74
1. Determination of the optimum amount of Carbon disulfide

Analytical
Alkali Cellulose Stirring rod
Balance
Carbon disulfide (CS2) Beakers Timer
1.2 Objectives
To determine the optimum amount of carbon disulfide to proceed to the
reaction.
1.3 Hypothesis
The optimum amount of carbon disulfide is 200 g.
1.4 Procedures
1.4.1 Place 500 g of alkali cellulose in a beaker.

1.4.2. Add 125 g of CS2.
1.4.4 Weigh the mixture and record.
1.4.5 Repeat steps 1.4.1 to 1.4.4 using 150,175, 200, and 225 grams of
CS2.

Project Study 75

Table 3.15: Determination of the amount of Carbon disulfide
Weight of
Weight of Weight of
Alkali
Alkali Carbon Time
Trial Cellulose Observation
Cellulose Disulfide (minutes)
Xanthate
(grams) (grams)
(Grams)
The alkali cellulose turned greenish
1 500 125 180 551.43
brown xanthate balls
The alkali cellulose turned into brown
2 500 150 180 561.51
xanthate balls.
The alkali cellulose turned into deep
3 500 175 180 566.99
orange xanthate balls.
4 500 200 180 565.21
5 500 225 180 563.35
1.6 Analysis
In the process of xanthation of the alkali cellulose treated with carbon
disulfide becomes deep orange in color and will eventually form into balls,
at certain time signifying that the reaction is gradually taking place
(Chemical process industries, Shrieves). The amount of carbon disulfide at
175 g (which is 35% of the mass of alkali cellulose) onwards form deep
orange cellulose xanthate balls
1.7 Conclusion
Among the five trials made, Trial 3 with 175 g carbon disulfide (35% of mass
of alkali cellulose) has been chosen since this is the trial that formed
xanthate balls with a deep orange color which is an indicator that xanthation
had occurred at minimum amount of carbon disulfide. Although Trials 4 and
5 also formed deep orange xanthate balls, cost in terms of the reagent used
is considered.

Project Study 76
2. Determination of the Optimum Time for Xanthation
Figure 3.13 Determination of the Optimum Time for Xanthation Setup

Analytical
Alkali Cellulose Stirring rod
Balance
Carbon disulfide (CS2) Beakers Timer
2.2 Objectives
To determine the appropriate time for the xanthation of the alkali cellulose.
2.3 Hypothesis
The required time of xanthation allows the carbon disulfide to react through
the alkali cellulose is 120 minutes.
2.4 Procedures
2.4.1 Place 500 g of alkali cellulose in a beaker.

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2.4.2. Add 175 g of CS2.

2.4.5 Repeat steps 2.4.1 to 2.4.4 using 60mins, 90mins, 120mins,
150mins, and 180mins xanthation time.
Table 3.16: Determination of the Optimum Time for Xanthation
Weight Weight of
Weight of
of Alkali
Alkali Time
Trial Carbon Cellulose Observation
Cellulose (minutes)
Disulfide Xanthate
(grams)
(grams) (grams)
The solution is still fibrous
1 500 175 30 548.17 and there is no formation of
xanthate balls.
The solution is still fibrous
2 500 175 60 552.19 and there is no formation of
xanthate balls.
The solution is quite forming
3 500 175 90 557.85 into deep green xanthate
balls.
The solution is forming into
4 500 175 120 561.46
green xanthate balls.
5 500 175 150 564.35
pale orange xanthate balls.

6 500 175 180 567.09
deep orange xanthate balls.
2.6 Analysis
The minimum time needed for xanthation should be determined in
consideration of economizing the cost and time of process. The desired

Project Study 78
color of the xanthate solution was formed and observed in the 180 minutes
of xanthation. This shows that 180 minutes is needed to form the xanthate
balls which are required for the next reaction.
2.7 Conclusion
A time of 180 minutes is required to allow high conversion (as indicated by
the color of the crumb) of alkali cellulose to alkali cellulose xanthate.
III. ALKALIZATION
After allowing carbon disulfide to penetrate in the alkali cellulose ate the required
time, the alkali cellulose xanthate is dissolved in dilute sodium hydroxide solution
to form viscose.
1. Determination of the Optimum Concentration of NaOH Solution for

Viscose
Figure 3.14 Determination of the Optimum Concentration of NaOH Solution for

Viscose Setup

Analytical
Alkali Cellulose Xanthate Stirring rod
Balance
Sodium Hydroxide
Beakers Timer
(NaOH)
1.2 Objectives
To determine the appropriate concentration of NaOH solution for viscose
preparation.

Project Study 79
1.3 Hypothesis
The appropriate concentration of NaOH solution that will yield further
conversion of alkali cellulose to alkali cellulose xanthate is 3%.
1.4 Procedures
1.4.1 Place 500 g of alkali cellulose xanthate in a beaker.

1.4.2. Add 750 grams of 3% w/w NaOH solution.
1.4.3 Let the mixture stand for 180 minutes in 10-15C.
1.4.5 Repeat steps 1.4.1 to 1.4.4 using 5% w/w, 7% w/w, 9% w/w, and
11% w/w NaOH solution.
Table 3.17: Determination of the Optimum Concentration of NaOH Solution for

Viscose
Weight of
Concentration Weight of
Alkali
of Sodium Time Viscose
Trial Cellulose
Hydroxide (% Solution
Observation
Xanthate (minutes)
m/m) (grams)
(grams)
The solution is not viscous and 2

1 500 3 180 1247.89 layers of NaOH and alkali
cellulose xanthate formed.
The alkali cellulose xanthate is
2 500 5 180 1248.17 fully dissolved forming viscose
solution.
3 500 7 180 1247.97 fully dissolved but forming less
viscose solution.
viscose solution.
viscose solution.

