Experimental Study: Pamantasan NG Lungsod NG Maynila

PAMANTASAN NG LUNGSOD NG MAYNILA
University of the City of Manila

College of Engineering and Technology
Department of Chemical Engineering
EXPERIMENTAL
STUDY
METHODS OF RESEARCH
Data gathering is an essential step for ensuring the feasibility of the study. Here, the
researchers have gathered the data and information regarding the profile, properties and
availability of the raw material, the operating conditions that will yield high results, the market
viability and the standards properties of the desired product as well as the available testing
facilities were collected. The descriptive and experimental method were used to obtain all
necessary data and information needed in this study.
A. Descriptive Method
Descriptive research was conducted to gather information about the profile,
properties, availability and current status for both the copra meal (raw material) and alkyd
resin (product). The researchers gathered all the necessary information through electronic
sources, government websites and government agencies.
The historical data of the demand and supply of alkyd resin were gathered from
Philippine Statistics Authority. The information gathered were used specifically in the market
study to determine the market feasibility of the product. Also, the yearly production of coconut
in the Philippines as well as the properties and characteristics of copra meal were gathered
from Philippine Coconut Authority (PhilCoA). The information gathered were used as a basis
on the determination of the current amount of copra meal produced in the country and as a
basis on the typical composition of the raw material. Moreover, the researchers tried to gather
data on the standard properties of alkyd resin however, only Alkyd-based Metal Primer (for
Paint and Varnishes) Specifications were obtained. Lastly, the researchers made use of the
internet to access and collect several electronic books, journals, and theses that served as
the references and foundation of the study.
Esterification of Hydrolyzed Copra (Cocos nucifera) Meal for the Production of

PROJECT
Alkyd Resin 43
Dionisio, C.P., Fulugan, C.L., Redublo, A.P. STUDY
B. Experimental Method
The experimental method is the scientific undertaking of the research. The researchers
conducted the experimental study in the laboratory by considering different parameters
obtained on literature and studies to come up with the best quality of the product. The
produced alkyd resin was then tested through various testing facilities.
All of the experimentations involved in the study, which includes the preparation and
analysis of copra meal, pre-treatment and conditioning of copra meal, mannitol production
and alkyd resin production, were carried out in PLDTSFH-CHE Laboratory at Pamantasan ng
Lungsod ng Maynila (PLM).
The raw material and product were characterized in different testing facilities. First,
the proximate analysis of the raw material was conducted at the laboratory of Department of
Agriculture to determine moisture, crude oil, crude fiber, ash, and carbohydrate content of
copra meal. Next, the testing for the Fourier Transform Infrared Spectroscopy (FTIR) of
mannose, mannitol and the alkyd resin were carried out at De La Salle University Chemistry
Instrument and Research Testing Center and Adamson University Chemistry Laboratory. FTIR
analysis was performed to check the presence of chemical bonds and functional groups in
the samples. Finally, testing for the High-Performance Liquid Chromatography (HPLC) of alkyd
resin were carried out at University of Sto. Tomas - Analytical Services Laboratory. HPLC is a
technique used to separate, identify, and quantify each component in a mixture.

PROJECT
Alkyd Resin 44
Figure 3.1. Conceptual Framework
Esterification of Hydrolyzed Copra (Cocos nucifera) Meal for the Production of Alkyd Resin
Dionisio, C.P., Fulugan, C.L., Redublo, A.P.
PROJECT STUDY 45
ANALYSIS OF CONCEPTUAL FRAMEWORK
The conceptual framework is the research paradigm which shows the overview of the
research study, and includes the methods applied to achieve the research objectives. In order
to determine the feasibility of the research project, three sections of the study were evaluated:
(1) Market Study, (2) Experimental Study, and (3) Technical Study.
First, data gathering was conducted wherein the researchers visited several
government institutions, and utilized various researches, books, and websites. The raw
material profile (status, generation, sources, and properties of copra meal), the alkyd resin
profile and its market demand and supply, the existing and conventional processes of alkyd
resin production, as well as the mechanism of reactions were collected. Moreover, various
journals provided insights that served as the foundation and basis of the literature and
experimentation in the study.
Next, the market study was conducted to analyze and determine the marketability of
the product, alkyd resin. Historical data of market demand and supply were gathered and
projected to evaluate its potential to be sold in the local market, and to determine the market
share and plant rated capacity. Marketing program were developed to meet the company’s
objectives, mission, and goals within the specific timeframe. Moreover, marketing strategies
were developed to let the product penetrate the local market and compete with the existing
products. As the marketability of the alkyd resin was proven, the experimentation was
conducted after.
Then, the experimental study was done in a laboratory scale. The copra meal was
analyzed to determine its moisture, oil, and carbohydrate content. Several process
parameters were varied to optimize the quality and quantity of the product produced. The
alkyd resin product was characterized using FTIR, HPLC, and its physical and chemical
properties were determined, which were compared to the standard and existing product
properties. The optimum parameter values from the experiment were used in the scaled-up
designs in the technical study.

PROJECT
Alkyd Resin 46
Lastly, in the technical study, the detailed manufacturing process (DMP) was
presented to give an overview on how the manufacturing plant will operate. The input and
output of materials in each process were calculated through material and energy balances.
Moreover, suitable equipment for each process were chosen and designed together with the
piping systems, instrumentation and process control, and the wastewater treatment facility of
the manufacturing plant. Safety was also discussed as part of plant operations.
The completion of the market study, experimental study, and technical study
established the feasibility of the study.

PROJECT
Alkyd Resin 47
Figure 3.2. Theoretical Framework

PROJECT
Alkyd Resin 48
ANALYSIS OF THEORETICAL FRAMEWORK
The framework shown above presents the major parts in the experimental study: (1)
pretreatment of copra meal, (2) mannitol production, and (3) alkyd resin production, its sub-
process as well as the variation of parameters used in the study.
The pretreatment of copra meal consists of drying, grinding, and leaching. Drying was
performed on copra meal to reduce its moisture content by varying drying conditions such as
time and temperature. Then, it was grinded to reduce its particle size wherein the grinding
time was determined. Lastly, leaching was done to remove residual oil in the copra meal by
varying leaching conditions such as solvent type, ratio of copra meal to solvent, temperature,
and time. The oil content of the defatted copra meal after leaching was determined using
Soxhlet Apparatus to calculate the amount of oil removed.
The second part of the experimentation is the mannitol production which includes
hydrolysis, neutralization, and reduction. In hydrolysis, mannan was reacted with an acid to
produce the hydrolysate. Parameters such as acid type, acid concentration, ratio of defatted
copra meal to acid, temperature, and time were varied. Then, hydrolysate was neutralized to
remove protein from copra meal and increase its pH by varying the type and amount of
neutralizing agent used. It was then filtered to remove crude fiber, isolating the mannose in
liquid form. The total reducing sugar content of mannose was determined using Benedict’s
Solution test. Afterwards, mannose was reacted with sodium borohydride to produce
mannitol, and parameters such as ratio of sodium borohydride to mannose, temperature, and
time were varied. To determine if mannitol was produced, the melting point and hydroxyl value
was tested, and FTIR and HPLC analysis was performed.
The last part of the experimentation is the alkyd resin production which consists of
esterification. Mannitol was reacted with phthalic anhydride and benzoic acid to produce a
polyester, alkyd resin. The ratio of the three reactants, process temperature, and time were
varied in the study to determine the optimum conditions for this process.

PROJECT
Alkyd Resin 49
Table 3.1 Summary of Variation of Parameters

PROCESS PARAMETER UNIT USED ON STUDIES VARIATIONS
Temperature C 60, 70 50, 60, 70, 80, 90
Drying
Time hr 2-4, 6 1, 2, 3, 4, 5
Grinding Grinding Time min 10 2, 4, 6, 8, 10
Acetone, Hexane, Chloroform, Acetone,
Type of Solvent Ether, Isopropanol, Petroleum Ether,
Ethanol Isopropanol, Hexane
Leaching Copra Meal to
w:v 1:5 1:1, 1:2, 1:3, 1:4, 1:5
Solvent Ratio
Temperature C 25, 50 40, 50, 60, 70, 80
Time min 15 15, 30, 45, 60, 75
Type of Acid HCl, H2SO4, H3PO4 HCl, H2SO4, H3PO4
0.20, 1.00, 1.80, 2.60,
Concentration % w/v 0.05
3.40
Hydrolysis Defatted Copra Meal 1:4, 1:6 1:8, 1:10,
w:v 1:10
to Acid Ratio 1:12
Temperature C 100, 148 80, 90, 100, 110, 120
Time min 30 30, 60, 90, 120, 150
Neutralization Type Na2CO3 Na2CO3, Ca(OH)2, KOH
Mannose to Sodium 1:0.50, 1:0.75, 1:1,
molar
Borohydride Ratio 1:1.25, 1:1.50
Reduction
Temperature C Room temperature 25, 30, 40, 50, 60
Time min 50, 120 30, 60, 90, 120, 150
0, 10, 20, 30, 40, 50,
Evaporation Time min 60, 70, 80, 90, 100,
110, 120, 130, 140
Palmitic Acid, Benzoic
Alkyd Resin Modifier Benzoic Acid
Acid, Oleic Acid
Mannitol Phthalic
1:1:1, 1:1:2, 1:1:3,
Anhydride to Oleic molar -
1:2:1, 1:3:1
Esterification Acid Ratio
220, 230, 240, 250,
Temperature C 220-250
260
60, 120, 180, 240,
Time min
300
Table 3.1 shows the summary of variation of parameters based on literature and
studies. These variations of parameters will be used in the experimental study to determine
the most appropriate or optimal conditions in synthesizing alkyd resin from copra meal.

PROJECT
Alkyd Resin 50
EXPERIMENTAL METHOD
The experimental method was developed to produce alkyd resin from copra meal. In order
to achieve the desired product quality and to determine the most suitable operating
conditions for each process, several parameter variations obtained from different literature
and studies were considered.
Before the experiment proper, the carbohydrate, moisture, and oil content of copra meal
were determined by proximate analysis. The experimental method is divided into three parts.
First part is the pretreatment of the copra meal which consists of drying, grinding, and
leaching. The amount of moisture content after drying was determined by oven drying method
while amount of oil removed was determined through Soxhlet Method. Next part is the
mannitol production which comprises of hydrolysis, neutralization, reduction, and
evaporation. The hydroxyl value of mannitol was tested, as well as the FTIR analysis were
performed. Last part is the alkyd resin production is eesterification. Optimum parameter in
each process was determined by the highest percentage yield accompanied by qualitative
determination.
Qualitative analysis of alkyd resin such as Fourier Transform Infrared Spectroscopy (FTIR)
and High Performance Liquid Chromatography (HPLC) and quantitative analysis such as
viscosity, specific gravity, acid value, non-volatile content, and hydroxyl value were determined
to ensure the validity of the optimum parameters obtained in the experiment.
A dry-run of the whole experiment using the optimum parameters was done to determine
if there were any significant changes in the final product. The results from the laboratory-scale
experimentation was used in alkyd resin production in industrial scale.

PROJECT
Alkyd Resin 51
OBJECTIVES OF THE EXPERIMENTAL STUDY
A. General Objectives
To produce alkyd resin from copra meal that conforms to the properties of the standard
and commercial products shown in Table 3.2.
Table 3.2. Standard, Existing, and Proposed Properties of Alkyd Resin

PARAMETER STANDARD EXISTING[3] PROPOSED
Color Pale Yellow Amber Pale Yellow
Clear viscous
Appearance Clear liquid Clear liquid
liquid [2]
Specific Gravity @ 27°C 0.940-0.960 0.9328 0.950
Viscosity @ 25°C - 472.00 stokes 472 Stokes
Flash Point 24°C [2] 35 °C 31°C
Acid Value 8 mg KOH/g [1] 6.39 mg KOH/g 7.7 mg KOH/g
Nonvolatile Content - 50.08 % 50.08 %
Hydroxyl Value 45mg KOH/g [1] 45mg KOH/g
1730 cm–1 (C=O), 1270 cm–1 (OH),
FTIR Peak Value (cm-1)
1375 cm–1 (C–O), 1081 cm–1 (C–O)
Sources:
[1] John Wiley & Sons. Resins for Surface Coatings: Alkyd & Polyesters, Volume II 2nd ed.
[2] National Industrial Chemicals Notification
[3] Pacific Resins, Inc.
B. Specific Objectives
To determine the optimal operating conditions for each processes that would produce
alkyd resin with properties conforming to the standard and commercial product;
To calculate the percent yield of each processes that will be used as basis in upscaling
to industrial set-up;
To determine if the desired products from hydrolysis, reduction, and esterification were
produced by evaluating the peaks in the FTIR spectroscopy;
To identify the equivalent unit operation and equipment of each laboratory process and
apparatus.

PROJECT
Alkyd Resin 52
EXPERIMENTAL STUDY
The experimental method of the study focused on performing the process in a laboratory
scale set-up. The experiment is divided into the following sections:
I. Raw Material
I-1. Copra Meal Collection
I-2. Characterization of Copra Meal
A. Proximate Analysis (Carbohydrate Content)
B. Equilibrium Moisture Content
II. Pretreatment of Copra Meal
II- 1. Drying
II-2. Grinding
II-3. Leaching
III. Mannitol Production
III-1. Hydrolysis
III-2. Neutralization
III-3. Reduction
III-4. Evaporation
IV. Alkyd Resin Production
IV-1. Esterification
V. Characterization of Alkyd Resin
1. Physical and Chemical Properties
2. FTIR of Alkyd Resin
3. HPLC

PROJECT
Alkyd Resin 53
LIST OF REAGENTS AND LABORATORY APPARATUS AND EQUIPMENT
Reagents
The reagents used in the experimentation are summarized in Table 3.3 shown below.
The reagents were obtained from Chemistry and Chemical Engineering Laboratory, PLM and
purchased from Alyson’s Chemicals Enterprises Inc, located at 1425 Gregorio Araneta
Avenue, Quezon City and RB Chemodities in Bambang, Manila.
Table 3.3. Reagents and their Corresponding Properties
Reagent Process Function
Solvents
 Acetone
 Petroleum ether Dissolves residual oil from copra
Leaching
 Isopropanol meal
 Hexane
 Chloroform
Acids
 Phosphoric Catalyzes the hydrolysis of beta-
Hydrolysis
 Hydrochloric glycosidic bonds in copra meal
 Sulfuric
Bases
 Calcium Hydroxide Neutralizes any remaining acid in
Neutralization
 Sodium Carbonate the hydrolysis step
 Potassium Hydroxide
Quantitative Analysis of Used to quantify the amount of
Benedict’s Reagent
Mannose reducing sugars in the hydrolysate
Used to reduce mannose to
Sodium Borohydride Reduction
mannitol
Reacts with mannitol to form
Phthalic Anhydride
polyester, alkyd resin
Monobasic Acid Esterification
 Benzoic Acid Acts as a modifier in alkyd resin
 Oleic Acid production
 Stearic Acid

PROJECT
Alkyd Resin 54
Laboratory Apparatus and Equipment
The laboratory apparatus used in the experimentation with their corresponding

description are presented in Table 3.4.
Table 3.4. List of Laboratory Apparatus
Laboratory Laboratory
Description Description
Apparatus Apparatus
1000mL,
3-neck round A laboratory
bottom flask glassware used as Oven
the reacting vessel
in hydrolysis,
reduction, and Used for drying the
polymerization steps copra meal
1000mL in volume
with 3 ports for
material, and
equipment input
Beaker Blender
Container used for

Used to reduce the
measuring, stirring,
particle size of the
mixing and heating
dried copra meal
liquids
Analytical Balance Used to determine

Sieve
the average particle
size of copra meal
A digital instrument
through sieve
that is used to
analysis.
measure the mass
It is also used to
of an object in S.I
separate coarse
unit (grams)
particle (greater
than 0.250mm) to
the desired.