Project Study 80
1.6 Analysis
An optimum amount concentration of NaOH for viscose formation is
determined in consideration of economizing cost of reagents. Based on
the result, 5% m/m concentration of NaOH solution will suffice the
dissolution of cellulose xanthate balls, which can achieve viscose
solution of colloidal consistency. Too low will result to settling of the
undissolved cellulose and too high will result to viscose of less
consistency, which will yield to weaker films.
1.7 Conclusion
The 5% w/w NaOH solution is the optimum amount needed to dissolve
the cellulose xanthate.
2. Determination of the Optimum Ratio of Sodium Hydroxide Solution to

Alkali Cellulose Xanthate
Figure 3.15 Determination of the Optimum Ratio of Sodium Hydroxide Solution to

Alkali Cellulose Xanthate Setup

Alkali Cellulose Analytical
Stirring rod
Xanthate Balance
NaOH Beakers Timer
2.2 Objectives
To determine the appropriate ratio of Sodium Hydroxide Solution to Alkali
Cellulose Xanthate

Project Study 81
2.3 Hypothesis
The appropriate ratio of sodium hydroxide solution will be the one that will
dissolve the alkali cellulose xanthate.
2.4 Procedures

2.4.5 Repeat steps 2.4.1 to 2.4.4 using 500 g, 750 g, 1000 g, and 1250 g
NaOH solution.

Table 3.18: Determination of the Optimum Ratio of Sodium Hydroxide Solution to
Alkali Cellulose Xanthate
Weight of Weight of Weight of
NaOH Alkali Cellulose Time Viscose
Trial Ratio Solutions Xanthate (minutes) Solution
Observation
(grams) (grams) (grams)
The solution is not
viscous and 2 layers of
1 1:0.50 250 500 180 748.62
NaOH and alkali cellulose
xanthate formed.

2 1:1 500 500 180 997.73 xanthate is fully dissolved
forming viscose solution.

xanthate is fully dissolved
3 1:1.5 750 500 180 1249.51
but forming less viscose
solution.
4 1:2 1000 500 180 1498.41
solution.
5 1:2.5 1250 500 180 1747.19
solution.

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2.6 Analysis
From the trials made, it shows that the amount of the sodium hydroxide
solution with alkali cellulose xanthate have significant effects in forming the
viscose solution. Low amount of NaOH solution will not fully dissolve the
alkali cellulose whereas too high amount of NaOH will dilute the viscose,
resulting to low viscosity. Thus, the amount yields an optimum higher
viscosity is at 1:1.5 alkali cellulose to NaOH solution ratio.
2.7 Conclusion
The 1:1.5 ratio of 5% w/w NaOH solution with the alkali cellulose xanthate
is the optimum amount needed to dissolve the cellulose xanthate with
colloidal consistency.
3. Determination of the Optimum Alkalization Time

Alkali Cellulose Analytical
Stirring rod
Xanthate Balance
NaOH Beakers Timer
3.2 Objectives
To determine the optimum alkalization time for the alkali cellulose xanthate
to form viscose solution.
3.3 Hypothesis
The optimum alkalization time is 180 minutes.
3.4 Procedures

3.4.5 Repeat steps 3.4.1 to 3.4.4 using 60 mins, 90mins, 120 mins, 150
mins, and 180 mins alkalization time.

Project Study 83
Table 3.19: Determination of the Optimum Alkalization Time
Weight of
Weight of Weight of
Alkali
NaOH Time Viscose
Trial Cellulose Observation
Solution (minutes) Solution
Xanthate
(grams) (grams)
(grams)
1 500 750 30 1247.29 There are no visible changes.
2 500 750 60 1247.75 There are no visible changes.

3 500 750 90 1248.22 layers of NaOH and alkali cellulose
xanthate formed.
4 500 750 120 1248.81 layers of NaOH and alkali cellulose
xanthate formed.

5 500 750 150 1249.12 slightly dissolved forming viscose
solution.

6 500 750 180 1249.63 fully dissolved forming viscose
solution.
3.6 Analysis
From the trials made, it shows that the alkalization time have significant
effects in forming the viscose solution. It is evident that at 180 minutes, the
viscose solution is formed and no lumps remained.
3.7 Conclusion
The alkalization time needed to form the viscose solution is 180 minutes.

Project Study 84
IV. RIPENING
Ripening is done after Alkalization to prepare the viscose solution for casting.
1. Determination of the Optimum Ripening Time of Viscose Solution

Viscose Solution
1.2 Objectives
To determine the optimum ripening time for viscose solution to be prepared
for casting.
1.3 Hypothesis
The optimum ripening time for viscose solution is 120 minutes.
1.4 Procedures
1.4.1 Let the viscose solution stand in a temperature of 10-15 OC for 30
minutes.
1.4.2 Observe and record observations.
1.4.3 Repeat steps 1.4.1 and 1.4.2 using 60, 90, 120, 150, 180, 210, and
240 minutes ripening time.

Table 3.20: Determination of the Optimum Ripening Time of Viscose Solution
Time
Setup Observation
(min)
The viscose solution shows no changes in comparison after
1 30
alkalization.
The viscose solution doesn’t show any changes but it slightly
2 60
changed its color into a darker orange.
3 90 The viscose solution slightly thickens.
4 120 The viscose solution is thicker than the previous setup.
7 210 There is no observable change from the previous setup.
8 240 There is no observable change from the previous setup.