PROJECT
Alkyd Resin 55
Hot Plate
Erlenmeyer Flask
Electrically-powered
Used to measure,
device used for
mix, and store liquid
heating with
and suitable for
magnetic stirrer.
heating liquids
Stirring Rod Thermometer

Used to stir liquids, Used to measure
mixtures, and temperature of the
solutions during mixtures during the
reaction reaction
Filter Paper A piece of porous Funnel

Used to efficiently
paper used for
transfer liquids from
filtering defatted
one container to
copra meal from the
another with small
spent solvent, and
opening and hold
mannose from the
the filter paper
neutralized sugar
during filtration
solution
Stopwatch
Condenser
Used to measure the
Used for liquefying amount of time a
recovered solvent certain process
occurred
Vials Syringe
Used to transfer
Used to store liquids small volume of
and reagents liquids from one
container to another

PROJECT
Alkyd Resin 56
EXPERIMENTAL PROCEDURE
I. RAW MATERIAL
I-1. Copra Meal Collection
The copra meal to be used in the experimentation was obtained from Brgy. Calamias,
Ibaan, Batangas through Mr. Raul C. Alcazar.
Figure 3.3. Raw Material Collection
I-2. Characterization of Copra Meal

A. Proximate Analysis
The copra meal composition such as moisture, crude oil, crude fiber, and ash was
analyzed though proximate analysis in Department of Agriculture. The results of the analysis
is summarized in the Table 3.5. According to Khuwijitjaru, P., et.al (2012), total carbohydrate
content is the difference in proximate analysis (moisture, protein, fat/oil, crude fiber, and ash).
Table 3.5. Proximate Analysis of Copra Meal

Composition Percent Content (%)
Moisture 12.3
Oil/Fat 9.3
Crude Fiber 13.8
Protein 19.4
Ash 5.6
Carbohydrates 39.6
Source: Department of Agriculture, 2018

PROJECT
Alkyd Resin 57
From Table 3.5, 39.6% of carbohydrates is the desired component from copra meal. It
was pretreated to remove excess moisture and residual oil through drying and leaching,
respectively. Afterwards, it was hydrolyzed to remove crude fiber which was the unreacted
component during the reaction. Moreover, it was subjected to neutralization to precipitate out
the protein.
B. Equilibrium Moisture Content
Prior to the experimentation, the equilibrium moisture content of copra meal was
determined. It is the moisture level where the particle neither gains nor loses moisture since
it is at equilibrium with the relative humidity of the surrounding environment. As shown in the
equation below, it is defined as the difference between the total moisture content and free
moisture content.
𝑿∗ = 𝑿𝑻 − 𝑿
Where: 𝑋 = Free Moisture Content
𝑋𝑇 = Total Moisture Content
𝑋 ∗ = Equilibrium Moisture Content
According to the proximate analysis done by Department of Agriculture Laboratory, the

total moisture content of copra meal is 12.3% while the equilibrium moisture content is about
4-5% (Pestaño, 2016).
Determination of Equilibrium Moisture Content of Copra Meal
B-1. Materials and Apparatus

MATERIAL APPARATUS
 Copra Meal  Analytical Balance
 Oven Dryer
 Digital Timer
 Aluminum Foil

PROJECT
Alkyd Resin 58
B-2. Laboratory Set-up
Figure 3.4. Laboratory Set-up for Equilibrium Moisture Content Determination
B-3. Objective
To determine the equilibrium moisture content of copra meal which will be used as a
basis for obtaining the optimum drying parameters for the pretreatment of the raw materials.
B-4. Hypothesis
The equilibrium moisture content of copra meal will be in the range of 4-5%
B-5. Procedure
1. Prepare 50 grams of copra meal and dry at 70C.
2. Weigh and record the mass of the dried copra meal every 30 minutes.
3. Stop the drying process when the difference in the mass of dried copra meal is
negligible.

PROJECT
Alkyd Resin 59
B-6. Data and Results

Table 3.6. Determination of Equilibrium Moisture Content of Copra Meal
Mass (g)
Time (hr)
Trial 1 Trial 2 Trial 3
0 50.0226 50.2884 50.1634
0.5 49.5629 50.1732 49.7510
1.0 49.3185 50.0640 49.4924
1.5 48.9720 49.6219 49.2661
2.0 48.5622 49.3617 49.0489
2.5 48.3992 49.0719 48.8605
3.0 48.0503 48.5691 48.4789
3.5 47.6832 48.1673 47.8430
4.0 47.0748 47.8445 47.5541
4.5 46.8331 47.3018 47.1980
5.0 46.3565 46.7643 46.7635
5.5 46.0764 46.5494 46.4892
6.0 45.9188 46.3107 46.1141
6.5 45.9047 46.2635 46.0502
Free Moisture Removed at 6.5 hours (g) 4.1179 4.0249 4.1132
Free Moisture Removed at 6.5 hours (%) 8.2321 8.0036 8.1996
Average Free Moisture Content (%) 8.1451
EQUILIBRIUM MOISTURE CONTENT 4.1549
B-7. Sample Calculation
𝐷𝑖𝑓𝑓𝑒𝑟𝑒𝑛𝑐𝑒 = 𝑀𝑎𝑠𝑠(𝑡−1) − 𝑀𝑎𝑠𝑠𝑡

𝐷𝑖𝑓𝑓𝑒𝑟𝑒𝑛𝑐𝑒 = 45.9188𝑔 − 45.9047𝑔 = 0.0141𝑔
𝑀𝑎𝑠𝑠𝑖𝑛𝑖𝑡𝑖𝑎𝑙 − 𝑀𝑎𝑠𝑠𝑓𝑖𝑛𝑎𝑙
𝐹𝑟𝑒𝑒 𝑀𝑜𝑖𝑠𝑡𝑢𝑟𝑒 𝐶𝑜𝑛𝑡𝑒𝑛𝑡 = 𝑥 100%
𝑀𝑎𝑠𝑠𝑖𝑛𝑖𝑡𝑖𝑎𝑙
50.0226𝑔 − 45.9047𝑔
𝐹𝑟𝑒𝑒 𝑀𝑜𝑖𝑠𝑡𝑢𝑟𝑒 𝐶𝑜𝑛𝑡𝑒𝑛𝑡 = 𝑥100% = 8.2321%
50.0226𝑔
8.2321% + 8.0036% + 8.1996%
𝐴𝑣𝑒𝑟𝑎𝑔𝑒 𝐹𝑟𝑒𝑒 𝑀𝑜𝑖𝑠𝑡𝑢𝑟𝑒 𝐶𝑜𝑛𝑡𝑒𝑛𝑡 = = 8.1451%
3
PROJECT
Alkyd Resin 60
For equilibrium moisture content,

𝑋 = 𝑋𝑇 − 𝑋 ∗
𝑋 ∗ = 𝑋𝑇 − 𝑋
𝑋 ∗ = 12.3% − 8.1451%
𝑋 ∗ = 4.1549%
B-8. Analysis
The obtained free moisture content of copra meal from the three trials are 8.2321%,
8.0036% and 8.1996% with an average value of 8.1451%. These low values of moisture
content indicates that the raw material is safe for long-term storage. However, according to
Geankoplis (1993), the moisture content of the material must be reduced to avoid microbial
growth.
The calculated value for the equilibrium moisture content based on the free moisture
content and the total moisture content is 4.1549% which falls between the typical ranges of
4-5% for copra meal.
B-9. Conclusion
The equilibrium moisture content of copra meal is 4.1549 %
II. PRETREATMENT OF COPRA MEAL

II-1. Drying of Copra Meal
The effectiveness of drying processes can have a large impact on product quality and
process efficiency in subsequent processes (Parikh, 2014). Raghavan, V. & Dev, S. (2012)
also stated that drying is important because of ease of handling due to reduction in bulk and
reduction in handling costs, and dry biomaterials are less prone to microbiological
degradation in storage. Thus, copra meal with an initial moisture content of 12.3% or 30.75
grams moisture content in 250 grams of copra meal was dried.

PROJECT
Alkyd Resin 61
Optimum parameters such as drying temperature and time were determined based on
the equilibrium moisture content, wherein it is desirable to have a final moisture content close
to the equilibrium content.
Materials and Apparatus

MATERIAL APPARATUS
 Oven Dryer
 Digital Timer
 Aluminum Foil
Laboratory Set-up
Figure 3.5. Laboratory Set-up for Drying of Copra Meal

PROJECT
Alkyd Resin 62
A. Determination of Optimum Drying Temperature of Copra Meal

A-1. Objective
To determine the optimum drying temperature of copra meal that would result to a
lower final moisture content.
A-2. Hypothesis
The optimum drying temperature is 70°C.
A-3. Procedure
1. Weigh 5 sets of 250 grams copra meal and dry each trials under 50°C, 60°C, 70°C,
80°C and 90°C respectively for 1 hour.
2. Weigh and record the mass of dried copra meal after drying.
A-4. Data and Results
Table 3.7. Determination of Optimum Drying Temperature
Trial 1 2 3 4 5
Mass of Copra Meal (g) 250 250 250 250 250
Initial Moisture Content (g) 30.75 30.75 30.75 30.75 30.75
Initial Moisture Content (%) 12.3 12.3 12.3 12.3 12.3
Temperature (⁰C) 50 60 70 80 90
Time (hr) 1 1 1 1 1
Mass of Dried CM (g) 246 243 242 240 239
Mass of Water Removed (g) 4 7 8 10 11
Final Moisture Content (g) 26.75 23.75 22.75 20.75 19.75
Final Moisture Content (%) 10.75 9.50 9.10 8.30 7.90
Figure 3.6. Dried Copra Meal under Different Drying Temperatures

PROJECT
Alkyd Resin 63
A-5. Sample Calculation
𝐹𝑖𝑛𝑎𝑙 𝑀𝑜𝑖𝑠𝑡𝑢𝑟𝑒 𝐶𝑜𝑛𝑡𝑒𝑛𝑡 (%)

𝐼𝑛𝑖𝑡𝑖𝑎𝑙 𝑀𝑜𝑖𝑠𝑡𝑢𝑟𝑒 𝐶𝑜𝑛𝑡𝑒𝑛𝑡 − 𝑀𝑎𝑠𝑠 𝑜𝑓 𝑊𝑎𝑡𝑒𝑟 𝑅𝑒𝑚𝑜𝑣𝑒𝑑
= 𝑥100%
𝑀𝑎𝑠𝑠 𝑜𝑓 𝐶𝑀
30.75𝑔 − 10𝑔
𝐹𝑖𝑛𝑎𝑙 𝑀𝑜𝑖𝑠𝑡𝑢𝑟𝑒 𝐶𝑜𝑛𝑡𝑒𝑛𝑡 (%) = 𝑥100% = 8.30%
250𝑔
A-6. Analysis
After drying at different temperatures from 50C to 90C, it was observed that there is
no noticeable change in appearance of copra meal. The selection of the optimum drying
temperature is based on the final moisture content of the copra meal. The table shows that
there is a decrease in the final moisture content as the drying temperature increases giving
drying temperatures of 80C and 90C with the lowest amount of final moisture content.
However, among those two drying temperatures, the difference on the final moisture content
is very low at 0.40%, showing a minimal increment. Thus, the selected optimum drying
temperature is at 80C.
A-7. Conclusion
The optimum drying temperature is at 80C with a final moisture content of 8.30%
B. Determination of Optimum Drying Time of Copra Meal

B-1. Objective
To determine the optimum drying time of copra meal until constant weight was
achieved.
B-2. Hypothesis
The optimum drying time is 4 hours.

PROJECT
Alkyd Resin 64
B-3. Procedure
1. Weigh 5 sets of 250 grams copra meal and dry each trial at 80C for 1hr, 2hrs, 3hrs,
4hrs and 5hrs respectively.
2. Weigh and record the mass of dried copra meal after drying.

Table 3.8. Determination of Optimum Drying Time
Trial 1 2 3 4 5
Mass of CM (g) 250 250 250 250 250
Initial Moisture Content (g) 30.75 30.75 30.75 30.75 30.75
Initial Moisture Content (%) 12.3 12.3 12.3 12.3 12.3
Time (hour) 1 2 3 4 5
Mass of Dried CM (g) 240 236 233 230 230
Mass of Water Removed (g) 10 14 17 20 20
Final Moisture Content (g) 20.75 16.75 13.75 10.75 10.75
Final Moisture Content (%) 8.30 6.70 5.50 4.30 4.30
Figure 3.7. Dried Copra Meal under Different Drying Time

𝐹𝑖𝑛𝑎𝑙 𝑀𝑜𝑖𝑠𝑡𝑢𝑟𝑒 𝐶𝑜𝑛𝑡𝑒𝑛𝑡 (%)
𝐼𝑛𝑖𝑡𝑖𝑎𝑙 𝑀𝑜𝑖𝑠𝑡𝑢𝑟𝑒 𝐶𝑜𝑛𝑡𝑒𝑛𝑡 − 𝑀𝑎𝑠𝑠 𝑜𝑓 𝑊𝑎𝑡𝑒𝑟 𝑅𝑒𝑚𝑜𝑣𝑒𝑑
= 𝑥100%
𝑀𝑎𝑠𝑠 𝑜𝑓 𝐶𝑀

PROJECT
Alkyd Resin 65
30.75𝑔 − 20𝑔
𝐹𝑖𝑛𝑎𝑙 𝐹𝑟𝑒𝑒 𝑀𝑜𝑖𝑠𝑡𝑢𝑟𝑒 𝐶𝑜𝑛𝑡𝑒𝑛𝑡 (%) = 𝑥100% = 4.30%
250𝑔
B-6. Analysis
It was observed that there is no noticeable change in appearance of copra meal after
drying at different drying time at a temperature of 80C. The selection of the optimum drying
time is based on the final moisture content of the copra meal. The table shows that there is a
decrease in the moisture content as the drying time increases resulting into lowest amount of
final moisture content at drying time of 4 hours and 5 hours. However, among those two, 4
hours was selected as the optimum drying time since constant weight was already achieved
after 4 hours of drying.
B-7. Conclusion
The optimum drying time for copra meal is 4 hours having a final moisture content of
4.30%
II-2. Grinding of Dried Copra Meal
Size reduction is a process of reducing large solid unit masses to small unit masses,
coarse particles or fine particles, which leads to increase of surface area for reaction (Archana,
K., et.al., 2013) The dried copra meal was ground in order to rupture the cell and expose more
surface area necessary for the next processes. In addition to that, it also makes handling
easier in the subsequent processing steps.
Parameters such as mesh size and grinding time were varied. Optimum mesh size was
determined based on the highest oil removed when leached, while optimum grinding time was
chosen based on the percent recovery after grinding.

PROJECT
Alkyd Resin 66

MATERIAL APPARATUS
 Dried Copra Meal  Analytical Balance
 Blender
 Digital Timer
 Sieve Tray
Laboratory Set-up
Figure 3.8. Laboratory Set-up for Grinding of Dried Copra Meal

PROJECT
Alkyd Resin 67
A. Determination of Average Particle Size of Dried Copra Meal
A-1. Objective
To determine the average particle size of copra meal which will be used as a basis for
selecting the optimum mesh size of ground copra meal.
A-2. Hypothesis
The average particle size of the copra meal would be 0.710 mm.
A-3. Procedure
1. Weigh 50 grams of dried copra meal using analytical balance; then place it in the
blender and grind it for 10 minutes.
2. Sieve the ground copra meal using Tyler sieve then weigh the mass retained in each
sieve screen.
3. Calculate the mass fraction in each sieve size and determine the average particle size.
Table 3.9. Determination of Average Particle Size of Dried Copra Meal

Sieve Size Range Average Particle
Mass Retained (g) Mass Fraction (%)
(mm) Size (mm)
+ 2.0 1.1713 2.34
- 2.000 + 1.000 1.500 13.3567 26.64
- 1.000 + 0.710 0.855 15.7083 31.34
- 0.710 + 0.500 0.605 17.8613 35.63
- 0.500 + 0.355 0.428 1.7682 3.53
- 0.355 + 0.250 0.303 0.2261 0.45
pan - 0.0371 0.07
TOTAL 50.1290 100
Note: Negative sign (-) means the sample passed through the sieve, while positive sign (+)
means the sample was retained on the sieve.

PROJECT
Alkyd Resin 68
Figure 3.9. Particle Size Distribution
Computing for the average particle size using the sieve screen sizes,
𝑆𝑖𝑒𝑣𝑒 𝑆𝑖𝑧𝑒 𝐴 + 𝑆𝑖𝑒𝑣𝑒 𝑆𝑖𝑧𝑒 𝐵

̅̅̅̅) =
𝐴𝑣𝑒𝑟𝑎𝑔𝑒 𝑃𝑎𝑟𝑡𝑖𝑐𝑙𝑒 𝑆𝑖𝑧𝑒 (𝑃𝑆
2
0.710 𝑚𝑚 + 0.500 𝑚𝑚
̅̅̅̅) =
𝐴𝑣𝑒𝑟𝑎𝑔𝑒 𝑃𝑎𝑟𝑡𝑖𝑐𝑙𝑒 𝑆𝑖𝑧𝑒 (𝑃𝑆
2
𝐴𝑣𝑒𝑟𝑎𝑔𝑒 𝑃𝑎𝑟𝑡𝑖𝑐𝑙𝑒 𝑆𝑖𝑧𝑒 (𝑃𝑆 ̅̅̅̅) = 0.605 𝑚𝑚
Using the mass retained, we can compute for the mass fraction in each sieve screen by:
𝑀𝑎𝑠𝑠 𝑅𝑒𝑡𝑎𝑖𝑛𝑒𝑑
𝑀𝑎𝑠𝑠 𝐹𝑟𝑎𝑐𝑡𝑖𝑜𝑛 (%) = ∗ 100
𝑇𝑜𝑡𝑎𝑙 𝑀𝑎𝑠𝑠
17.8613
𝑀𝑎𝑠𝑠 𝐹𝑟𝑎𝑐𝑡𝑖𝑜𝑛 (%) = ∗ 100
50.1290
𝑀𝑎𝑠𝑠 𝐹𝑟𝑎𝑐𝑡𝑖𝑜𝑛 (%) = 35.63%
PROJECT
Alkyd Resin 69
A-6. Analysis
The average particle size of the copra meal depends on the size range on which the
highest mass fraction was retained. From the experiment, it was observed that the highest
mass fraction passed through 0.710 mm-sieve but retained on 0.500mm-sieve, which
represents 35.63% of the dried copra meal introduced in the sieve tray. From this size range,
the average particle size of 0.605mm was computed.
A-7. Conclusion
The average particle size of the dried copra meal is 0.605 mm.
B. Determination of Optimum Mesh Size of Dried Copra Meal
B-1. Objective
To determine the optimum mesh size of dried copra meal that would yield high oil
removal when leached.
B-2. Hypothesis
Smaller particle size would result to high oil removal, thus mesh 60 (0.250mm) would
be the optimum mesh size.
B-3. Procedure
1. Weigh 5 sets of 230 grams of dried copra meal using analytical balance; then place it
in the blender and grind the 4 sets for 8 minutes, one set will serve as the control.
2. Sieve each set of ground copra meal using Mesh 24, 32 42, and 60, then weigh the
recovered ground copra meal.
3. Place the ground copra meal in the beaker, then add 460mL of isopropanol. Heat in
a hot plate for 15minutes at 50°C, then weigh the defatted copra meal.
4. Calculate the oil removed by subtracting the defatted copra meal from ground copra
meal.

PROJECT
Alkyd Resin 70

Table 3.10. Determination of Optimum Mesh Size of Dried Copra Meal
1 2 3 4 5
Trial
(control) (Mesh 24) (Mesh 32) (Mesh 42) (Mesh 60)
Mass of Dried
230 230 230 230 230
Copra Meal (g)
Mass of Ground
- 227 227 226 226
Copra Meal (g)
Mass of Defatted
227 222 222 219 217
Copra Meal (g)
Mass of Oil
3 5 5 7 9
Removed
Some of the
dried copra meal
The dried and ground copra meal completely
Observation did not mix with
mixed with the solvent, forming a slurry mixture
the solvent, even
after stirring.
B-5. Analysis
As shown in Table 3.10, the mesh size of the copra meal is indirectly proportional to
the amount of oil removed. Highest amount of oil was removed at mesh 60 (0.250mm),
yielding an oil removal thrice of that of the control (dried copra meal). Furthermore, it was
observed that the control yields low oil removal due to its low surface area for reaction and
inability to completely mix with the solvent. This also justifies that grinding of dried copra meal
is necessary for more effective oil removal.

PROJECT
Alkyd Resin 71
B-6. Conclusion
The optimum size of copra meal is mesh 60 (0.250mm).
B. Determination of Optimum Grinding Time of Dried Copra Meal
B-1. Objective
To determine the optimum grinding time of dried copra meal that would yield the
highest percentage recovery when passed through Tyler Mesh 60 (0.250mm) sieve.
B-2. Hypothesis
Longer grinding time would result to smaller particle size of copra meal, thus majority
of the dried copra meal will pass through Mesh 60 (0.250mm) at 10 minutes of grinding.
B-3. Procedure
1. Weigh 5 sets of 230 grams of dried copra meal using analytical balance; then place it
in the blender and grind each set for 2, 4 6, 8 and 10 minutes.
2. Sieve the ground copra meal using Tyler Mesh 60 (0.250mm) and record the weight
of the ground copra meal that passed through the sieve.
Table 3.11. Determination of Optimum Grinding Time of Dried Copra Meal

Trial 1 2 3 4 5
Mass of Dried Copra
230 230 230 230 230
Meal (g)
Time (min) 2 4 6 8 10
Mass of Copra Meal
that passed through 213 218 222 226 227
0.250mm sieve (g)
Percent Recovery (%) 92.61 94.78 96.52 98.26 98.70

PROJECT
Alkyd Resin 72
𝑀𝑎𝑠𝑠 𝑃𝑎𝑠𝑠𝑒𝑑 𝑇ℎ𝑟𝑜𝑢𝑔ℎ 0.250𝑚𝑚 𝑆𝑖𝑒𝑣𝑒

𝑃𝑒𝑟𝑐𝑒𝑛𝑡 𝑌𝑖𝑒𝑙𝑑 (%) = ∗ 100
𝑀𝑎𝑠𝑠 𝐷𝑟𝑖𝑒𝑑 𝐶𝑜𝑝𝑟𝑎 𝑀𝑒𝑎𝑙
226𝑔
𝑃𝑒𝑟𝑐𝑒𝑛𝑡 𝑌𝑖𝑒𝑙𝑑 (%) = ∗ 100
230𝑔
𝑃𝑒𝑟𝑐𝑒𝑛𝑡 𝑌𝑖𝑒𝑙𝑑 (%) = 98.26%
B-6. Analysis
As shown in Table 3.11, the mass of copra meal that passed through 0.250 mm sieve
increases as the time of grinding also increases. At 8 minutes grinding, 98.26% of copra meal
was recovered, however minimal increment was observed in the succeeding minutes of
grinding.
B-7. Conclusion
The grinding time of copra meal is 8 minutes with 98.26% recovery.
II-3. Leaching of Ground Copra Meal
Leaching is a process of extracting substances from a solid phase through intimate

contact with an immiscible liquid phase called a solvent. (Couper, J.R., et.al., 2012). In this
study, copra meal has 9.3% oil (Department of Agriculture, 2018) which needs to be removed
to isolate the desired carbohydrate. The theoretical mass of oil is:
𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑚𝑎𝑠𝑠 𝑜𝑓 𝑜𝑖𝑙 = (𝑚𝑎𝑠𝑠 𝑜𝑓 𝑐𝑜𝑝𝑟𝑎 𝑚𝑒𝑎𝑙)(𝑝𝑒𝑟𝑐𝑒𝑛𝑡 𝑜𝑖𝑙 𝑐𝑜𝑛𝑡𝑒𝑛𝑡)

𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑚𝑎𝑠𝑠 𝑜𝑓 𝑜𝑖𝑙 = (250𝑔𝑟𝑎𝑚𝑠)(0.093)
𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑚𝑎𝑠𝑠 𝑜𝑓 𝑜𝑖𝑙 = 23.25𝑔𝑟𝑎𝑚𝑠

PROJECT
Alkyd Resin 73
Several parameters such as solvent type, ratio of defatted copra meal to solvent,
operating temperature and time were varied to achieve high oil removal. Furthermore, the
selection of optimum parameter will be based on the percent of oil removed using the formula:
𝑎𝑐𝑡𝑢𝑎𝑙 𝑚𝑎𝑠𝑠 𝑜𝑓 𝑜𝑖𝑙 𝑟𝑒𝑚𝑜𝑣𝑒𝑑 (𝑔)
𝑝𝑒𝑟𝑐𝑒𝑛𝑡 𝑜𝑖𝑙 𝑟𝑒𝑚𝑜𝑣𝑒𝑑 (%) = ∗ 100
𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑚𝑎𝑠𝑠 𝑜𝑓 𝑜𝑖𝑙 (𝑔)
The actual mass is the amount of oil that was removed during the experiment, while
the theoretical mass is the maximum amount of oil that could be removed. The higher the
percent oil removed, the better the reaction.

MATERIAL APPARATUS
 Ground Copra Meal  Beaker
 Isopropanol  Erlenmeyer flask
 Acetone  Hotplate
 Hexane  Thermometer
 Chloroform  Digital timer
 Petroleum ether  Stirrer
 Funnel and filter paper
Laboratory Set-up
Figure 3.10. Laboratory Set-up for Leaching of Ground Copra Meal

Leaching (left) and Filtration (right) of Ground Copra Meal

PROJECT
Alkyd Resin 74
Figure 3.11. Defatted Copra Meal after Leaching
A. Determination of Optimum Type of Solvent for Leaching

A-1. Objective
To determine the optimum type of solvent that would give the highest oil percent
removal in leaching of copra meal.
A-2. Hypothesis
The best solvent is hexane.
A-3. Procedure
1. Weigh 226g ground copra meal and 452mL chloroform, then place them in 1L
beaker covered with foil.
2. Heat the beaker in a hotplate for 50°C for 15min, then filter the mixture using filter
paper and funnel.
3. Weigh and record the mass of defatted copra meal and the spent solvent.
4. Repeat steps 1-3 using different solvents: acetone, petroleum ether, isopropanol,
and hexane.

PROJECT
Alkyd Resin 75
Figure 3.12. Defatted Copra Meal Samples using Different Solvents

Table 3.12. Determination of Optimum Type of Solvent for Leaching
Trial 1 2 3 4 5
Mass of Ground
226 226 226 226 226
Copra Meal (g)
Petroleum
Type of Solvent Chloroform Acetone Isopropanol Hexane
Ether
Volume of
452 452 452 452 452
Solvent (g)
Mass of Solvent
674 355 296 356 296
(g)
Temperature (°C) 50 50 50 50 50
Mass of Defatted
222 218 223 217 220
Copra Meal (g)
Mass of Spent
541 201 124 267 181
Solvent (g)
Mass of Solvent
133 154 172 89 115
Loss (g)
Mass of Oil
4 8 3 8 6
Removed (g)
Percent Oil
17.20 34.41 12.90 34.41 25.81
Removed (%)
High oil Low oil
Low oil removal; removal High oil
removal however with more removal
Average oil
Observation with almost half than half of with
removal
minimal of the the solvent minimal
solvent loss solvent has has solvent loss
evaporated evaporated

PROJECT
Alkyd Resin 76
A-5. Sample Computation
Mass of Oil Removed using isopropanol (g):

𝑚𝑎𝑠𝑠 𝑜𝑓 𝑜𝑖𝑙 𝑟𝑒𝑚𝑜𝑣𝑒𝑑 = 𝑚𝑎𝑠𝑠 𝑜𝑓 𝑔𝑟𝑜𝑢𝑛𝑑 𝐶𝑀 − 𝑚𝑎𝑠𝑠 𝑜𝑓 𝑑𝑒𝑓𝑎𝑡𝑡𝑒𝑑 𝐶𝑀
𝑚𝑎𝑠𝑠 𝑜𝑓 𝑜𝑖𝑙 𝑟𝑒𝑚𝑜𝑣𝑒𝑑 = 226𝑔 − 218𝑔
𝑚𝑎𝑠𝑠 𝑜𝑓 𝑜𝑖𝑙 𝑟𝑒𝑚𝑜𝑣𝑒𝑑 = 8𝑔
Percent Oil Removed (%)

8𝑔
23.25𝑔
𝑝𝑒𝑟𝑐𝑒𝑛𝑡 𝑜𝑖𝑙 𝑟𝑒𝑚𝑜𝑣𝑒𝑑 (%) = 34.41%
A-6. Analysis
From Table 3.12, it shows that highest oil removed was obtained using isopropanol
and acetone among other solvents. However, during the reaction, almost half of the acetone
was not recovered, because its boiling point (56°C) is close to the operating temperature of
50°C, causing the solvent to vaporize. Same trend was also observed in using petroleum
ether since its boiling point is 47°C. On the other hand, isopropanol has high boiling point of
82.6°C, which explains the minimal solvent loss.
A-7. Conclusion
The best solvent type for leaching is isopropanol.
B. Determination of Optimum Ratio of Ground Copra Meal to Solvent

B-1. Objective
To determine the optimum ratio of ground copra meal to isopropanol that would give
the highest oil percent removal.
B-2. Hypothesis
A ratio of 1 part ground copra meal to 5 parts solvent (w/v) is optimal.

PROJECT
Alkyd Resin 77
B-3. Procedure
1. Weigh 226g ground copra meal and 226mL isopropanol, then place them in 2L beaker
covered with foil.
paper and funnel.
3. Weigh and record the mass of defatted copra meal. Then repeat steps 1-2 using
different amount of isopropanol: 452mL, 678mL, 904mL, and 1130mL.

Table 3.13. Determination of Optimum Ratio of Ground Copra Meal to Solvent
Trial 1 2 3 4 5
Mass of Ground
226 226 226 226 226
Copra Meal (g)
Type of Solvent Isopropanol Isopropanol Isopropanol Isopropanol Isopropanol
Ratio of Ground
CM to Solvent 1:1 1:2 1:3 1:4 1:5
(w/v)
Volume of Solvent
226 452 678 904 1130
(mL)
Temperature (°C) 50 50 50 50 50
Time (min) 15 15 15 15 15
Mass of Defatted
221 217 213 212 211
Copra Meal (g)
Mass of Oil
5 9 13 14 15
Removed (g)
Percent Oil
21.51 38.71 55.91 60.22 64.52
Removal (%)
B-5. Sample Computation

Mass of Oil Removed (g):
𝑚𝑎𝑠𝑠 𝑜𝑓 𝑜𝑖𝑙 𝑟𝑒𝑚𝑜𝑣𝑒𝑑 = 13

PROJECT
Alkyd Resin 78

13𝑔
23.25𝑔
B-6. Analysis
From Table 3.13, it shows that the ratio of the ground copra meal to solvent is directly
proportional to the percent of oil removed. At 1:3 (w/v), high amount of oil was removed,
however succeeding ratios of 1:4 and 1:5 led to a minimal increment of oil removal. On the
other hand, it was observed that lower ratios led to a more viscous mixture, making it difficult
to mix.
B-7. Conclusion
The optimum ratio of ground copra meal to isopropanol is 1:3 (w/v)
C. Determination of Optimum Temperature for Leaching
C-1. Objective
To determine the optimum temperature for leaching that would give the highest oil
percent removal.
C-2. Hypothesis
Higher temperature of leaching would result to higher percentage oil removal, thus
70°C would be the optimum temperature.

PROJECT
Alkyd Resin 79
C-3. Procedure
1. Weigh 226g ground copra meal and 678mL isopropanol, then place them in 1L beaker
covered with foil.
paper and funnel.
3. Weigh and record the mass of defatted copra meal. Then repeat steps 1-2 using
different leaching temperatures: 50°C, 60°C, 70°C and 80°C
C-4. Data and Results

Table 3.14. Determination of Optimum Temperature for Leaching
Trial 1 2 3 4 5
Mass of Ground
226 226 226 226 226
Copra Meal (g)
Ratio of Ground
CM to Solvent 1:3 1:3 1:3 1:3 1:3
(w/v)
Volume of Solvent
678 678 678 678 678
(mL)
Temperature (°C) 40 50 60 70 80
Time (min) 15 15 15 15 15
Mass of Defatted
213 213 212 210 209
Copra Meal (g)
Mass of Oil
13 13 14 16 17
Removed (g)
Percent Oil
55.91 55.91 60.22 68.82 73.12
Removed (%)
C-5. Sample Computation


PROJECT
Alkyd Resin 80

16𝑔
23.25𝑔
C-6. Analysis
From Table 3.14, it was observed that increasing the operating temperature led to
more oil removed from the copra meal. Highest oil removal was recorded at 80°C, however
it was observed during the experiment that solvent recovery is low since it is close to the
boiling point of isopropanol. Moreover, the researchers decided to select 70°C since there is
only a minimal increment between the oil removal of 70 and 80°C.
C-7. Conclusion
The optimum temperature for leaching is 70°C.
D. Determination of Optimum Time for Leaching
D-1. Objective
To determine the optimum time for leaching that would give the highest oil percent
removal.
D-2. Hypothesis
Higher time of leaching would result to higher percentage yield, thus 75min would be
the optimum yield.

PROJECT
Alkyd Resin 81
D-3. Procedure
1. Weigh 226g ground copra meal and 678mL isopropanol, then place them in 1L
beaker covered with foil.
paper and funnel.
3. Determine and record the mass of defatted copra meal and spent solvent.
4. Repeat steps 1-3 using different leaching time: 30min, 45min, 60min, and 75min
D-4. Data and Results
Table 3.15. Determination of Optimum Time for Leaching
Trial 1 2 3 4 5
Mass of Ground
226 226 226 226 226
Copra Meal (g)
Ratio of Ground
CM to Solvent 1:3 1:3 1:3 1:3 1:3
(w/v)
Volume of Solvent
678 678 678 678 678
(mL)
Temperature (°C) 70 70 70 70 70
Time (min) 15 30 45 60 75
Mass of Defatted
211 209 208 206 206
Copra Meal (g)
Mass of Oil
15 17 18 20 20
Removed (g)
Percent Oil
64.52 73.12 77.42 86.02 86.02
Removed (%)
D-5. Sample Computation


PROJECT
Alkyd Resin 82

20𝑔
23.25𝑔
D-6. Analysis
As shown in Table 3.15, there was a direct proportionality between the operating time
and the percent of oil removed. At 60 minutes of leaching, oil removed reached 20 grams
(86.02% yield), however further leaching to 75 minutes did not have significant difference.
D-7. Conclusion
The optimum time for leaching is 60 minutes.
E. Determination of Oil Content of Defatted Copra Meal through Soxhlet Apparatus
A Soxhlet Extraction Method is a form of continuous solid-liquid extraction where a

desired compound is extracted from solid material using a solvent. The defatted copra meal
obtained from leaching was analyzed through Soxhlet Apparatus to determine the remaining
oil content in the copra meal. The percent oil content can be determined using the formula:
𝒎𝒂𝒔𝒔 𝒐𝒇 𝒐𝒊𝒍 𝒐𝒃𝒕𝒂𝒊𝒏𝒆𝒅 (𝒈)

𝒑𝒆𝒓𝒄𝒆𝒏𝒕 𝒐𝒊𝒍 𝒄𝒐𝒏𝒆𝒏𝒕 (%) = ∗ 𝟏𝟎𝟎
𝒎𝒂𝒔𝒔 𝒐𝒇 𝒅𝒆𝒇𝒂𝒕𝒕𝒆𝒅 𝒄𝒐𝒑𝒓𝒂 𝒎𝒆𝒂𝒍 (𝒈)
E-1. Materials and Apparatus

MATERIAL APPARATUS
 Defatted Copra Meal  3-neck flask (1L)
 Isopropanol  Hotplate
 Condenser
 Soxhlet Extractor
 Thermometer
 Digital timer
 Pump

PROJECT
Alkyd Resin 83
E-2. Laboratory Set-up
Figure 3.13. Laboratory Set-up for Oil Content of Defatted Copra Meal Determination
E-3. Objective
To determine the oil content of defatted copra meal in order to justify the oil removal
through leaching.
E-4. Hypothesis
The oil content of defatted copra meal would be less than 2%.
E-5. Procedure
1. Weigh 206grams defatted copra meal and 500mL isopropanol, then place them in the
soxhlet extractor and round bottom flask, respectively. Prepare the set-up as shown in
Figure 3.13.
2. Set the hotplate at 90°C to reflux, and turn on the pump to allow the flow of water in
the condenser.