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1.6 Analysis
In preparation for casting, it is needed that the viscose solution doesn’t show
any observable change with respect to its viscosity. Based on the
conventional process stated from Shrieves’ Chemical Process Industries,
the ripening time of viscose solution is 16-24 hours. However, it is observed
that leaving the solution for more than 12 hours, it coagulates and forms a
gelatinous solid and some liquid.
1.7 Conclusion
The optimum ripening time needed to prepare the viscose solution for
casting is 180 minutes.
V. CASTING
In casting, the syrupy viscose solution is reconverted to cellulose by shaping it into
a film via mold and then immersed in dilute sulfuric acid solution bath until the film
solidifies.
Laboratory Setup:
Figure 3.16: Casting to Drying Setup

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1. Determination of the Optimum Concentration of H2SO4 Solution for

Viscose Film

Viscose Solution Glass tray Tong
Sulfuric Acid (H2SO4) Glass slides Timer
Spatula Oven dryer Graduated cylinder
Filter
1.2 Objectives
To determine the optimum concentration of H2SO4 solution for casting
1.3 Hypothesis
The optimum concentration of H2SO4 solution is 24% by volume
1.4 Procedures
1.4.1 Place 12% v/v H2SO4 solution in a glass tray.
1.4.2 Filter the resulting viscose solution to separate viscose liquid from
undissolved cellulose.
1.4.3 Prepare three sets of glass slides and spread the top surfaces with
viscose using spatula.
1.4.4 Dry the slides at 100OC at 10 minutes until the solution partially dries.
1.4.5 After drying, dip each of the slides with viscose solution into the acid
bath for 30 seconds.
1.4.6 Remove from the bath and record the observations.
1.4.7 Repeat steps 1.4.1 to 1.4.6 using 16% v/v, 20% v/v, 24% v/v, and
28% v/v H2SO4 solution.

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Table 3.21: Determination of the Optimum Concentration of H2SO4 Solution for

Viscose Film
Concentration of Immersion
Setup Observation
H2SO4 (% v/v) Time (sec)
The film is yellowish dirty white with soft
1 12 30
surface after immersion.
The film is yellowish dirty white with soft
2 16 30
The film is dirty white with soft surface the

3 20 30
can be easily tear apart.
The film is dirty white, strong and has

4 24 30
a hard surface.
5 28 30 The film is dirty white and is brittle.
1.6 Analysis
In casting, it is needed that the film is formed by the reaction between
viscose solution and H2SO4, thus forming cellophane. Thus, 5% NaOH w/w
solution was chosen. Undissolved fiber might disrupt the formation of
cellophane.
1.7 Conclusion
The 24% v/v H2SO4 solution is the optimum concentration needed to in
casting to reconvert viscose into cellulose.
2. Determination of Optimum Casting Time


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2.2 Objectives
To determine the optimum time for casting of viscose solution.
2.3 Hypothesis
The optimum tine for casting is 30 seconds.
2.4 Procedures
2.4.1 Place 24% v/v H2SO4 solution in a glass tray.
2.4.2 Filter the resulting viscose solution to separate viscose liquid from
undissolved cellulose.
2.4.3 Prepare three sets of glass slides and spread the top surfaces with
viscose using spatula.
2.4.4 Dry the slides at 100OC at 10 minutes until the solution partially dries.
2.4.5 After drying, dip each of the slides with viscose solution into the acid
bath for 15 seconds.
2.4.6 Remove from the bath and record the observations.
2.4.7 Repeat steps 2.4.1 to 2.4.6 using 30, 45, 60, 75 seconds casting
time.
Table 3.22: Determination of Optimum Casting Time
Concentration of Immersion
Trial Observation
H2SO4 (% v/v) Time (sec)
The film is yellowish dirty white
1 24 15
with soft surface after immersion.
The film dirty white with hard
2 24 30
3 24 45
4 24 60
5 24 75 The film is dirty white and is brittle.

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2.6 Analysis
Time of immersion is a necessary to be identify because it determines the
strength of the film. 30 seconds of immersion time exhibits the desired
condition of the film since at this time interval, the film starts to harden
enough.
2.7 Conclusion
30 seconds is the optimum casting time needed for casting to reconvert
viscose into cellulose.
VI. HOT WATER WASHING
In this process, the formed viscose film from casting is washed by hot water
immersion to remove the excess acid from casting.
1. Determination of the Temperature of Hot Water Bath

Ceramic tray Hot Water Thermometer
1.2 Objectives
To determine the appropriate temperature of water for hot water washing of
viscose film.
1.3 Hypothesis
The appropriate temperature of hot water bath is 50OC
1.4 Procedures
1.4.1 Prepare viscose film dipped in acid bath.
1.4.2 Heat water at 30OC
1.4.3 Soak the viscose film at hot water bath for 30 seconds.
1.4.4 Remove from the hot water bath and record the observations.
1.4.5 Repeat steps 1.4.1 to1.4.4 using 40OC, 50OC, 60OC, and 70OC hot
water bath.

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Table 3.23: Determination of the Temperature of Wash Water Bath
Temperature of Wash Immersion

Trial Observation
Water (oC) Time (sec)
Yellowish dirty white with
1 30 30
undesirable smell still present
Yellowish dirty white with
2 40 30
undesirable smell still present
3 50 30 Dirty white; odorless
1.6 Analysis
Temperature affects the rate of removal of excess acid and other impurities
formed during the casting process. Water at temperature 50 OC can suffice
the removal of undesirable smell caused by the acid and reaction by-
products.
1.7 Conclusion
Wash water bath at 50OC is the appropriate temperature of water for the
washing of viscose film.
2. Determination of Hot Water Washing Time

Viscose Solution Glass tray Tongs
2.2 Objectives
To determine the appropriate time of hot water washing of viscose film.
2.3 Hypothesis
The appropriate time for hot water washing is 45 seconds.
2.4 Procedures
2.4.1 Prepare viscose films dipped in acid bath.

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2.4.2 Heat water at 50OC

2.4.3 Soak the viscose film at hot water baths for 30 seconds.
2.4.4 Remove from the hot water bath and record the observations.
2.4.5 Repeat steps 2.4.1 to 2.4.4 using 45 sec, 60 sec, 75 sec, and 90 sec
immersion time.

Table 3.24: Determination of How Water Washing Time
Temperature of Wash Immersion Time

Trial Observation
Water (oC) (sec)
Dirty white with undesirable
1 50 30
smell still present
Dirty white, have odorless
2 50 45
smell
3 50 60 Dirty white with odorless smell
2.6 Analysis
The amount of immersion time in wash water is a factor on the removal of
undesirable smell and color caused by reaction by-products. 45 seconds
was chosen as the washing since this time interval is already enough to
remove the reaction by-products as well as excess acid.
2.7 Conclusion
45 seconds is the optimum hot water washing time needed for washing off
the acid from the viscose film.
VII. BLEACHING
Sodium hypochlorite (NaClO) is used as a bleaching agent in this process which

removes the remaining color and odor of the viscose film.
Sodium hypochlorite is a clear, slightly yellowish solution with a characteristic odor.

It has a relative density of is 1,1 (5,5% watery solution). As a bleaching agent for
domestic use it usually contains 5% sodium hypochlorite (with a pH of around 11, it is

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irritating). If it is more concentrated, it contains a concentration 10-15% sodium

hypochlorite (with a pH of around 13, it burns and is corrosive).
The higher the sodium hypochlorite strength, the faster the decomposition rate
becomes. The presence of transition metal ions is known to catalyze the decomposition
of liquid sodium hypochlorite, contributing to the loss of sodium hypochlorite strength
and the formation of oxygen. Loss of sodium hypochlorite strength means more product
will be needed when the sodium hypochlorite is used as a disinfectant.
Oxygen build-up can pose problems when storing sodium hypochlorite in storage
containers or bleach transport piping due to pressure build-up. By removing suspended
solids to nearly undetectable levels from the sodium hypochlorite solution, the rate of
decomposition is significantly reduced. In addition, the formation of oxygen is nearly
eliminated, resulting in significantly reduces the rate of decomposition and nearly
eliminates the formation of oxygen.
Sodium hypochlorite is very reactive, and actually unstable. Left exposed to the
atmosphere, chlorine gas evaporates from the solution at a considerable rate, and if it
is heated the sodium hypochlorite falls apart into salt and oxygen. This also happens
when it comes into contact with acids, sunlight, certain metals, and many gases, and is
one of the reasons why bleach can be used on a large scale - after use it decomposes
to benign products (salt and water) which can be flushed into the drainage system
without problem. (May, P and Cotton, S. Molecules that Amaze Us. 2015)
1. Determination of the Bleaching Time

Sodium Hypochlorite
(NaClO)
1.2 Objectives
To determine the optimum time of the bleaching of the viscose film
1.3 Hypothesis
The optimum for bleaching viscose film is 2 minutes.

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1.4 Procedures
1.4.1 Prepare hot water washed-viscose film.
1.4.2 Place NaClO bath in ceramic tray.
1.4.3 Soak the viscose film in NaClO bath for 1 minute.
1.4.4 Remove from the NaClO bath and record the observations.
1.4.5 Repeat steps 1.4.1 to 1.4.4 using 2, 3, 4, and 5 minutes bleaching
time.

Table 3.25: Determination of the Optimum Concentration of NaClO Solution for
Viscose
Concentration of Immersion Time

Trial Observation
NaClO (%) (min)
1 5 1 Dirty white
2 5 2 Slightly dirty white
3 5 3 White
4 5 4 White
5 5 5 White
1.6 Analysis
Upon immersion of the samples at each trial, gradual changes of color can
be noticed from yellowish dirty white to white at a specific time period. After
3 minutes onwards, the sample remained white thus, removing the
undesirable colors and odors resulted from the previous processes.
1.7 Conclusion
The optimum time of bleaching to remove color and odor of the viscose film
is three (3) minutes.

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VIII. WASHING OF BLEACHED FILM
The bleached film is washed to remove the excess sodium hypochlorite in the
bleaching process.
1. Determination of the Optimum Washing Time of the Bleached Film

Ceramic Plate Film
Timer Water
1.2 Objectives
To determine the minimum washing time for the film where the hypochlorite
present has been removed.
1.3 Hypothesis
The minimum washing time for the film is 30 seconds that will allow the
removal of excess hypochlorite in the film.
1.4 Procedure
1.4.1 Prepare water in a basin.
1.4.2 Immerse the film into the water for 10 seconds.
1.4.3 Record the observations.
1.4.4 Repeat steps 1.4.1 to 1.4.3 using 20, and 30 seconds washing time.