PROJECT
Alkyd Resin 84
3. After 4 hours, determine the mass of recovered oil by vaporizing the solvent in the
round bottom flask.
E-6. Data and Results
Table 3.16. Determination of Oil Content of Defatted Copra Meal through Soxhlet Apparatus
Mass of Defatted Copra Meal (g) 206
Volume of Isopropanol (mL) 500
Mass of Oil Obtained (g) 2
Percent Oil Content (%) 0.97
E-7. Sample Calculation
Percent Oil Content (%)

𝑚𝑎𝑠𝑠 𝑜𝑓 𝑜𝑖𝑙 𝑜𝑏𝑡𝑎𝑖𝑛𝑒𝑑 (𝑔)
𝑝𝑒𝑟𝑐𝑒𝑛𝑡 𝑜𝑖𝑙 𝑐𝑜𝑛𝑒𝑛𝑡 (%) = ∗ 100
𝑚𝑎𝑠𝑠 𝑜𝑓 𝑑𝑒𝑓𝑎𝑡𝑡𝑒𝑑 𝑐𝑜𝑝𝑟𝑎 𝑚𝑒𝑎𝑙 (𝑔)
2𝑔
𝑝𝑒𝑟𝑐𝑒𝑛𝑡 𝑜𝑖𝑙 𝑐𝑜𝑛𝑡𝑒𝑛𝑡 (%) = ∗ 100
206𝑔
𝑝𝑒𝑟𝑐𝑒𝑛𝑡 𝑜𝑖𝑙 𝑐𝑜𝑛𝑡𝑒𝑛𝑡 (%) = 0.97%
E-8. Analysis
In the study, the initial oil content of copra meal of 9.3% was reduced to 0.97% through
leaching using isopropanol at 1:3 (w/v) ratio. This proves that significant amount of residual
oil was removed at 70°C reaction for 60 minutes.
E-9. Conclusion
The final oil content of defatted copra meal is 0.97%.

PROJECT
Alkyd Resin 85
III. MANNITOL PRODUCTION
III-1. Acid Hydrolysis

Dilute acid hydrolysis uses dilute acid such as phosphoric, hydrochloric, and sulfuric
acid to hydrolyze dried and ground copra meal. The hydrolyzed copra meal contents are
separated into solid and liquid fractions, followed by neutralization of the hydrolysate. (Bensah
and Mensah, 2013)
Figure 3.14. Hydrolysis of Mannan to Mannose

In this study, parameters such as acid type, acid concentration, substrate to acid ratio,
and reaction time were considered. The optimum parameters were chosen based from the
percent yield of mannose. To calculate the yield:
𝒎𝒂𝒔𝒔 𝒐𝒇 𝒆𝒙𝒕𝒓𝒂𝒄𝒕𝒆𝒅 𝒎𝒂𝒏𝒏𝒐𝒔𝒆

%𝒚𝒊𝒆𝒍𝒅 =
𝒎𝒂𝒔𝒔 𝒐𝒇 𝒕𝒐𝒕𝒂𝒍 𝒆𝒙𝒕𝒓𝒂𝒄𝒕𝒂𝒃𝒍𝒆 𝒎𝒂𝒏𝒏𝒐𝒔𝒆
The mass of total extractable mannose is first calculated as 51% of the starting mass
of ground copra meal (Saittagaroon, 2006). The formula for total extractable mannose is,
𝒎 𝒕𝒐𝒕𝒂𝒍 𝒆𝒙𝒕𝒓𝒂𝒄𝒕𝒂𝒃𝒍𝒆 𝒎𝒂𝒏𝒏𝒐𝒔𝒆 = 𝟎. 𝟓𝟏(𝒎 𝒈𝒓𝒐𝒖𝒏𝒅 𝑪𝑴 )
The mass of extracted mannose is determined using Benedict’s Test. Benedict’s

Reagent is often used to detect the presence of and amount of reducing sugars in a
solution. (Collins, International GCSE Biology, pp. 42-43) The principle of Benedict's test is
that reducing sugars, such as mannose, reduce the cupric compounds (Cu2+) present in the

PROJECT
Alkyd Resin 86
Benedict's Reagent to cuprous compounds (Cu+) which are precipitated as insoluble

red cupric oxide (Cu2O).
Figure 3.15. Benedict’s Reagent Before and After Reacting with Reducing Sugars
The reaction mechanism shown in Figure 3.15, indicates that a mole of precipitated
cupric oxide (Cu2O) is equivalent to a mole of reducing sugar. This means that the amount of
reducing sugar in the solution can be determined indirectly by stoichiometry
Figure 3.16. Benedict’s Reagent Reaction Mechanism
In order to determine the amount of reducing sugars after each hydrolysis trials, 1mL
of sample hydrolysate (supernatant) was collected and reacted with 5mL of Benedict’s
Reagent. After reaction, the precipitated cupric oxide is filtered, washed, dried, and weighed.
The amount of mannose in the sample is then calculated as
𝒎𝒂𝒔𝒔 𝒐𝒇 𝑪𝒖𝟐 𝑶 𝟏 𝒎𝒐𝒍 𝑪𝒖𝟐 𝑶 𝟏 𝒎𝒐𝒍 𝒎𝒂𝒏𝒏𝒐𝒔𝒆 𝟏𝟖𝟎. 𝟏𝟓𝟔𝒈 𝒎𝒂𝒏𝒏𝒐𝒔𝒆

𝒎 𝒆𝒙𝒕𝒓𝒂𝒄𝒕𝒆𝒅 𝒎𝒂𝒏𝒏𝒐𝒔𝒆/𝒎𝑳 = × × ×
𝒎𝑳 𝒉𝒚𝒅𝒓𝒐𝒍𝒚𝒔𝒂𝒕𝒆 𝟏𝟒𝟑. 𝟎𝟗𝟏𝒈 𝑪𝒖𝟐 𝑶 𝟏 𝒎𝒐𝒍 𝑪𝒖𝟐 𝑶 𝟏 𝒎𝒐𝒍 𝒎𝒂𝒏𝒏𝒐𝒔𝒆
The total amount of extracted mannose is calculated as,
𝒎 𝒆𝒙𝒕𝒓𝒂𝒄𝒕𝒆𝒅 𝒎𝒂𝒏𝒏𝒐𝒔𝒆 = 𝑽𝒔𝒖𝒑𝒆𝒓𝒏𝒂𝒕𝒂𝒏𝒕 × 𝒎 𝒆𝒙𝒕𝒓𝒂𝒄𝒕𝒆𝒅 𝒎𝒂𝒏𝒏𝒐𝒔𝒆/𝒎𝑳

PROJECT
Alkyd Resin 87

MATERIAL APPARATUS
 Defatted Copra Meal  3-neckround bottom flask (1L)
 Hydrochloric Acid  Hotplate
 Phosphoric Acid  Condenser
 Sulfuric Acid  Thermometer
 Benedict’s reagent  Digital timer
 Pump
Laboratory Set-up
Figure 3.17. Laboratory Set-up for Acid Hydrolysis of Defatted Copra Meal
Figure 3.18. Production of Mannose

PROJECT
Alkyd Resin 88
A. Determination of Optimum Type of Acid for Hydrolysis

A-1. Objective
To determine the optimum type of acid in hydrolyzing mannan in copra meal that would
give highest percent yield of mannose.
A-2. Hypothesis
The optimum acid type to use is hydrochloric acid.
A-3. Procedure
1. Weigh 3 sets of 206g defatted copra meal and prepare 824mL of 1.80% w/w
hydrochloric acid, then place it in the 3-neck round bottom flask.
2. Put the 3-neck round bottom flask to the hotplate and set to 100°C for 30 minutes.
3. Afterwards, filter the mixture using funnel and filter paper, then measure the
hydrolysate solution (liquid) obtained.
4. Determine the concentration of mannose in the hydrolysate solution using Benedict ’s
reagent.
5. Repeat the steps 1-4 using different acid type such as sulfuric and phosphoric acid.

Table 3.17 Determination of Optimum Type of Acid for Hydrolysis
TRIAL 1 2 3
Type of Acid Hydrochloric Sulfuric Phosphoric
Mass of Defatted CM (g) 206 206 206
Concentration of Acid
1.80 1.80 1.80
(% w/w)
Ratio of Defatted
1:4 1:4 1:4
CM to Acid
Temperature (°C) 100°C 100°C 100°C
Time (min) 30 30 30
Volume of Hydrolysate (mL) 789 796 785
Mass of Red Cu2O Precipitate per
0.0746 0.0716 0.0801
mL of hydrolysate (g)
Mass of Mannose (g) 74.11 71.76 79.17
% Yield 70.54% 68.30% 75.36%

PROJECT
Alkyd Resin 89
For trial 3 in Table 3.16,
The total extractable mannose is calculated as,
𝑚 𝑡𝑜𝑡𝑎𝑙 𝑒𝑥𝑡𝑟𝑎𝑐𝑡𝑎𝑏𝑙𝑒 𝑚𝑎𝑛𝑛𝑜𝑠𝑒 = 0.51(206𝑔)

𝒎 𝒕𝒐𝒕𝒂𝒍 𝒆𝒙𝒕𝒓𝒂𝒄𝒕𝒂𝒃𝒍𝒆 𝒎𝒂𝒏𝒏𝒐𝒔𝒆 = 𝟏𝟎𝟓. 𝟎𝟔𝒈
0.0801𝑔 𝐶𝑢2 𝑂 1 𝑚𝑜𝑙 𝐶𝑢2 𝑂 1 𝑚𝑜𝑙 𝑚𝑎𝑛𝑛𝑜𝑠𝑒 180.156𝑔 𝑚𝑎𝑛𝑛𝑜𝑠𝑒
𝑚 𝑒𝑥𝑡𝑟𝑎𝑐𝑡𝑒𝑑 𝑚𝑎𝑛𝑛𝑜𝑠𝑒 = × × ×
𝑚𝐿 ℎ𝑦𝑑𝑟𝑜𝑙𝑦𝑠𝑎𝑡𝑒 143.091𝑔 𝐶𝑢2 𝑂 1 𝑚𝑜𝑙 𝐶𝑢2 𝑂 1 𝑚𝑜𝑙 𝑚𝑎𝑛𝑛𝑜𝑠𝑒
𝑔 𝑚𝑎𝑛𝑛𝑜𝑠𝑒
𝑚 𝑒𝑥𝑡𝑟𝑎𝑐𝑡𝑒𝑑 𝑚𝑎𝑛𝑛𝑜𝑠𝑒 = 0.10084838
𝑚𝐿 ℎ𝑦𝑑𝑟𝑜𝑙𝑦𝑠𝑎𝑡𝑒
𝑚 𝑒𝑥𝑡𝑟𝑎𝑐𝑡𝑒𝑑 𝑚𝑎𝑛𝑛𝑜𝑠𝑒 = 785𝑚𝐿 ℎ𝑦𝑑𝑟𝑜𝑙𝑦𝑠𝑎𝑡𝑒 × 0.10084838
𝒎 𝒆𝒙𝒕𝒓𝒂𝒄𝒕𝒆𝒅 𝒎𝒂𝒏𝒏𝒐𝒔𝒆 = 𝟕𝟗. 𝟏𝟕𝒈 𝒎𝒂𝒏𝒏𝒐𝒔𝒆
The percent yield is calculated as,
79.17𝑔
%𝑦𝑖𝑒𝑙𝑑 =
105.06𝑔
%𝒚𝒊𝒆𝒍𝒅 = 𝟕𝟓. 𝟑𝟔%
A-6. Analysis
The highest percent yield of mannose is obtained using phosphoric acid at 75.36%
compared to the 68.30 and 70.54% of sulfuric and hydrochloric acid respectively. This is
attributed to phosphoric acid being a triprotic acid or an acid with 3 protonating hydrogens,
which attacks beta glycosidic bonds holding the mannose together in a more aggressive
manner.
A-7. Conclusion
The optimum acid type to use in hydrolysis, which extracted the highest amount of
mannose (79.17g) with a percent yield of 75.36%, is phosphoric acid.

PROJECT
Alkyd Resin 90
B. Determination of Optimum Acid Concentration for Hydrolysis

B-1. Objective
To determine the optimum acid concentration in hydrolyzing copra meal that would
give highest percent yield of mannose.
B-2. Hypothesis
The optimum acid concentration is between 2.0-3.0 (%w/w)
B-3. Procedure
phosphoric acid, then place it in the 3-neck round bottom flask.
4. Determine the concentration of mannose in the hydrolysate using Benedict ’s reagent.
5. Repeat the steps 1-4 using different concentration such as 1.0, 1.8, 2.6, 3.4% w/w
phosphoric acid.
Table 3.18. Determination of Optimum Acid Concentration for Hydrolysis
TRIAL 1 2 3 4 5
Type of Acid Phosphoric Phosphoric Phosphoric Phosphoric Phosphoric
Mass of Defatted CM (g) 206 206 206 206 206
0.20 1.00 1.80 2.60 3.40
(% w/w)
Ratio of Defatted CM to
1:4 1:4 1:4 1:4 1:4
Acid
Temperature (°C) 100°C 100°C 100°C 100°C 100°C
Time (min) 30 30 30 30 30
Volume of Hydrolysate
789 790 779 784 788
(mL)
Mass of Red Cu2O
Precipitate per mL of 0.0476 0.0626 0.0789 0.0892 0.0908
hydrolysate (g)
Mass of Mannose (g) 47.28 62.26 77.38 88.05 90.08
% Yield 45.00 59.26 73.65 83.81 85.74

PROJECT
Alkyd Resin 91


𝒎 𝒆𝒙𝒕𝒓𝒂𝒄𝒕𝒆𝒅 𝒎𝒂𝒏𝒏𝒐𝒔𝒆 = 𝟖𝟖. 𝟎𝟒𝟕𝟓𝒈 𝒎𝒂𝒏𝒏𝒐𝒔𝒆
88.0475𝑔
105.06𝑔
%𝒚𝒊𝒆𝒍𝒅 = 𝟖𝟑. 𝟖𝟏%
B-6. Analysis
The highest percent yield (83.81%) of mannose is obtained using 2.60% w/v
phosphoric acid. The succeeding variation of 3.40% w/v phosphoric acid has a higher percent
yield (85.74%), however, the difference of mannose extracted is not significantly greater.
Thus, the optimal acid concentration was determined to be 2.60% w/v phosphoric.
B-7. Conclusion
The optimum phosphoric acid concentration to use in hydrolysis, which extracted

88.05g of mannose with a percent yield of 83.81%, is 2.60% w/v phosphoric acid.

PROJECT
Alkyd Resin 92
C. Determination of Optimum Ratio of Copra Meal to Acid for Hydrolysis

C-1. Objective
To determine the optimum mass to volume ratio of copra meal to acid in hydrolysis
that would give highest percent yield of mannose.
C-2. Hypothesis
Higher ratio would result to higher yield, thus the optimal ratio is 1:10.
C-3. Procedure
phosphoric acid (1:4 ratio), then place it in the 3-neck round bottom flask.
5. Repeat the steps 1-4 using different ratio such as 1:6, 1:8, 1:10, 1:12 (%m/w).
Table 3.19. Determination of Optimum Ratio of Copra Meal to Acid for Hydrolysis
TRIAL 1 2 3 4 5
2.60 2.60 2.60 2.60 2.60
(% w/w)
1:4 1:6 1:8 1:10 1:12
Acid
Time (min) 30 30 30 30 30
785 1185 1550 1953 2398
(mL)
Mass of Red Cu2O
hydrolysate (g)
Mass of Mannose (g) 87.47 89.82 92.11 94.45 92.99
% Yield 83.26 81.69 87.67 89.90 85.51

PROJECT
Alkyd Resin 93
C-5. Sample Calculation

For trial 3 in Table 3.18

𝒎 𝒆𝒙𝒕𝒓𝒂𝒄𝒕𝒆𝒅 𝒎𝒂𝒏𝒏𝒐𝒔𝒆 = 𝟗𝟐. 𝟏𝟏𝟎𝟑𝒈 𝒎𝒂𝒏𝒏𝒐𝒔𝒆
92.1103𝑔
105.06𝑔
%𝒚𝒊𝒆𝒍𝒅 = 𝟖𝟕. 𝟔𝟕%
C-6. Analysis
Starting from the third trial with a mass to volume ratio of 1:8, there was no significant
increase in concentration of mannose, with increasing mass to volume ratios as shown in the
data. The third trial extracted 92.11g of mannose which represents a percent yield of 87.67%
Thus, the optimal mass to volume ratio of copra meal to acid was determined to be 1:8.
C-7. Conclusion
The optimum mass to volume ratio of copra meal to acid to use in hydrolysis, which
extracted 92.11g of mannose with a percent yield of 87.67%, is 1:8.