Table 3.26: Determination of the Optimum Washing Time of the Bleached Film
Washing Time (seconds) Observation

10 It still has hypochlorite odor
15 Slightly has hypochlorite odor
20 Odorless
25 Odorless
30 Odorless
1.6 Analysis
In this process, the optimum washing time of the bleached film is
determined. It is necessary to wash the film in order to remove the odor of
the hypochlorite left in the film. As shown from the table above as the time

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increases the odor is more removed. The time 20 seconds is chosen since
it is the minimum time that has removed the odor of the hypochlorite.
1.7 Conclusion
The minimum time of washing is 20 seconds.
IX. PLASTICIZING
After removing the excess hypochlorite from the bleaching process, the film is
immersed in a glycerol bath in order to remove the brittleness of the film.
1. Determination of the Optimum Time of Immersion in Glycerol Bath

Ceramic Plate Film
Timer Water
1.2 Objective
To determine the time of immersion of the film in the glycerol bath.
1.3 Hypothesis
The appropriate time of immersion of the film is 20 seconds in the glycerol
bath that will allow the glycerol to plasticize the film.
1.4 Procedure
1.4.1 Prepare 60 ml of glycerol in a basin
1.4.2 Immerse the film into the glycerol bath for 5 seconds.
1.4.3 Record the observation.
1.4.4 Repeat steps 1.4.1 to 1.4.3 using 10, 15, and 20 seconds immersion
time.

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Table 3.27: Determination of the Optimum Immersion Time in the
Glycerol Bath
Immersion Time (seconds) Observation
5 The film is brittle
10 The film is soft and slightly elastic
15 The film is quite soggy and greasy
20 The film is soggy and greasy
1.6 Analysis
The immersion of the film in the glycerol bath gives the film its plastic
property. Glycerol adds to the mechanical plasticity of the film which is
responsible for the flexibility of the film. Stated in the table above the film
becomes softer, sag and increasing in its flexible. The film immersed 10
seconds in the glycerol bath is just enough to plasticize the film it adds
flexibility and does not sag the film.
1.7 Conclusion
The optimum immersion time in the glycerol bath is 10 seconds.
X. DRYING
Drying is for the removal of a significant amount of liquid absorbed by the film from
the post-conditioning it underwent.
1. Determination of the Optimum Drying Temperature of the Film
Oven Film Timer
1.2 Objective
To determine the temperature for drying needed to remove the excess
moisture absorbed by the film from the upstream processes.
1.3 Hypothesis
The appropriate drying temperature of the film is 110C that will allow the
removal of the excess moisture absorbed by the film from the upstream
processes.

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1.4 Procedure
1.4.1 Set the oven at 100°C
1.4.2 Dry the film in the oven for 3 minutes.
1.4.4 Repeat steps 1.4.1 to 1.4.3 using 110°C, 120°C, and 130°C drying
temperature.

Table 3.28: Determination of the Optimum Drying Temperature of the Film
Temperature (°C) Time (min.) Observation

100 1 The film is still wet
110 1 The film is damp
120 1 The film is quite dry
The film turned into
130 1
light brown
1.6 Analysis
In drying the film, the moisture is reduced and the dried sheet is formed.
The dried film for 1 min at 100°C. is still wet from the upstream processes,
while the film dried for 1 min at 130°C. has its color turned into light brown
which is an indication of the film being burnt. 120°C at 1 min results into a
quite dry film.
1.7 Conclusion
The optimum drying temperature is at 120°C
2. Determination of the Optimum Drying Time of the Film

Oven Film Timer
2.2 Objective
To determine the time for drying needed to remove the excess moisture
absorbed by the film from the upstream processes.

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2.3 Hypothesis
The appropriate drying time of the film is 3 mins that will allow the removal
of the excess moisture absorbed by the film from the upstream processes.
2.4 Procedure
2.4.1 Set the oven at 120°C
2.4.2 Dry the film in the oven for 1 minute.
2.4.4 Repeat steps 2.4.1 to 2.4.3 using 1.5, 2, 2.5 and 3 minutes drying
time.

Table 3.29: Determination of the Optimum Drying Time of the Film
Temperature (°C) Time (min.) Observation

120 1 The film is quite dry
120 1.5 The film is dry
120 2 The film turned into light brown
120 2.5 The film turned into brown
120 3 The film turned into dark brown
2.6 Analysis
In drying the film, the moisture is reduced and the dried sheet is formed.
The dried film for 1 min. is just quite dry from the upstream processes, while
the film dried for 3 mins. has shrunk and parts of it is burnt. 1.5 mins. is just
enough to dry the film and not burn it.
2.7 Conclusion
The optimum drying time is 1.5 mins.

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Figure 3.17: Experimental Procedure Flow Diagram

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EXPERIMENTAL DRY-RUN RESULTS
In this section, a dry-run was done using the optimum operating conditions that
were obtained from the experimentation. This was performed in order to calculate the
overall yield of the process.
Table 3.30: Experimental Dry-run Results

Process Composition Symbol Mass In Mass Out
Pineapple Crown PCL 374
Leaves
Accumulation Acc 0.0374
Cutting
Cut Pineapple 373.6270
CPCL
Crown Leaves
Total 373.6644 373.6644
Corn Cobs CC 125
Accumulation Acc 0.0125
Cutting
Cut Corn Cobs CCC 124.5423
Total 124.5548 124.5548
NaOH Pellets NaOH 269.0114
Water H2O 1225.4966
NaOH Dilution
NaOH Solution SH 1494.5080
Total 1494.5080 1494.5080
Pineapple Crown 498.1693
Leaves and Corn PCM
Alkaline Cobs Mixture
Hydrolysis NaOH Solution SHS 1494.5080
Digested Products DP 1992.6773
Total 1992.6773 1992.6773
Digestion Products DP 1992.6773
Filtered Alkali 447.7646
FAC
Filtration Cellulose
Black Liquor BL 1544.9128
Total 1992.6773 1992.6773
Filtered Alkali 447.7646
FAC
Cellulose
Xanthation CS2 CS2 156.7176
Alkali Cellulose 507.7640
ACX
Xanthate

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Side Product 96.7182

SPR
Reaction
Total 604.4822 604.4822
NaOH Pellets 38.0823
Water 723.5637
NaOH Dilution
NaOH Solution 761.6460
Total 761.6460 761.6460
Alkali Cellulose 507.7640
ACX
Xanthate
Alkalization NaOH Solution NaOH 761.6460
Viscose Solution VS 1269.4100
Total 1269.4100 1269.4100
Viscose Solution VS 1269.4100
Ripened Viscose 1269.4100
Ripening RVS
Solution
Total 1269.4100 1269.4100
Ripened Viscose 1269.4100
RVS
Solution
Filtered Viscose 1194.3866
Filtration FVS
Solution
Cake C 75.0234
Total 1269.4100 1269.4100
Sulfuric Acid SA 176.4160
Acid Bath Water H2O 122.1807
Dilution Acid Bath AB 298.5966
Total 298.5966 298.5966
Filtered Viscose 1194.3866
FVS
Solution
Acid Bath AB 298.5966
Casting
Acid Bath Film ABF 933.5361
Spent Acid Bath SAB 559.4471
Total 1492.932 1492.9832
Acid Bath Film ABF 933.5361
Hot Water HW 233.3840
Hot Water
Hot Washed Film HWF 1011.1708
Washing
Spent Hot Water 155.7494
SHWB
Bath

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Total 1166.9201 1166.9201

Hot Washed Film HWF 1011.1708
NaClO NaClO 252.7927
Bleaching Bleached Film BF 1039.6862
Spent NaClO Bath SNB 224.2772
Total 1263.9635 1263.9635
Bleached Film BF 1039.6862
Water WB 259.9216
Washing of
Washed Film WF 1161.1002
Bleached Film
Spent Water Bath SWB 138.5076
Total 1299.6078 1299.6078
Washed Film WF 1161.1002
Glycerol GB 290.2750
Plasticizing Plasticized Film PF 1184.1062
Spent Glycerol Bath SGB 267.2690
Total 1451.3752 1451.3752
Plasticized Film PF 1184.1062
Water Vapor WV 228.3662
Drying
Dried Film DF 955.7400
Total 1184.1062 1184.1062
From Table 3.30, it is shown that for 500 grams of raw material undergone into the
process of xanthation to produce viscose film, the total weight of the film produced is
955.74 grams. The total alpha-cellulose content of the final product is 375.125 grams
accounting to the 25:75 ratio of 48.79% and 83.77% alpha-cellulose of corncobs and
pineapple crown leaves, respectively. The total yield of the process with respect to alpha-
cellulose is 39.25%.

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SUMMARY OF THE OPTIMUM PARAMETERS
Table 3.31: Summary of Optimum Parameters
PROCESS PARAMETER OPTIMUM PARAMETER

PCL Length 20 mm.
Corncobs Particle
4.75 mm.
Diameter
Alkaline Hydrolysis Time 60 mins
Temperature 40 C
Reagent NaOH
Concentration 18%
Time 180 mins
Xanthation 35% grams of sample (175
Ratio to Raw Material
grams)
Concentration 5% NaOH
Alkalization
Time 180 mins
Ageing Time 180 mins
Concentration 24% H2SO4
Casting
Time 30 secs
Time 45 secs
Hot Water Washing
Temperature 50 C
Bleaching Time 3 mins
Washing Time 20 secs
Plasticizing Time 10 secs
Temperature 120C
Drying
Time 1.5 mins.
Table 3.31 shows the optimum parameters that were extracted from the
experimentation done that is used to yield the desired product for the production of
Viscose Film from Pineapple Crown Leaves and Corncobs.

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ANALYTICAL TESTS RESULTS
Efficiency of the Process

1. ATR-FTIR
To qualitatively asses the efficiency of the alkaline hydrolysis, xanthation,

alkalization and casting processes, Attenuated Total Reflectance – Fourier Transform
Infrared (ATR-FTIR) Spectroscopy was applied on recovered alkali cellulose, alkali
cellulose xanthate, viscose solution, and viscose film. The results obtained were
compared to the study, “Fourier Transform Infrared Spectroscopy for Natural Fibres”, by
Fan,M. et al. The resulting spectra were shown in the figures below:
Hemicellulose
C=O Band at 1735 cm-1
Lignin
C=C Aromatic at 1595 cm-1
C-O-C Ether Linkage at 1263 cm-1
Cellulose
C-C Ring Breathing Band at 1155 cm-1
C-O-C Glycoside Ether at 1105 cm-1
Figure 3.18: ATR-FTIR Spectra of Recovered Alkali Cellulose

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Hemicellulose
Lignin
Cellulose
Figure 3.19: ATR-FTIR Spectra of Produced Alkali Cellulose Xanthate
As shown from the FTIR Spectra in Figure 3.18 and 3.19, it is observed that the C-
C ring band at 1155 cm-1 and C-O-C glycoside ether at 1105 cm-1 are at peak, thus
indicates that the process successfully recovered the alkali cellulose and alkali cellulose
xanthate, and not degrade it. On the other hand, there is an absence of peak of C=O
band at 1735 cm-1 which indicates the loss of hemicellulose upon the process. It is also
noticeable that at 1595 cm-1 and 1263 cm-1 there is an absence of peak which shows
the loss of C=C Aromatic and C-O-C Ether Linkage, therefore an absence of lignin.