PROJECT
Alkyd Resin 94
D. Determination of Optimum Temperature of Acid Hydrolysis

D-1. Objective
To determine the optimum temperature in hydrolysis that would give highest percent
yield of mannose.
D-2. Hypothesis
The optimum temperature for hydrolysis is 100°C
D-3. Procedure
5. Repeat the steps 1-4 using different temperature such as 90, 100, 110, 120°C
Table 3.20. Determination of Optimum Temperature for Acid Hydrolysis
TRIAL 1 2 3 4 5
2.60 2.60 2.60 2.60 2.60
(% w/w)
1:8 1:8 1:8 1:8 1:8
Acid
Time (min) 30 30 30 30 30
1555 1562 1570 - -
(mL)
Mass of Red Cu2O
Precipitate per mL of 0.0364 0.0405 0.0470 - -
hydrolysate (g)
Mass of Mannose (g) 71.26 79.64 92.90 - -
% Yield 67.83 75.79 88.43 - -

PROJECT
Alkyd Resin 95
D-5. Sample Calculation


𝒎 𝒆𝒙𝒕𝒓𝒂𝒄𝒕𝒆𝒅 𝒎𝒂𝒏𝒏𝒐𝒔𝒆 = 𝟗𝟐. 𝟗𝟎𝟑𝟐𝒈 𝒎𝒂𝒏𝒏𝒐𝒔𝒆
92.9032𝑔
105.06𝑔
%𝒚𝒊𝒆𝒍𝒅 = 𝟖𝟖. 𝟒𝟑%
D-6. Analysis
No data were collected at trials 4 and 5 with temperatures 110 and 120°C respectively
as the temperature of the solution did not rise more than 102°C despite setting the hot plate
at higher temperatures. Thus, the optimal temperature to use is 100°C which extracted
92.90g of mannose, representing a percent yield of 88.43%
D-7. Conclusion
The optimum temperature for acid hydrolysis is 100°C, which extracted 92.90g of
mannose with a percent yield of 88.43%.

PROJECT
Alkyd Resin 96
E. Determination of Optimum Time for Acid Hydrolysis

E-1. Objective
To determine the optimum time in hydrolysis that would give highest percentage yield
to mannose.
E-2. Hypothesis
The optimum time for hydrolysis to use is 60 minutes.
E-3. Procedure
5. Repeat the steps 1-4 using different time such as 60, 90, 120, 150 minutes.
E-4. Data and Results
Table 3.21 Determination of Optimum Time for Acid Hydrolysis
TRIAL 1 2 3 4 5
2.60 2.60 2.60 2.60 2.60
(% w/w)
1:8 1:8 1:8 1:8 1:8
Acid
Time (min) 30 60 90 120 150
1558 1552 1560 1548 1561
(mL)
Mass of Red Cu2O
hydrolysate (g)
Mass of Mannose (g) 93.17 96.14 100.56 92.19 82.15
% Yield 88.68 91.51 95.72 87.50 78.19

PROJECT
Alkyd Resin 97
E-5. Sample Calculation


𝒎 𝒆𝒙𝒕𝒓𝒂𝒄𝒕𝒆𝒅 𝒎𝒂𝒏𝒏𝒐𝒔𝒆 = 𝟏𝟎𝟎. 𝟓𝟔𝟎𝟕𝒈 𝒎𝒂𝒏𝒏𝒐𝒔𝒆
100.5607𝑔
105.06𝑔
%𝒚𝒊𝒆𝒍𝒅 = 𝟗𝟓. 𝟕𝟐%
E-6. Analysis
Trials 4 and 5 exhibited a decrease in concentration of recovered mannose. This is

attributed to breaking down of mannose at longer hydrolysis reaction times Thus, the optimal
hydrolysis time to use is 90 minutes which extracted the highest amount of mannose at
100.56g, representing a percent yield of 95.72%
E-7. Conclusion
The optimum reaction time for acid hydrolysis is 90 min which extracted 100.56g of
mannose representing a 95.72% yield

PROJECT
Alkyd Resin 98
III-2. Neutralization
Neutralization is a chemical reaction in which an acid and a base react quantitatively

with each other to form a salt. The pH of the neutralized solution depends on the acid strength
of the reactants. For pH control, chemicals such as sodium carbonate, calcium hydroxide and
potassium hydroxide are used. In this study, neutralization is used to remove the excess
phosphoric acid after acid hydrolysis

MATERIAL APPARATUS
 Hydrolysate  pH meter
 Sodium Carbonate  Beaker
 Calcium Hydroxide  Hotplate with magnetic stirrer
 Potassium Hydroxide  Analytical Balance
Laboratory Set-up
Figure 3.19 Neutralization of Hydrolysate
A. Determination of Optimum Type of Neutralizing Agent

A-1. Objective
To determine the optimum type of neutralizing agent that would precipitate out the
protein and would yield a pH of 4.6-4.8.

PROJECT
Alkyd Resin 99
A-2. Hypothesis
The optimum type of neutralizing agent is calcium hydroxide.
A-3. Procedure
1. Weigh 5 grams of sodium carbonate and prepare 100g of hydrolysate, then place them
in a beaker.
2. Put the beaker in a hotplate under stirring at room temperature for 10 minutes then
record the pH.
3. Repeat the procedure by using calcium hydroxide and potassium hydroxide as the
neutralizing agent.
Table 3.22. Determination of Optimum Type of Neutralizing Agent
Trial 1 2 3
Type of Neutralizing Agent Sodium Carbonate Calcium Hydroxide Potassium Hydroxide
Mass of Hydrolysate (g) 100 100 100
pH before treatment 1.6 1.6 1.6
pH after treatment 6.5 3.3 8.9
The precipitate
No precipitate No precipitate
calcium phosphate
Observation formed during the formed during the
is insoluble to the
reaction reaction
solution
Figure 3.20. Neutralization using Different Bases
A-5. Analysis
Based on Table 3.21, addition of sodium carbonate, calcium hydroxide and potassium
hydroxide increased the pH of the hydrolysate from 0.6 to 6.5, 3.4 and 8.9 respectively.

PROJECT
Alkyd Resin 100
However, the salt formed during the neutralization with sodium carbonate and potassium
hydroxide as the neutralizing agent, is soluble to the solution. On the other hand, the salt
formed in the second trial was found to be insoluble to the solution and can be separated
through filtration process Thus, the selected neutralizing agent in this process is calcium
hydroxide
A-6. Conclusion
The optimum type of neutralizing agent for the neutralization of the hydrolysate is
calcium hydroxide.
B. Determination of the Amount of Neutralizing Agent
B-1 Objective
To determine the amount of neutralizing agent that would give a pH ranging from 4.6
to 4.8.
B-2. Hypothesis
The amount of calcium carbonate that will raise the pH to 4.7 will be greater than 5
grams.
B-3. Procedure
1. Weigh 5 grams and prepare another five to ten sets of 1 gram of calcium hydroxide.
2. Add each set of calcium hydroxide to the hydrolysate and record the corresponding
change in pH.
3. Stop the addition of calcium hydroxide when it reached the desired pH
4. Filter the mixture and record the mass of the neutralized and filtered hydrolysate
(mannose).
5. Calculate the percent yield.

PROJECT
Alkyd Resin 101

Table 3.23. Determination of the Amount of Neutralizing Agent
Amount of Calcium Hydroxide pH
5g 3.3
6g 3.8
7g 4.1
8g 4.2
9g 4.4
10 g 4.7
Mass of Neutralized Hydrolysate (g) 96
Mass of Cake (g) 13
Mass of Mannose in Neutralized
5.68
Hydrolysate (g)
% Yield 93.16
The neutralization reaction is described by the following equations
BASE + ACID  SALT + WATER

3Ca(OH)2 + 2H3PO4  Ca3(PO4)2 + 6H2O
Calcium Hydroxide Phosphoric Acid Calcium Phosphate Water
𝑇ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑀𝑎𝑠𝑠 𝑜𝑓 𝐶𝑎(𝑃𝑂4 )2

1 𝑚𝑜𝑙 𝐶𝑎(𝑂𝐻)2 1 𝑚𝑜𝑙 𝐶𝑎3 (𝑃𝑂4 )2 310.2 𝑔 𝐶𝑎3 (𝑃𝑂4 )2
= 10𝑔 𝐶𝑎(𝑂𝐻)2 𝑥 𝑥 𝑥
74.10 𝑔 𝐶𝑎(𝑂𝐻)2 3 𝑚𝑜𝑙 𝐶𝑎(𝑂𝐻)2 1 𝑚𝑜𝑙 𝐶𝑎3 (𝑃𝑂4 )2
𝑇ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑀𝑎𝑠𝑠 𝑜𝑓 𝐶𝑎(𝑃𝑂4 )2 = 13.9541 𝑔 𝐶𝑎3 (𝑃𝑂4 )2
𝐴𝑐𝑡𝑢𝑎𝑙 𝑌𝑖𝑒𝑙𝑑 13 𝑔
% 𝑌𝑖𝑒𝑙𝑑 = 𝑥 100 = 𝑥 100
𝑇ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑌𝑖𝑒𝑙𝑑 13.9541 𝑔
% 𝑌𝑖𝑒𝑙𝑑 = 93.16%
B-6. Analysis
Based on the table, the neutralized hydrolysate reached the desired pH of 4.7 after
the addition of 10 g calcium hydroxide. Additionally, the recorded mass of cake or the
precipitate calcium phosphate during the neutralization process was found to be almost equal
to the theoretical yield of 13.9541 g, resulting to a 93.16% yield.

PROJECT
Alkyd Resin 102
Additionally, the amount of mannose present in the neutralized hydrolysate was again
determined using Benedict’s Quantitative Test. The amount of mannose in 96g (99.84mL) of
neutralized hydrolysate is found to be 5.68g.
Lastly, only a representative sample was neutralized out of the total amount of 170.6g
(1560mL) of hydrolysate. Thus, the actual amount of Ca(OH)2 to be used is calculated as
170.6g. Similarly, the actual amount of mannose in is calculated to be 100.94g in 1638g of
solution
B-7. Conclusion
The amount of neutralizing agent, calcium hydroxide, required during the neutralization
process is 170.6g.
III-3. Reduction
Reduction of the aldehyde group of mannose yields its sugar alcohol counterpart,
mannitol (Rastogi, S.C., 2003). The reduction mechanism of mannose to mannitol is shown
in Figure 2.6.
Figure 3.21 Reduction of Mannose to Mannitol
In a study by Hricoviniova (2011), The reduction of mannose with sodium borohydride

yielded mannitol in very good yield (78 %). Sodium borohydride is a good reducing agent and
is very effective for the reduction of aldehydes and alcohols. Presented in Figure 2.7 is the
reaction mechanism of reducing mannose to mannitol using sodium borohydride.

PROJECT
Alkyd Resin 103
Figure 3.22 Reduction of Mechanism Using Sodium Borohydride

In this study, parameters such as sodium borohydride concentration, reaction
temperature, and reaction time were considered. The optimum parameters were chosen
based from the percent yield of mannitol. To calculate the yield:
𝒎 𝒆𝒙𝒑𝒆𝒓𝒊𝒎𝒆𝒏𝒕𝒂𝒍 𝒎𝒂𝒏𝒏𝒊𝒕𝒐𝒍
%𝒚𝒊𝒆𝒍𝒅 = × 𝟏𝟎𝟎%
𝒎 𝒕𝒉𝒆𝒐𝒓𝒆𝒕𝒊𝒄𝒂𝒍 𝒎𝒂𝒏𝒏𝒊𝒕𝒐𝒍
Where mexperimental mannitol is the amount of mannitol obtained from experimentation

trials and mtheoretical mannitol is the stoichiometric amount of mannitol that can be obtained based
on the amount of mannose introduced. The formula for the theoretical mass of mannitol is,
𝟏 𝒎𝒐𝒍 𝒎𝒂𝒏𝒏𝒐𝒔𝒆 𝟏 𝒎𝒐𝒍 𝒎𝒂𝒏𝒏𝒊𝒕𝒐𝒍 𝟏𝟖𝟐. 𝟏𝟕𝟐𝒈 𝒎𝒂𝒏𝒏𝒊𝒕𝒐𝒍

𝒎 𝒕𝒉𝒆𝒐𝒓𝒆𝒕𝒊𝒄𝒂𝒍 𝒎𝒂𝒏𝒏𝒊𝒕𝒐𝒍 = 𝒎 𝒎𝒂𝒏𝒏𝒐𝒔𝒆 × × ×
𝟏𝟖𝟎. 𝟏𝟓𝟔𝒈 𝒎𝒂𝒏𝒏𝒐𝒔𝒆 𝟏 𝒎𝒐𝒍 𝒎𝒂𝒏𝒏𝒐𝒔𝒆 𝟏 𝒎𝒐𝒍 𝒎𝒂𝒏𝒏𝒊𝒕𝒐𝒍
The experimental mass of mannitol is determined by crystallizing the formed mannitol.

In crystallization, the amount of water in the solution is reduced, effectively reducing the
solubility of mannitol, thus, it crashes out as solid crystals.

PROJECT
Alkyd Resin 104
Figure 3.23. Determination of the Amount of Mannitol

MATERIAL APPARATUS
 Mannose Solution  1L Beaker
 Sodium Borohydride  Magnetic Stirrer
 Distilled Water  Thermometer
 Crystallizing Pan
 Hotplate
Laboratory Set-up
Figure 3.24. Laboratory Set-up for Reduction

PROJECT
Alkyd Resin 105
Figure 3.25. Production of Mannitol
A. Determination of the Optimal Molar Ratio of Mannose to Sodium Borohydride

A-1. Objective
To determine the optimum mole ratio of mannose to sodium borohydride that would
yield high amount of mannitol.
A-2. Hypothesis
The optimum molar ratio of mannose to sodium borohydride is 1:1
A-3. Procedure
1. Weigh 5 sets of 1638g of mannose solution in a beaker.
2. For a molar ratio of 1:0.50, add 10.57g of sodium borohydride to the mannose solution
and react the mixture for 30 mins at room temperature (25°C).
3. Crystallize and weigh the mannitol obtained.
4. Replicate the procedure for molar ratios 1:0.75, 1:1, 1:1.25. 1:1.50

PROJECT
Alkyd Resin 106
Table 3.24 Determination of Optimum Molar Ratio of Mannose to Sodium Borohydride

TRIAL 1 2 3 4 5
Mass of
100.94 100.94 100.94 100.94 100.94
Mannose (g)
Molar Ratio (mol
mannose: mol 1:0.50 1:0.75 1:1 1:1.25 1:1.50
NaBH4)
Mass of NaBH4
10.60 15.90 21.20 26.50 31.80
(g)
Temperature
25 25 25 25 25
(°C)
Time (min) 30 30 30 30 30
Mass of
11 24 37 54 57
Mannitol (g)
% Yield (%) 10.78 23.51 36.25 52.91 55.84
Figure 3.26. Production of Mannitol under different molar ratios
The amount of sodium borohydride to be added for a molar ratio of 1:1.25 is calculated as,
𝒎𝒐𝒍 𝒎𝒂𝒏𝒏𝒐𝒔𝒆 𝟏. 𝟐𝟓 𝒎𝒐𝒍 𝑵𝒂𝑩𝑯𝟒 𝟑𝟕. 𝟖𝟒𝟏𝒈 𝑵𝒂𝑩𝑯𝟒

𝒎𝑵𝒂𝑩𝑯𝟒 = 𝒎𝒎𝒂𝒏𝒏𝒐𝒔𝒆 × × ×
𝟏𝟖𝟎. 𝟏𝟓𝟔𝒈 𝒎𝒂𝒏𝒏𝒐𝒔𝒆 𝟏 𝒎𝒐𝒍 𝒎𝒂𝒏𝒏𝒐𝒔𝒆 𝒎𝒐𝒍 𝑵𝒂𝑩𝑯𝟒

PROJECT
Alkyd Resin 107
𝑚𝑜𝑙 𝑚𝑎𝑛𝑛𝑜𝑠𝑒 1.25 𝑚𝑜𝑙 𝑁𝑎𝐵𝐻4 37.841𝑔 𝑁𝑎𝐵𝐻4

𝑚𝑁𝑎𝐵𝐻4 = 100.94 × × ×
180.156𝑔 𝑚𝑎𝑛𝑛𝑜𝑠𝑒 1 𝑚𝑜𝑙 𝑚𝑎𝑛𝑛𝑜𝑠𝑒 𝑚𝑜𝑙 𝑁𝑎𝐵𝐻4
𝒎𝑵𝒂𝑩𝑯𝟒 = 𝟐𝟔. 𝟓𝟎𝒈 𝑵𝒂𝑩𝑯𝟒
The theoretical mass of mannitol is calculated as,

1 𝑚𝑜𝑙 𝑚𝑎𝑛𝑛𝑜𝑠𝑒 1 𝑚𝑜𝑙 𝑚𝑎𝑛𝑛𝑖𝑡𝑜𝑙 182.172𝑔 𝑚𝑎𝑛𝑛𝑖𝑡𝑜𝑙

𝑚 𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑚𝑎𝑛𝑛𝑖𝑡𝑜𝑙 = 100.94𝑔 × × ×
180.156𝑔 𝑚𝑎𝑛𝑛𝑜𝑠𝑒 1 𝑚𝑜𝑙 𝑚𝑎𝑛𝑛𝑜𝑠𝑒 1 𝑚𝑜𝑙 𝑚𝑎𝑛𝑛𝑖𝑡𝑜𝑙
𝒎 𝒕𝒉𝒆𝒐𝒓𝒆𝒕𝒊𝒄𝒂𝒍 𝒎𝒂𝒏𝒏𝒊𝒕𝒐𝒍 = 𝟏𝟎𝟐. 𝟎𝟔𝟗𝟓𝒈
54𝑔
%𝑦𝑖𝑒𝑙𝑑 = × 100%
102.0695𝑔
%𝒚𝒊𝒆𝒍𝒅 = 𝟓𝟐. 𝟗𝟏%

A-6. Analysis
The highest percent yield of mannitol is obtained using a molar ratio of 1:1.50 of
mannose to sodium borohydride at 55.84%. At this trial, however, severe bubbling and
foaming occurred due to the rapid evolution of hydrogen gas attributed to the high
concentration of sodium borohydride. The previous trial (4) produced mannitol with a
comparable yield at 52.91%. In addition, the reaction and evolution of hydrogen gas, on this
trial, was observed to be slower and much more contained.
A-7. Conclusion
The optimal molar ratio of mannose to sodium borohydride is 1:1.25 with a percent
yield of 52.91%.