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Hemicellulose
Lignin
Cellulose
C-C Ring Breathing Band at 1155
cm-1
C-O-C Glycoside Ether at 1105
cm-1
Figure 3.20: ATR-FTIR Spectra of Produced Viscose Solution

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Hemicellulose
a
Lignin
Cellulose
Figure 3.21: ATR-FTIR Spectra of the product Viscose Film
Figures 3.20 and 3.21 shows the ATR-FTIR Spectra of Viscose solution and
Viscose Film, respectively. As observed from the spectra, high presence of cellulose is
present in the 1155 cm-1 and 1105 cm-1 wavelength. From the results, it can be concluded
that the applied conditions and the processes met its objective, i.e. to remove
hemicellulose and lignin, and to obtain highly concentrated cellulose and shows negligible
degradation.
2. Ultraviolet Visible Spectrometer (UV-Vis)

Aside from the ATR-FTR, UV-VIS is also used to qualitatively asses the
efficiency of the xanthation process. UV-Vis was applied on recovered alkali
cellulose xanthate. The resulting spectra were shown in the figures below:

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Figure 3.22: UV-Vis Spectra of the Produced Alkali Cellulose Xanthate
Figure 3.22 shows absorption peaks at wavelengths around 236 nm, which is
below 250 nm; and 305 nm, which is in between of 280 and 370 nm. In the study, “A Real-
Time Technique for Monitoring Cellulose Dissolution during the Xanthation Process”, by
He, L. et al, the range between 280 and 370 nm signifies presence of alkali cellulose
xanthate after the xanthation process produced with the set conditions. As compared in
the study of He, L. et al, the results can be concluded that the applied conditions in the
xanthation process met its objective, i.e. to remove hemicellulose and lignin, and to obtain
highly concentrated alkali cellulose xanthate.
Physical Test Results
The density of the viscose film was obtained using the water displacement method
wherein the sample was put in 50 ml water and the change in volume was recorded. The
results were shown in table 3.32. The average density obtained was 1.52 g/ml. From table
3.33, the density of the produced viscose film is in the range of the density for the standard
and existing viscose film.
Table 3.32: Density of Viscose Film
1 3.63 2.3 1.58
2 3.54 2.4 1.48
3 3.57 2.4 1.49
4 3.60 2.4 1.50
5 3.55 2.3 1.54
Average Density 1.52

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Figure 3.23, 3.24, and 3.25 shows the physical properties of the produced viscose
film tested by DOST-ITDR, and following is the table of the properties of the Standard,
Existing, and of the Produced Viscose Film. In figure 3.23, Tensile Strength, Tensile
Strength at Break, Elongation at Break, Elongation at Yield, and Yield Strength are
shown. Mean Specimen Dimension in mm is shown in figure 3.24; and Water Absorption
and remark on the Physical appearance is shown in figure 3.25.
Figure 3.23 Results of Tensile Strength Test of Viscose Film Tested by DOST-ITDR
Tensile Strength is the highest stress a material can support before failing. From
the figure 3.23, the produced viscose film has an average tensile strength of 10.263 MPa.
Compared from the Standard and Existing Properties shown in Table 3.33, the produced
Viscose Film wasn’t able to attain the value for the Tensile Strength. On the other hand,
from the same table, the Elongation at Break with an average of 22.99 MPa was able to
surpass the existing value and was in the range of standard value for the property of
viscose film. Elongation at break is the ratio of final length and initial length after the
sample has broken, while elongation at yield is ratio of the increased length with the initial
length at the yield point, or at the point until the sample still exhibits elasticity.
The results can be improved by using a controlled environment as done on an
industrial scale.

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Figure 3.24 Results of ASTM D882-09 Test for Viscose Film
From figure 3.24, the average thickness of the produced viscose film 7.201 mm or
7201 microns. As shown in table 3.33, the thickness of the produced film is thicker than
the standard and existing one. This can be accounted for the lack of proper material to
cast the film thinner as done in the industry.

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Figure 3.25 Results of ASTM D570 Test for Viscose Film
From figure 3.25 the average water absorption of the produced film is 114.60%.
As shown in table 3.33 this property is within the range of the existing value for the said
property. As an observation from the DOST-ITDR result, the produced fil exhibits no
changes in appearance after the 24-hour immersion test.

Project Study 113
Table 3.33 Properties of the Standard, Existing, and Produced Viscose Film
Property Standard(a) Existing(b) Produced

Tensile Strength
8 - 20 MPa(i) 10 MPa (g) 10.263
(MPa)
Tensile Strength at
- - 0.784
Break (MPa)
Elongation at Break
10-50 (f) 18 (g) 22.99
(%)
Yield Strength (MPa) - - 10.263
Elongation at Yield
- - 10.667
(%)
Water Absorption for
50% (equilibrium) 45-115%(c) 114.60%
24 hours
21.0 – 42.0 27.7 – 34.7 0.0358 mm = 35.8
Thickness
microns (g) microns microns
1.50 – 1.55 g/cm3 1.50 – 1.52 g/cm3
Density (d) (c) 1.52 g/ cm3
Transparent to
Appearance Transparent Translucent
Translucent
Wavelength peak
C-C Ring Breathing Band at 1155cm-1
FT-IR Analysis at 1155 cm-1 and
C-O-C Glycoside Ether at 1105 cm-1 (h)
1105 cm-1
Alkali cellulose xanthate below 250 Wavelength peak
UV-VIS Analysis nm; and between 280 and 370 nm at 236 nm and
wavelength (e) 305 nm
Source: (a) Film Properties of Plastics and Elastomers, 2nd Edition. Laurence W.
McKeen, Liesl K. Maey, (b) Uncoated Regenerated Cellulose Film, (c) Cellulose
(Regenerated Cellulose) Material Information, (d) Physico-mechanical properties of
materials (cellophane), (e) “A Real-Time Technique for Monitoring Cellulose
Dissolution during the Xanthation Process” by He, L. et al, (f) Polymer Chemistry,
2000. Mechanical Property. Dr. Whisnant, D., (g) MatWeb LLC Material Property Data.
Goodfellow Cellophane, Rayophane Regenerated Cellulose Film, (h) “Fourier
Transform Infrared Spectroscopy for Natural Fibres”, by Fan,M. et al, and (i) Food
Packaging: Principle and Practice, Third Edition. Gordon L. Robertson.