PROJECT
Alkyd Resin 108
B. Determination of Optimal Reduction Temperature

B-1. Objective
To determine the optimum reduction temperature that would yield high amount of
mannitol.
B-2. Hypothesis
The optimum temperature is 30°C
B-3. Procedure
2. Add 26.50g of sodium borohydride to the mannose solution and react the mixture for
30 mins at room temperature (25°C).
4. Replicate the procedure for temperatures 30, 40, 50, 60°C
Table 3.25 Determination of Optimum Molar Ratio of Mannose to Sodium Borohydride
TRIAL 1 2 3 4 5
Mass of
100.94 100.94 100.94 100.94 100.94
Mannose (g)
Molar Ratio (mol
mannose: mol 1:1.25 1:1.25 1:1.25 1:1.25 1:1.25
NaBH4)
Mass of NaBH4
26.50 26.50 26.50 26.50 26.50
(g)
Temperature
25 30 40 50 60
(°C)
Time (min) 30 30 30 30 30
Mass of
60 58 58 56 54
Mannitol (g)
% Yield (%) 58.78 56.82 56.82 54.86 52.91

PROJECT
Alkyd Resin 109


60𝑔
%𝑦𝑖𝑒𝑙𝑑 = × 100%
102.0695𝑔
%𝒚𝒊𝒆𝒍𝒅 = 𝟓𝟖. 𝟕𝟖%

B-6. Analysis
The highest percent yield of mannitol is obtained using a reaction temperature of 25°C
(trial 1) or room temperature at 58.78%. This is the only trial that required no heating as the
room temperature at the laboratory was nearly 25°C. It was observed that there was slight
decline in the amount of recovered mannitol as the reaction temperature was increased. This
is attributed to the instability of sodium borohydride in water at room temperature alone, much
more at elevated temperatures. (Martelli et al, 2010)
B-7. Conclusion
The optimal reaction temperature in the reduction of mannose to mannitol is 25°C

with a percent yield of 58.78%.

PROJECT
Alkyd Resin 110
C. Determination of Optimal Reduction Time

C-1. Objective
To determine the optimum reduction time that would yield high amount of mannitol.
C-2. Hypothesis
The optimum reduction time is 120 minutes
C-3. Procedure
2. Add 26.50g of sodium borohydride to the mannose solution and react the mixture for
30 mins at room temperature (25°C).
4. Replicate the procedure for times 60, 90, 120, and 150 minutes
Table 3.26 Determination of Optimum Reduction Time

TRIAL 1 2 3 4 5
Mass of Mannose
100.94 100.94 100.94 100.94 100.94
(g)
Molar Ratio (mol
mannose: mol 1:1.25 1:1.25 1:1.25 1:1.25 1:1.25
NaBH4)
Mass of NaBH4 (g) 26.50 26.50 26.50 26.50 26.50
Temperature (°C) 25 25 25 25 25
Time (min) 30 60 90 120 150
Mass of Mannitol
56 66 89 91 91
(g)
% Yield (%) 54.86 64.66 87.20 89.15 89.15

PROJECT
Alkyd Resin 111
Figure 3.27. Amount of Mannitol Crystallized under Different Operating Time


89𝑔
%𝑦𝑖𝑒𝑙𝑑 = × 100%
100.0695𝑔
%𝒚𝒊𝒆𝒍𝒅 = 𝟖𝟕. 𝟐𝟎%

PROJECT
Alkyd Resin 112
C-6. Analysis
The highest percent yield of mannitol is obtained using reaction times 120 and 150
minutes, both at 89.15%. Looking at the preceding trial (3), however, a comparable yield was
also attained at 87.20%. It was observed that the reaction did not proceed beyond 90
minutes. Thus, the third trial was selected as the optimum.
Additionally, the volume of the optimal trial was found to be 1542mL (1645g)
C-7. Conclusion
The optimal reaction time in the reduction of mannose to mannitol is 90 minutes with
a percent yield of 87.20%.
III-4. Evaporation
Evaporation is a unit operation used in chemical processing industries to increase the

concentration of a solute in a solution by evaporating the solvent, usually water. In this study,
mannitol was concentrated by evaporation in order to prepare it for the subsequent process.
Parameters such as evaporation time, rate of evaporation, initial and final

concentrations, were considered and determined. The initial concentration of the feed is
already known from the previous process. The final concentration is set near the saturation
point of mannitol in which is also the same as its solubility in water. According to Wang et al
(2008), the solubility of mannitol in water is 216 mg/mL at 25° C. The final concentration
was set to 200mg/mL, to ensure that the mannitol remains in solution and no crystallization
occurs.
The final concentration of mannitol was indirectly determined by monitoring the

amount of evaporated water. Since the amount of mannitol in the solution is constant,
evaporating the water portion will decrease the overall volume of the solution, thus, increasing
the concentration of mannitol. In order to determine the amount of water to be removed,
material balance is used and is represented by,

PROJECT
Alkyd Resin 113
Figure 3.28. Material Balance for Evaporation of Mannitol Solution
Conducting an overall material balance,
𝑭=𝑽+𝑪
Conducting a solute balance,
𝑭(0.0577) = 𝑪(0.20)
(1645𝑔)(0.0577) = 𝑪(0.20)
𝑪 = 𝟒𝟕𝟒. 𝟓𝟖𝒈
Substituting known values in the first equation,
𝑭=𝑽+𝑪
1645𝑔 = 𝑽 + 474.58𝑔
𝑽 = 𝟏𝟏𝟕𝟎. 𝟒𝟐𝒈
The material balance indicates that for a feed of 1645g solution at 5.77%
concentration, 1170.42g of water must be evaporated to increase the concentration to 20%.

PROJECT
Alkyd Resin 114

MATERIAL APPARATUS
 Mannitol Soultion  Thermometer
 Beaker
 Hotplate with magnetic stirrer
 Analytical Balance
Laboratory Set-up
Figure 3.28. Set-up for Evaporation of Mannitol Solution
A. Determination of Time of Evaporation

A-1. Objective
To determine the time of evaporation that would produce 200mg/mL of mannitol.
A-2. Hypothesis
The time of evaporation is 2 hours.
A-3. Procedure
1. Weigh 1645g of mannitol solution in a beaker

2. Place the beaker on a hotplate set to 100°C
3. Monitor the mass of the solution by weighing it every 10 minutes

PROJECT
Alkyd Resin 115
Table 3.27 Determination of the Time and Rate of Evaporation

Time (min) Mass of Solution (g) Mass of Water Evaporated (g)
0 1645 0
10 1533 112
20 1425 220
30 1322 323
40 1212 433
50 1102 543
60 1015 630
70 921 724
80 830 815
90 760 885
100 695 950
110 612 1033
120 554 1091
130 502 1143
140 471 1174
For calculations at time: 140 minutes,
𝒎𝒆𝒗𝒂𝒑𝒐𝒓𝒂𝒕𝒆𝒅 𝒘𝒂𝒕𝒆𝒓 = 𝒎𝒊𝒏𝒊𝒕𝒊𝒂𝒍 𝒔𝒐𝒍𝒖𝒕𝒊𝒐𝒏 − 𝒎𝒇𝒊𝒏𝒂𝒍 𝒔𝒐𝒍𝒖𝒕𝒊𝒐𝒏

𝑚𝑒𝑣𝑎𝑝𝑜𝑟𝑎𝑡𝑒𝑑 𝑤𝑎𝑡𝑒𝑟 = 1645𝑔 − 471𝑔
𝒎𝒆𝒗𝒂𝒑𝒐𝒓𝒂𝒕𝒆𝒅 𝒘𝒂𝒕𝒆𝒓 = 𝟏𝟏𝟕𝟒𝒈
The concentration of mannitol at time: 140 minutes is calculated as,
89𝑔 𝑚𝑎𝑛𝑛𝑖𝑡𝑜𝑙
𝐶𝑚𝑎𝑛𝑛𝑖𝑡𝑜𝑙 (%) = × 100%
𝑉𝑓𝑖𝑛𝑎𝑙 𝑠𝑜𝑙𝑢𝑡𝑖𝑜𝑛

PROJECT
Alkyd Resin 116
𝐶𝑚𝑎𝑛𝑛𝑖𝑡𝑜𝑙 = × 100%
(𝑚𝑓𝑖𝑛𝑎𝑙 𝑠𝑜𝑙𝑢𝑡𝑖𝑜𝑛 )(𝜌𝑓𝑖𝑛𝑎𝑙 𝑠𝑜𝑙𝑢𝑡𝑖𝑜𝑛 )−1
𝐶𝑚𝑎𝑛𝑛𝑖𝑡𝑜𝑙 = × 100%
𝑔 −1
(471𝑔) (1.0467 𝑚𝐿)
𝑪𝒎𝒂𝒏𝒏𝒊𝒕𝒐𝒍 = 𝟏𝟗. 𝟕𝟗%
A-6. Analysis
It was observed that at 140 minutes of evaporation, 1174g of water was already
evaporated which is close to the theoretical value of 1170g calculated using material balance.
This gives a final concentration of mannitol at 19.79% which is very close to the desired
concentration of 20%
A-7. Conclusion
The time of evaporation is 140 minutes yielding 471g of concentrated mannitol

solution at 19.77% w/v concentration.
IV. Esterification
Alkyd resins are organic polyesters derived from a polyhydric alcohol and a polybasic
acid. In this study, mannitol is the polyhydric alcohol and phthalic anhydride is the polybasic
acid to be used. When a hydroxyl group of mannitol reacts with a carboxylic acid group of
phthalic anhydride, an ester is formed. Water is the by-product of this reaction, hence, it is
sometimes referred to as a condensation reaction.
Figure 3.29. Esterification of Mannitol and Phthalic Anhydride

PROJECT
Alkyd Resin 117
The esterification reaction shown in Figure 2.8 is reversible, thus, water must be
removed in order to shift the reaction and favor the formation of esters. As the equation
shows, the reaction takes place between the hydroxyl group of the alcohol and the carboxyl
group of the acid (Elliott, 1993).
Parameters such as molar ratios of the reactants, reaction temperature, and reaction
time were considered in this study. The optimum parameters were chosen based on the acid
value of the alkyd resin after the reaction. The acid value is technically defined as the number
of milligrams of potassium hydroxide (KOH) required to neutralize one gram of sample under
a set of specified conditions. The acid value also determines the extent of reaction, where a
smaller value dictates a more complete esterification reaction. The acid value determination
was based on the formulas and methods of analysis provided by the International Union of
Pure and Applied Chemistry (IUPAC). The acid value and is calculated as:
𝒂𝑵
𝒂𝒄𝒊𝒅 𝒗𝒂𝒍𝒖𝒆 = 𝟓𝟔. 𝟏 ( )
𝒑
Where a is the volume of methanolic potassium hydroxide solution in mL, N is the

normality of the methanolic potassium hydroxide solution, and p is the weight of sample
product in grams. The normality of the methanolic KOH used throughout the experimentation
was 0.1374N.
Figure 3.30 Titration for Acid Value Determination

PROJECT
Alkyd Resin 118
The yield is simple taken as the quotient of the final mass and the initial mass. The yield is
calculated as,
𝒎𝒑𝒓𝒐𝒅𝒖𝒄𝒕
𝒚𝒊𝒆𝒍𝒅 (%) = × 𝟏𝟎𝟎%
𝒎𝒓𝒆𝒂𝒄𝒕𝒂𝒏𝒕𝒔

MATERIAL APPARATUS
 Concentrated Mannitol Solution  Thermometer
 Phthalic Anhydride  250mL Beaker
 Benzoic Acid  Hotplate with magnetic stirrer
 Stearic Acid  Analytical Balance
 Oleic Acid
Laboratory Set-up
Figure 3.31. Laboratory Set-up for Esterification Figure 3.32. Production of Alkyd Resin
A. Determination of the Optimal Alkyd Resin Modifier

A-1. Objective
To determine the optimal type of modifier that would yield a clear and fluid alkyd resin
with a relatively low acid value
A-2. Hypothesis
The optimal modifier to use is oleic acid

PROJECT
Alkyd Resin 119
A-3. Procedure
1. Weigh 5 sets of 471g concentrated mannitol solution in a beaker.
2. For a molar ratio of 1:1:1 of mannitol to phthalic anhydride to palmitic acid, add 72.33g
of phthalic anhydride and 125.25g of palmitic acid to the beaker.
3. React the mixture at 240°C for 1 hour then measure the acid value.
4. Replicate the procedure using benzoic and oleic acids as modifier.
Table 3.28 Determination of the Optimal Alkyd Resin Modifier

TRIAL 1 2 3
Type of Modifier Palmitic Acid Benzoic Acid Oleic Acid
Mass of Mannitol in Solution (g) 89.96 89.96 89.96
Molar Ratio
(mol mannitol: mol phthalic 1:1:1 1:1:1 1:1:1
anhydride: mol modifier)
Mass of Phthalic Anhydride (g) 72.33 72.33 72.33
Mass of Modifier (g) 125.25 59.64 137.97

Temperature (°C) 240°C 240°C 240°C
Time (min) 60 60 60
Mass of Alkyd Resin (g) 277 211 290
Acid Value (mgKOH) 6521.32 7325.14 5401.37
Yield (%) 96.33 95.08 96.58
Cloudy liquid Clear solid Clear liquid
Appearance

PROJECT
Alkyd Resin 120
The amount of mannitol in 471g of solution is calculated as follows,
𝒎𝒎𝒂𝒏𝒏𝒊𝒕𝒐𝒍 = (𝑪𝒎𝒂𝒏𝒏𝒊𝒕𝒐𝒍 )(𝑽𝒔𝒐𝒍𝒖𝒕𝒊𝒐𝒏 )
𝑚𝑚𝑎𝑛𝑛𝑖𝑡𝑜𝑙 = (𝐶𝑚𝑎𝑛𝑛𝑖𝑡𝑜𝑙 )(𝑚 × 𝜌−1 )𝑠𝑜𝑙𝑢𝑡𝑖𝑜𝑛
From the previous process, the concentration mannitol and density of solution were
determined. Substituting these values to the above equation,
𝑔 −1
𝑚𝑚𝑎𝑛𝑛𝑖𝑡𝑜𝑙 = (0.1977) (471𝑔 × 1.0467 )
𝑚𝐿 𝑠𝑜𝑙𝑢𝑡𝑖𝑜𝑛
𝒎𝒎𝒂𝒏𝒏𝒊𝒕𝒐𝒍 = 𝟖𝟖. 𝟗𝟔𝒈
The acid value for a resin sample of 0.8962g requiring 628mL of 0.1374N KOH is calculated as,
𝒂𝑵
𝒑
(628𝑚𝐿)(0.1374𝑁)
𝑎𝑐𝑖𝑑 𝑣𝑎𝑙𝑢𝑒 = 56.1 [ ]
0.8962𝑔
𝒂𝒄𝒊𝒅 𝒗𝒂𝒍𝒖𝒆 = 𝟓𝟒𝟎𝟏. 𝟑𝟕 𝒎𝒈𝑲𝑶𝑯
Finally, the yield is calculated as,
𝒚𝒊𝒆𝒍𝒅 (%) = × 𝟏𝟎𝟎%
290𝑔
𝑦𝑖𝑒𝑙𝑑 (%) = × 100%
(89.96 + 72.33 + 137.97)𝑔
𝒚𝒊𝒆𝒍𝒅 (%) = 𝟗𝟔. 𝟓𝟖%

PROJECT
Alkyd Resin 121
A-6. Analysis
Oleic acid as a modifier gave a clear liquid product as compared to the cloudy liquid
that stearic acid and clear solid that benzoic acid yielded. Besides the appearance, oleic acid
as a modifier gave the lowest number of acid value. Acid value is an indicator of how complete
the esterification reaction is, where a lower value represents a more complete reaction.
Comparing the three modifiers based on the appearance of the product obtained
In terms of the yield, all three modifiers are uniform at 96.33, 95.08, and 96.58%.
Nevertheless, oleic acid modifier gave the highest yield at 96.58%
A-7. Conclusion
The optimal alkyd resin modifier type is oleic acid with the lowest acid value at 5401.37
mgKOH and a percent yield of 96.58%.
B. Determination of the Optimal Molar Ratio of Mannitol to Phthalic Anhydride to Oleic Acid
B-1. Objective
To determine the optimal molar ratio of mannitol to phthalic anhydride to oleic acid
that would yield high amount of alkyd resin with low acid value.
B-2. Hypothesis
The optimal modifier to use is 1:1:1
B-3. Procedure
2. For a molar ratio of 1:1:1 of mannitol to phthalic anhydride to oleic acid, add 72.33g
of phthalic anhydride and 137.97g of oleic acid to the beaker.
4. Replicate the procedure using ratios, 1:1:2, 1:1:3, 1:2:1, and 1:3:1