Project Study 114
EXPERIMENTAL STUDY RECOMMENDATIONS
This research can be further improved and investigated. Hence, the researchers
recommend the following:
 To utilize other source of cellulose
 To consider other essential parameters that may influence the process
 To use other laboratory equipment that will be of great contributor in increasing the
process yield, impose uniform thickness for the film, and imply equal density for
the film
 To utilize other reagents and parameters for xanthation, and film forming
 To evaluate other significant mechanical properties of the produced viscose film
 To apply other analytical tests that will confirm the presence and measure the
amount of the target substances

Project Study 115

Methodology and Data Presentation: Pamantasan NG Lungsod NG Maynila

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Methodology and Data Presentation: Pamantasan NG Lungsod NG Maynila

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PAMANTASAN NG LUNGSOD NG MAYNILA

College of Engineering and Technology

Production of Viscose Film via Xanthation of Alkali Hydrolyzed Pineapple

 Philippine Statistics Authority (PSA)– Quezon Avenue

Production of Viscose Film via Xanthation of Alkali Hydrolyzed Pineapple

The experimental method is the scientific undertaking of the research. In here,

 Pamantasan ng Lungsod ng Maynila (PLM) Medicine Laboratory

 Adamson University Technology Research and Development Center

 De La Salle University (DLSU) Chemistry Instrument and Research

 Department of Science and Technology – Industrial Technology

Production of Viscose Film via Xanthation of Alkali Hydrolyzed Pineapple

Figure 3.1: Conceptual Framework of the Study

Production of Viscose Film via Xanthation of Alkali Hydrolyzed Pineapple

ANALYSIS OF CONCEPTUAL FRAMEWORK

Production of Viscose Film via Xanthation of Alkali Hydrolyzed Pineapple

Figure 3.2: Theoretical Framework of the Study

Production of Viscose Film via Xanthation of Alkali Hydrolyzed Pineapple

ANALYSIS OF THEORETICAL FRAMEWORK

After producing the alkali cellulose, it is converted to cellulose xanthate through

The obtained cellulose xanthate is the converted to viscose solution by alkalization.

Production of Viscose Film via Xanthation of Alkali Hydrolyzed Pineapple

SUMMARY OF VARIATION PARAMETERS

Table 3.1: Summary of Variation Parameters

Production of Viscose Film via Xanthation of Alkali Hydrolyzed Pineapple

Production of Viscose Film via Xanthation of Alkali Hydrolyzed Pineapple

The researchers devised an experimental method to obtain Viscose Film from

Production of Viscose Film via Xanthation of Alkali Hydrolyzed Pineapple

OBJECTIVES OF THE EXPERIMENTAL STUDY

Property Standard(a) Existing(b) Produced

Appearance Transparent Transparent to Translucent

Production of Viscose Film via Xanthation of Alkali Hydrolyzed Pineapple

 To determine the optimum operating conditions in the alkaline hydrolysis,

 To determine the properties of the chemical intermediates using physical,

 To identify the equivalent unit operations or unit processes and industrial

Production of Viscose Film via Xanthation of Alkali Hydrolyzed Pineapple

EXPERIMENTAL PROCESS FLOW DIAGRAM

Figure 3.3: Experimental Process Flow Diagram of the Study

Production of Viscose Film via Xanthation of Alkali Hydrolyzed Pineapple

LIST OF REQUIRED REAGENTS AND LABORATORY APPARATUSES

Table 3.3: List of Required Reagents and Laboratory Apparatuses

Process Required Reagents Laboratory

Production of Viscose Film via Xanthation of Alkali Hydrolyzed Pineapple

PREPARATION OF RAW MATERIALS AND REAGENTS

Prior to the experimentation of the pineapple crown leaves and corncobs,

The researchers went to the Adamson University Technology Research and

Production of Viscose Film via Xanthation of Alkali Hydrolyzed Pineapple

Table 3.4: Alpha-Cellulose Content of the Raw Materials

Raw Material %α-cellulose

B. Determination of the Bulk Density

1. Materials and Apparatuses

3.1.1 Prepare 5 sets of 10 pieces pineapple crown leaves.

Production of Viscose Film via Xanthation of Alkali Hydrolyzed Pineapple

3.2 For Corncobs

4. Data and Calculation

Table 3.5: Bulk Density of Pineapple Crown Leaves

Trial Mass (g) Change in Volume (mL) Bulk Density (g/mL)

𝑀𝑎𝑠𝑠 𝑜𝑓 𝑃𝐶𝐿 (𝑔)

(0.844 + 1.049 + 0.854 + 0.924 + 0.797) 𝑔/𝑚𝐿

Production of Viscose Film via Xanthation of Alkali Hydrolyzed Pineapple

Table 3.6: Bulk Density of Corncobs

Trial Mass (g) Change in Volume (mL) Bulk Density (g/mL)

𝑀𝑎𝑠𝑠 𝑜𝑓 𝐶𝑜𝑟𝑛𝑐𝑜𝑏𝑠 (𝑔)