PROJECT
Alkyd Resin 122
Table 3.29 Determination of the Optimal Molar Ratio of Mannitol to Phthalic Anhydride to Oleic Acid
TRIAL 1 2 3 4 5
Mass of Mannitol in
89.96 89.96 89.96 89.96 89.96
Solution (g)
Molar Ratio
(mol mannitol: mol
1:1:1 1:1:2 1:1:3 1:2:1 1:3:1
phthalic anhydride:
mol modifier)
Mass of Phthalic
72.33 72.33 72.33 144.66 216.99
Anhydride (g)
Mass of Oleic Acid
137.97 275.94 413.91 137.97 137.97
(g)
Time (min) 60 60 60 60 60
Mass of Alkyd Resin
287 411 531 342 425
(g)
Acid Value (mgKOH) 5321.12 8540.15 11567.21 7985.14 10987.02
Cloudy Cloudy
Appearance Clear liquid Clear solid Clear liquid
liquid liquid
Yield (%) 95.58 93.79 92.64 91.79 95.52
Figure 3.33. Alkyd Resin at Different Molar Ratio

PROJECT
Alkyd Resin 123
𝑔 −1
𝑚𝑚𝑎𝑛𝑛𝑖𝑡𝑜𝑙 = (0.1977) (471𝑔 × 1.0467 )
𝒂𝑵
𝒑
(498𝑚𝐿)(0.1374𝑁)
0.7214𝑔
𝒂𝒄𝒊𝒅 𝒗𝒂𝒍𝒖𝒆 = 𝟓𝟑𝟐𝟏. 𝟏𝟏𝟔𝟗 𝒎𝒈𝑲𝑶𝑯
𝒚𝒊𝒆𝒍𝒅 (%) = × 𝟏𝟎𝟎%
287𝑔
𝑦𝑖𝑒𝑙𝑑 (%) = × 100%
(89.96 + 72.33 + 137.97)𝑔
𝒚𝒊𝒆𝒍𝒅 (%) = 𝟗𝟓. 𝟓𝟖%

PROJECT
Alkyd Resin 124
B-6. Analysis
Based on the appearance of the products, trials 4 and 5 did not conform to the
standard and existing product which is a clear liquid. Trials 1, 2, and 3 yielded a clear liquid,
however, first trial gave the lowest acid value indicating that it has a higher extent of reaction
than the other trials. Moreover, trial 1 has the highest percent yield at 95.58%
B-7. Conclusion
The optimal ratio of mannitol to phthalic anhydride to oleic acid is 1:1:1 which gave
the lowest acid value and a percent yield of 95.58%
C. Determination of the Optimal Temperature of Esterification

C-1. Objective
To determine the optimal temperature of esterification that would yield high amount
of alkyd resin with low acid value.
C-2. Hypothesis
The optimal temperature is 240°C
C-3. Procedure
4. Replicate the procedure using temperatures 230, 240, 250, 260°C

PROJECT
Alkyd Resin 125
Table 3.30 Determination of the Optimal Temperature of Esterification

TRIAL 1 2 3 4 5
Mass of Mannitol in
89.96 89.96 89.96 89.96 89.96
Solution (g)
Molar Ratio
(mol mannitol: mol
1:1:1 1:1:1 1:1:1 1:1:1 1:1:1
phthalic anhydride:
mol modifier)
Mass of Phthalic
72.33 72.33 72.33 72.33 72.33
Anhydride (g)
Mass of Oleic Acid (g) 137.97 137.97 137.97 137.97 137.97
Time (min) 60 60 60 60 60
Mass of Alkyd Resin (g) 288 285 285 271 259
Acid Value (mgKOH) 6524.12 5987.68 5273.89 4536.14 3787.68
Almost
Appearance Light yellow Light brown Amber Dark brown
black
Yield (%) 95.92 94.92 94.92 90.26 86.26
Figure 3.34. Alkyd Resin under Different Temperatures

PROJECT
Alkyd Resin 126

𝑔 −1
𝑚𝑚𝑎𝑛𝑛𝑖𝑡𝑜𝑙 = (0.1977) (471𝑔 × 1.0467 )
𝒂𝑵
𝒑
(562𝑚𝐿)(0.1374𝑁)
0.8214𝑔
𝒂𝒄𝒊𝒅 𝒗𝒂𝒍𝒖𝒆 = 𝟓𝟐𝟕𝟑. 𝟖𝟗𝟏𝟕 𝒎𝒈𝑲𝑶𝑯
𝒚𝒊𝒆𝒍𝒅 (%) = × 𝟏𝟎𝟎%
285𝑔
𝑦𝑖𝑒𝑙𝑑 (%) = × 100%
(89.96 + 72.33 + 137.97)𝑔
𝒚𝒊𝒆𝒍𝒅 (%) = 𝟗𝟒. 𝟗𝟐%

PROJECT
Alkyd Resin 127
C-6. Analysis
Based on the appearance of the products, trials 4 and 5 did not conform to the
standard and existing product which is of light brown to amber in color. Trials 4 and 5 are
darker in color than the existing product attributed to high reaction temperature. Trials 1 and
2 yielded a clear liquid but are light in color, attributed to low reaction temperatures. Trial 3
yielded a clear amber liquid similar to the existing product.
Although trials 4 and 5 gave a lower acid value than trial 3, it was eliminated
considering its appearance. Considering the first three trials, trial 3 has the lowest acid value
and has more resemblance with the existing product in terms of color.
C-7. Conclusion
The optimal temperature of esterification is 240°C which yielded a clear amber liquid
with a percent yield of 94.92%
D. Determination of the Optimal Time of Esterification

D-1. Objective
To determine the optimal time of esterification that would yield high amount of alkyd
resin with low acid value.
D-2. Hypothesis
The optimal time is 300 minutes
D-3. Procedure
3. React the mixture at 240°C for 60 minutes then measure the acid value.
4. Replicate the procedure using times 120, 180, 240, 300 minutes

PROJECT
Alkyd Resin 128
Table 3.31. Determination of the Optimal Time of Esterification
TRIAL 1 2 3 4 5
Mass of Mannitol in
89.96 89.96 89.96 89.96 89.96
Solution (g)
Molar Ratio
(mol mannitol: mol
1:1:1 1:1:1 1:1:1 1:1:1 1:1:1
phthalic anhydride:
mol modifier)
Mass of Phthalic
72.33 72.33 72.33 72.33 72.33
Anhydride (g)
Mass of Oleic Acid
137.97 137.97 137.97 137.97 137.97
(g)
Time (min) 60 120 180 240 300
Mass of Alkyd Resin
282 284 285 287 288
(g)
Acid Value (mgKOH) 5293.14 798.28 102.98 9.56 7.14
Amber clear Amber clear Amber clear Amber clear Brown clear
Appearance
liquid liquid liquid liquid liquid
Yield (%) 93.92 94.58 94.92 95.58 95.92
D-5. Sample Calculation

PROJECT
Alkyd Resin 129
𝑔 −1
𝑚𝑚𝑎𝑛𝑛𝑖𝑡𝑜𝑙 = (0.1977) (471𝑔 × 1.0467 )
The acid value for a resin sample of 5.2436 requiring 6.5mL of 0.1374N KOH is calculated as,
𝒂𝑵
𝒑
(6.5𝑚𝐿)(0.1374𝑁)
5.2436𝑔
𝒂𝒄𝒊𝒅 𝒗𝒂𝒍𝒖𝒆 = 𝟗. 𝟓𝟓𝟓𝟏 𝒎𝒈𝑲𝑶𝑯
𝒚𝒊𝒆𝒍𝒅 (%) = × 𝟏𝟎𝟎%
287𝑔
𝑦𝑖𝑒𝑙𝑑 (%) = × 100%
(89.96 + 72.33 + 137.97)𝑔
𝒚𝒊𝒆𝒍𝒅 (%) = 𝟗𝟓. 𝟓𝟖%
D-6. Analysis
Based on the data, it was observed that the acid value drastically decreased with an
increase in reaction time. The acid values of trials 4 and 5 are the lowest, indicating that the
esterification is almost complete. However, trial 5 with a reaction time of 300 minutes yielded
a clear liquid that is significantly darker than the existing product. Additionally, the acid value
of trial 4 at 240 minutes is already relatively low.
D-7. Conclusion
The optimal time of esterification is 240 minutes which yielded a clear amber liquid
with a low acid value and a percent yield of 95.58%

PROJECT
Alkyd Resin 130
SUMMARY OF EXPERIMENTAL INPUT AND OUTPUT
Several parameters were varied in each process for optimization. The table below
shows the experimental input and the output in each process, as well as the byproducts
generated.
Table 3.32. Summary of Experimental Input and Output
Process Input Output
Drying 250 g Copra Meal 230 g Dried Copra Meal

Grinding 230 g Dried Copra Meal 226 g Ground Copra Meal
226 g Ground Copra Meal 759 g Mixture (Ground Copra
Leaching
533 g (678 mL) Isopropanol Meal - Isopropanol)
759g Mixture (Ground Copra 206 g Defatted Copra Meal
Filtration
Meal - Isopropanol) 492 g Spent Solvent and Oil
206 g Defatted Copra Meal
1878g Hydrolyzed Mixture
Acid Hydrolysis 1672g (1648 mL) Phosphoric
(Defatted Copra Meal – Acid)
Acid
1878g Hydrolyzed Mixture 1706 g Hydrolysate
Filtration
(Defatted Copra Meal –Acid) 98g Hydrolysis Cake
1706g Hydrolysate 1877g Mixture (Hydrolysate-
Neutralization
171 g Calcium Carbonate Calcium Hydroxide)
1877g Mixture (Hydrolysate- 1638g Mannose Solution
Filtration
Calcium Hydroxide) 222g Neutralized Cake
1638g Mannose Solution
Reduction 1645g Mannitol Solution
26.5g Sodium Borohydride
471g Concentrated Mannitol
Evaporation 1645g Mannitol Solution
Solution
Solution
Esterification 287g Alkyd Resin
73g Phthalic Anhydride
138g Oleic Acid

PROJECT
Alkyd Resin 131
SUMMARY OF OPTIMUM PARAMETERS
In order to achieve optimum yield of product, the following operating conditions in each
process should be used as shown in the table below. The optimum parameter values from the
experiment were used in the scaled-up designs in the technical study.
Table 3.33. Summary of Optimum Parameters
Process Parameter Optimum Parameter

Temperature 80 C
Drying
Time 4 hours
Grinding Time 8 minutes
Type of Solvent Isopropanol
Ground Copra Meal to Solvent Ratio 1:3 (w/v)
Leaching
Temperature 70 C
Time 60 minutes
Type of Acid Phosphoric Acid
Acid Concentration 2.60 (%w/w)
Acid Hydrolysis Defatted Copra Meal to Acid Ratio 1:8 (w/v)
Temperature 100 C
Time 90 minutes
Neutralization Type of Neutralizing Agent Calcium Hydroxide
Mannose to NaBH4 Molar Ratio 1:1.25
Reduction Temperature 25°C
Time 90 minutes
Evaporation Time 140 minutes
Modifier Type Oleic Acid
Molar Ratio (Mannitol:Phthalic
1:1:1
Esterification Anhydride:Oleic Acid)
Temperature 240°C
Time 240 minutes

PROJECT
Alkyd Resin 132
SUMMARY OF EXPERIMENTAL DRY-RUN
A dry-run, wherein the optimum operating conditions was used, was performed to
determine if there would be significant change in the yield of the intermediate process
materials and the product. The table below shows the amount of input and output in the dry-
run.
Table 3.34. Summary of Experimental Input and Output (Based on Dry-Run)

Process Input Output
231 g Dried Copra Meal
Drying 250 g Copra Meal
19 g Water Vapor
227 g Ground Copra Meal
Grinding 231 g Dried Copra Meal
4 g Oversized Copra Meal
227 g Ground Copra Meal 763 g Mixture (Ground Copra
Leaching
536 g (681 mL) Isopropanol Meal - Isopropanol)
763 g Mixture (Ground Copra 207 g Defatted Copra Meal
Filtration
Meal - Isopropanol) 556 g Spent Isopropanol and Oil
207 g Defatted Copra Meal
1895 g Hydrolyzed Mixture
Acid Hydrolysis 1688 g (1656 mL) 2.6% (w/v)
(Defatted Copra Meal – Acid)
Phosphoric Acid
1895 g Hydrolyzed Mixture 1792 g Hydrolysate
Filtration
(Defatted Copra Meal –Acid) 103 g Hydrolyzed Cake
1792 g Hydrolysate 1972 g Mixture (Hydrolysate-
Neutralization
180 g Calcium Hydroxide Calcium Hydroxide)
1972 g Mixture (Hydrolysate- 1730g Mannose Solution
Filtration
Calcium Hydroxide) 242g Neutralized Cake
1730 g Mannose Solution
Reduction 1759g Mannitol Solution
29 g Sodium Borohydride
Evaporation 1759 g Mannitol Solution Solution
1254 Water Vapor
308 g Alkyd Resin
Solution
Esterification
79 g Phthalic Anhydride
425g Water Vapor
149 g Oleic Acid

PROJECT
Alkyd Resin 133
SUMMARY OF EQUIVALENT INDUSTRIAL EQUIPMENT
The experimental study was done in a laboratory scale. The equivalent industrial
equipment of several laboratory apparatus used in the experiment are listed in the table
below. Moreover, the optimum parameter values from the experiment were used in the scaled-
up designs in the technical study.
Table 3.35 Summary of Equivalent Industrial Equipment
Process Laboratory Apparatus Industrial Equipment

Drying Oven Dryer Rotary Dryer
Grinding Blender Ball Mill
Leaching Beaker with Magnetic Stirrer Leaching Tank
Filtration Filter paper & funnel Rotary Drum Filter
Acid Hydrolysis 3-neck round bottom flask Hydrolysis Reactor
Filtration Filter paper & funnel Plate and Frame Filter Press 1
Neutralization Beaker with Magnetic Stirrer Neutralization Reactor
Filtration Filter paper & funnel Plate and Frame Filter Press 2
Reduction Beaker with Magnetic Stirrer Reduction Reactor
Evaporation Beaker and Hotplate Evaporator
Esterification Beaker with Magnetic Stirrer Esterification Reactor

PROJECT
Alkyd Resin 134
DETERMINATION OF PHYSICAL PROPERTIES

I. Determination of Density
A. Determination of Bulk Density of Solids and Mixtures
In designing material handling and storage equipment, the bulk density of the raw
material, intermediate process materials, by-products, and the main product is needed. Bulk
density is defined as the mass of the material divided by the total volume they occupy. The
total volume includes particle volume, inter-particle void volume, and internal pore volume.
The bulk density of a material is calculated as:
𝑊𝑠 𝑚𝑎𝑠𝑠 𝑜𝑓 𝑠𝑎𝑚𝑝𝑙𝑒 (𝑔)

𝜌𝑏 = =
𝑉 𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑐𝑜𝑛𝑡𝑎𝑖𝑛𝑒𝑟 (𝑚𝐿)
A-1. Materials and Apparatus

MATERIAL APPARATUS
 Dried Copra Meal  1L Beaker
 Ground Copra Meal
 Defatted Copra Meal
 Hydrolyzed Cake
 Neutralized Cake
 Ground Copra Meal-Isopropanol Mixture
 Defatted Copra Meal-Acid Mixture
 Hydrolysate-Calcium Hydroxide Mixture
A-2. Laboratory Set-up
Figure 3.35. Determination of Bulk Density of Solids

PROJECT
Alkyd Resin 135
A-3. Objective
To determine the bulk density of solid materials in the experiment such as copra meal,
dried copra meal, ground copra meal, defatted copra meal, hydrolyzed cake, and neutralized
cake, and mixtures (ground copra meal-isopropanol mixture, defatted copra meal-acid
mixture, hydrolysate-calcium hydroxide mixture) that will be used in designing handling and
storage equipment.
A-4. Procedure
For copra meal, dried copra meal, ground copra meal

1. Place the copra meal in a beaker until it fully occupy the 1000mL volume.
2. Weigh and record the sample and repeat for 5 trials.
3. Repeat the steps using dried copra meal, ground copra meal.
For defatted copra meal, hydrolyzed cake, and neutralized cake, ground copra meal-
isopropanol mixture, defatted copra meal-acid mixture, hydrolysate-calcium hydroxide
mixture
1. Place and weigh the defatted copra meal in a beaker, and record the volume occupied,
then calculate the bulk density.
2. Repeat the steps using hydrolyzed cake, neutralized cake, ground copra meal-
isopropanol mixture, defatted copra meal-acid mixture and hydrolysate-calcium
hydroxide mixture.

PROJECT
Alkyd Resin 136
Figure 3.36. Bulk Density of Different Solids and Mixtures in the Experimentation
Table 3.36. Determination of Bulk Density of Copra Meal
Trial Mass of Copra Meal (g) Volume Occupied (mL) Bulk Density (g/mL)
1 494 1000 0.494
2 475 1000 0.475
3 499 1000 0.499
4 479 1000 0.479
5 485 1000 0.485
Average 0.486

PROJECT
Alkyd Resin 137
Table 3.37. Determination of Bulk Density of Dried Copra Meal
Trial Mass of Dried Copra Meal (g) Volume Occupied (mL) Bulk Density (g/mL)
1 489 1000 0.489
2 496 1000 0.496
3 505 1000 0.505
4 493 1000 0.493
5 492 1000 0.492
Average 0.495
Table 3.38. Determination of Bulk Density of Ground Copra Meal
Trial Mass of Ground Copra Meal (g) Volume Occupied (mL) Bulk Density (g/mL)
1 561 1000 0.561
2 579 1000 0.579
3 572 1000 0.572
4 598 1000 0.598
5 525 1000 0.525
Average 0.567
Table 3.39. Determination of Bulk Density of Solids
Solid Mass of Solid (g) Volume Occupied (mL) Bulk Density (g/mL)
Defatted Copra Meal 176 300 0.5867
Hydrolyzed Cake 149 500 0.298
Neutralized Cake 289 350 0.8257
Table 3.40. Determination of Density of Mixtures
Trial Mass of Mixture (g) Volume Occupied (mL) Density (g/mL)

Ground Copra Meal-
680 750 0.9067
Isopropanol Mixture
Defatted Copra Meal-
1726 1700 1.0153
Acid Mixture
Hydrolysate-Calcium
1512 1500 1.0080
Hydroxide Mixture

PROJECT
Alkyd Resin 138
𝑊𝑠 494.00 𝑔 𝑔
𝐷𝑒𝑛𝑠𝑖𝑡𝑦 (𝜌𝑏 ) = = = 0.494
𝑉 1000 𝑚𝐿 𝑚𝐿
0.494 + 0.475 + 0.499 + 0.479 + 0.485 𝑔

𝐴𝑣𝑒𝑟𝑎𝑔𝑒 𝐷𝑒𝑛𝑠𝑖𝑡𝑦 (𝜌𝑎𝑣𝑒 ) = = 0.486
5 𝑚𝐿
A-7. Conclusion
The average bulk density of copra meal, ground copra meal, defatted copra meal,
hydrolyzed cake, and neutralized cake are 0.486 g/mL, 0.495 g/mL, and 0.567 g/mL
respectively and the bulk density of defatted copra meal, hydrolyzed cake, neutralized cake,
ground copra meal-isopropanol mixture, defatted copra meal-acid mixture, and hydrolysate-
calcium hydroxide mixture are 0.5867, 0.298, 0.8257, 0.9067, 1.1053, 1.0080g/mL
respectively.
B. Determination of Density of Liquids
Density determination by pycnometer is a very precise method. The pycnometer is a

glass flask with a close-fitting ground glass stopper with a capillary hole through it. This fine
hole releases a spare liquid after closing a top-filled pycnometer and allows for obtaining a
given volume of measured and/or working liquid with a high accuracy.
B-1. Materials and Apparatus
MATERIAL APPARATUS
 Spent Isopropanol  Analytical Balance
 Hydrolysate  Pycnometer (50mL)
 2.6% Phosphoric Acid
 Mannose Solution
 Mannitol Solution
 Concentrated Mannitol
 Alkyd Resin

PROJECT
Alkyd Resin 139
B-2. Laboratory Set-up
Figure 3.37. Determination of Density of Liquids
B-3. Objective
To determine the density of liquid materials in the experiment such as spent

isopropanol, 2.6% (w/v) phosphoric acid, hydrolysate, mannose solution, mannitol solution,
concentrated mannitol, and alkyd resin that will be used in designing handling and storage
equipment.
B-4. Procedure
1. Weigh the initial mass of empty 50mL pycnometer; fill the pycnometer with spent
isopropanol then weigh the final mass.
2. Calculate the mass of spent isopropanol by subtracting final to initial mass; then divide
by the volume of 50mL to determine the density.
3. Repeat the steps using hydrolysate, mannose solution, mannitol solution,
concentrated mannitol, and alkyd resin for 3 trials each.

PROJECT
Alkyd Resin 140

Table 3.41. Determination of Density of Spent Isopropanol
Mass of
Mass of
Pycometer with Mass of Spent Density
Trial Pycnometer Volume (mL)
Spent Isopropanol Isopropanol (g) (g/mL)
(g)
(g)
1 30 71 41 50 0.82
2 30 72 42 50 0.84
3 30 72 42 50 0.84
Average 0.8333
Table 3.42. Determination of Density of 2.6% (w/v) Phosphoric Acid

Mass of
Mass of Mass of 2.6%
Pycometer with Density
Trial Pycnometer Phosphoric Acid Volume (mL)
2.6% Phosphoric (g/mL)
(g) (g)
Acid (g)
1 30 83 53 50 1.06
2 30 83 53 50 1.06
3 30 83 53 50 1.06
Average 1.06
Table 3.43. Determination of Density of Hydrolysate

Mass of Mass of
Mass of Density
Trial Pycnometer Pycometer with Volume (mL)
Hydrolysate (g) (g/mL)
(g) Hydrolysate (g)
1 30 85 55 50 1.10
2 30 85 55 50 1.10
3 30 84 54 50 1.08
Average 1.0933

PROJECT
Alkyd Resin 141
Table 3.44. Determination of Density of Mannose Solution

Mass of
Mass of Pycometer Mass of
Density
Trial Pycnometer with Mannose Volume (mL)
(g/mL)
(g) Mannose Solution (g)
Solution (g)
1 30 82 52 50 1.04
2 30 82 52 50 1.04
3 30 82 52 50 1.04
Average 1.04
Table 3.45. Determination of Density of Mannitol Solution

Mass of
Mass of Mass of
Pycometer
Trial Pycnometer Mannitol Volume (mL) Density (g/mL)
with Mannitol
(g) Solution (g)
Solution (g)
1 30 83 53 50 1.06
2 30 84 54 50 1.08
3 30 83 53 50 1.06
Average 1.0667
Table 3.46. Determination of Density of Concentrated Mannitol Solution

Mass of
Mass of
Pycometer Mass of Density
with Mannitol Mannitol (g) (g/mL)
(g)
(g)
1 30 85 55 50 1.10
2 30 84 54 50 1.08
3 30 85 55 50 1.10
Average 1.0933

PROJECT
Alkyd Resin 142
Table 3.47. Determination of Density of Alkyd Resin

Mass of
Mass of
Pycometer Mass of Alkyd Density
with Alkyd Resin (g) (g/mL)
(g)
Resin (g)
1 30 50
2 30 50
3 30 50
Average
𝑊𝑠𝑝𝑒𝑛𝑡 𝑖𝑠𝑜𝑝𝑟𝑜𝑝𝑎𝑛𝑜𝑙 71 − 50𝑔 𝑔

𝐷𝑒𝑛𝑠𝑖𝑡𝑦 (𝜌𝑏 ) = = = 0.82
𝑉𝑜𝑙𝑢𝑚𝑒 50𝑚𝐿 𝑚𝐿
A-7. Conclusion
The density of spent isopropanol, 2.6% (w/v) phosphoric acid, hydrolysate, mannose
solution, mannitol solution, concentrated mannitol, and alkyd resin are 0.8333, 1.06, 1.0933,
1.04, and 1.0467, respectively.
II. Determination of Viscosity of Liquids
The viscosity of a liquid is a measure of the resistance to flow of one portion of a liquid
past another portion. One of the most frequently used methods of measuring viscosity is the
determination of the time necessary for a given volume of liquid to pass through a length of
capillary tubing. Ostwald viscometer is an example of this type of apparatus.
If 1 , 𝑑1 and 𝑡1 represent the viscosity, density and flow time for liquid under test and
2 , 𝑑2 and 𝑡2 represent the corresponding values for the reference liquid, then
1 𝑑1 𝑡1
=
2 𝑑2 𝑡2

PROJECT
Alkyd Resin 143
For determination of viscosity of samples,
2 𝑑1 𝑡1
1 =
𝑑2 𝑡2
A-1. Materials and Apparatus
MATERIAL APPARATUS
 Phosphoric Acid (2.6%)  Ostwald Viscometer
 Spent Isopropanol  Stopwatch
 Hydrolysate  Iron clamp
 Mannose Solution  Iron Stand
 Mannitol Solution
 Concentrated Mannitol
A-2. Laboratory Set-up
Figure 3.38. Determination of Viscosity of Liquids

PROJECT
Alkyd Resin 144
A-3. Objective
To determine the viscosity of a liquid using the Ostwald viscometer
A-4. Procedure
1. Put a certain amount of liquid in the large bulge viscometer and pull it by pipette until
the small bulge is full.
2. Let the liquid to flow through the capillary tube with run time when the liquid reaches
the mark shown on the viscometer and then stopped time when the liquid reaches the
bottom mark. Repeat the experiment and record the results (take average of results).
3. Repeat the experiment to other liquids.
Figure 3.39. Viscosity of Phosphoric Acid (2.6%), Spent Isopropanol, Hydrolysate, Mannose
Solution, Mannitol Solution and Concentrated Mannitol
Table 3.48. Determination of Viscosity of Water (Reference Liquid)

Trial Time (sec) Density (g/mL) Viscosity (poise)
1 115.44 0.9970 0.0091
2 112.90 0.9970 0.0091
3 112.37 0.9970 0.0091
Average 113.57 0.9970 0.0091

PROJECT
Alkyd Resin 145
Table 3.49 Determination of Viscosity of Phosphoric Acid (2.6%)

1 114.10 1.06 0.0097
2 112.38 1.06 0.0096
3 115.44 1.06 0.0098
Average 0.0097
Table 3.50 Determination of Viscosity of Spent Isopropanol

1 335.92 0.8333 0.0225
2 338.78 0.8333 0.0227
3 335.65 0.8333 0.0225
Average 0.0226
Table 3.51. Determination of Viscosity of Hydrolysate

1 161.29 1.0933 0.0142
2 161.70 1.0933 0.0142
3 160.32 1.0933 0.0141
Average 0.0142
Table 3.52. Determination of Viscosity of Mannose Solution

1 123.98 1.04 0.0104
2 122.41 1.04 0.0102
3 124.25 1.04 0.0104
Average 0.0103

PROJECT
Alkyd Resin 146
Table 3.53. Determination of Viscosity of Mannitol Solution

1 173.31 1.0667 0.0149
2 174.60 1.0667 0.0150
3 175.13 1.0667 0.0150
Average 0.0150
Table 3.54. Determination of Viscosity of Concentrated Mannitol Solution

1 136.49 1.0933 0.0120
2 136.25 1.0933 0.0120
3 135.07 1.0933 0.0119
Average 0.0120
Table 3.55. Determination of Viscosity of Alkyd Resin

1
2
3
Average

2 𝑑1 𝑡1
1 =
𝑑2 𝑡2
(0.0091 𝑝𝑜𝑖𝑠𝑒)(0.8333 𝑔/𝑚𝐿)(335.92 𝑠)
1 =
(0.9970 𝑔/𝑚𝐿)(113.57 𝑠)
1 = 0.0225 𝑝𝑜𝑖𝑠𝑒
A-7. Conclusion
The viscosity of phosphoric acid (2.6%), spent isopropanol, hydrolysate, mannose

solution, mannitol solution and concentrated mannitol are 0.0097 poise, 0.0226 poise,
0.0142 poise, 0.0103 poise, 0.0150 poise and 0.0120 respectively.

PROJECT
Alkyd Resin 147
QUALITATIVE ANALYSIS OF MANNOSE SOLUTION, CONCENTRATED MANNITOL SOLUTION,

AND ALKYD RESIN
Fourier Transform Infrared Spectroscopy (FTIR) Analysis was employed in order to

qualitatively analyze the intermediate process products such as mannose solution and
mannitol solution, and the product formed which is the alkyd resin. The FTIR analysis was
carried out at De La Salle University Chemistry Instrument and Research Testing Center.
I. MANNOSE SOLUTION (produced after hydrolysis and neutralization)
Figure 3.40 IR Spectrum of Mannose during Experiment
The peaks represent areas of the spectrum where specific bond vibrations occur. In
the 4000 – 2500 cm-1 region, an element (C or O or N) is detected to have a single bond to
H. Moreover, the rounded peak at 3361.70 cm-1 is attributed to O-H stretching bond
(Sasivardhan, O., 2016). Also, the broader the peak, the more O-H bond is present. On the
other hand, 1650 - 1550 cm-1 region corresponds to double bonded element to C wherein a
sharp peak at 1639.44 cm-1 is attributed to C=O bonding. Lastly, the peak at 1380.29 cm-1
corresponds to C-C bonding. The existence of the three bonds O-H, C=O and C-C proves the

PROJECT
Alkyd Resin 148
formation of mannose solution during the experiment. This was compared to the IR spectra
obtained from National Institute of Standards and Technology (NIST) shown below. It shows
that the two spectra has the same peaks at 3500-2500cm-1 and 2000-1500 cm-1 regions.
Figure 3.41 IR Spectra of Mannose (National Institute of Standards and Technology)
II. MANNITOL SOLUTION (produced after reduction and evaporation)
Figure 3.42. IR Spectrum of Mannitol during the Experiment

PROJECT
Alkyd Resin 149
All of the peaks 3399.71, 3288.81, 2967.80, 2947.12, and 2906.66 cm-1 belong to
the 4000 – 2500 cm-1 region. Since the peaks are broad and round, these peaks corresponds
to O-H stretching bonds, meaning it is an alcohol, which is the functional group of mannitol.
This was compared to the IR spectra obtained from National Institute of Standards and
Technology (NIST) shown below. It shows that the two spectra has the same round peaks at
3500-2500cm-1 regions.
Figure 3.43 IR Spectra of Mannitol (National Institute of Standards and Technology)

PROJECT
Alkyd Resin 150
III. ALKYD RESIN
Figure 3.44. IR Spectrum of Alkyd Resin product
As shown above, round peaks at 3411.40 and 2940.37 cm-1 corresponds to O-H
stretching bond. This indicates the unreacted mannitol during esterification. Moreover, the
peak value at 1723.09 cm-1 is attributed to C=O stretching bond, which confirms the presence
of an ester bond in our product. Furthermore, it is close to the values according to Coatings
Technology: Fundamentals, Testing and Processing Techniques of 1730 cm-1.

PROJECT
Alkyd Resin 151
Figure 3.45. Experimental Flow Diagram

PROJECT
Alkyd Resin 152
Esterification of Hydrolyzed Copra (Cocos nucifera) Meal for the Production of Alkyd Resin
Dionisio, C.P., Fulugan, C.L., Redublo, A.P.
PROJECT STUDY 153

PROJECT
Alkyd Resin 154

Experimental Study: Pamantasan NG Lungsod NG Maynila

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PAMANTASAN NG LUNGSOD NG MAYNILA

University of the City of Manila

Esterification of Hydrolyzed Copra (Cocos nucifera) Meal for the Production of

Esterification of Hydrolyzed Copra (Cocos nucifera) Meal for the Production of

Figure 3.1. Conceptual Framework

ANALYSIS OF CONCEPTUAL FRAMEWORK

Esterification of Hydrolyzed Copra (Cocos nucifera) Meal for the Production of

Esterification of Hydrolyzed Copra (Cocos nucifera) Meal for the Production of

Figure 3.2. Theoretical Framework

Esterification of Hydrolyzed Copra (Cocos nucifera) Meal for the Production of

ANALYSIS OF THEORETICAL FRAMEWORK

Esterification of Hydrolyzed Copra (Cocos nucifera) Meal for the Production of

Table 3.1 Summary of Variation of Parameters

Esterification of Hydrolyzed Copra (Cocos nucifera) Meal for the Production of

Esterification of Hydrolyzed Copra (Cocos nucifera) Meal for the Production of

OBJECTIVES OF THE EXPERIMENTAL STUDY

Table 3.2. Standard, Existing, and Proposed Properties of Alkyd Resin

Esterification of Hydrolyzed Copra (Cocos nucifera) Meal for the Production of

Esterification of Hydrolyzed Copra (Cocos nucifera) Meal for the Production of

LIST OF REAGENTS AND LABORATORY APPARATUS AND EQUIPMENT

Table 3.3. Reagents and their Corresponding Properties

Reagent Process Function

Esterification of Hydrolyzed Copra (Cocos nucifera) Meal for the Production of

Laboratory Apparatus and Equipment

The laboratory apparatus used in the experimentation with their corresponding

Table 3.4. List of Laboratory Apparatus

Container used for

Analytical Balance Used to determine

Esterification of Hydrolyzed Copra (Cocos nucifera) Meal for the Production of

Stirring Rod Thermometer

Filter Paper A piece of porous Funnel

Esterification of Hydrolyzed Copra (Cocos nucifera) Meal for the Production of

Figure 3.3. Raw Material Collection

I-2. Characterization of Copra Meal

Table 3.5. Proximate Analysis of Copra Meal

Esterification of Hydrolyzed Copra (Cocos nucifera) Meal for the Production of

B. Equilibrium Moisture Content

According to the proximate analysis done by Department of Agriculture Laboratory, the

Determination of Equilibrium Moisture Content of Copra Meal

B-1. Materials and Apparatus

Esterification of Hydrolyzed Copra (Cocos nucifera) Meal for the Production of

B-2. Laboratory Set-up

Figure 3.4. Laboratory Set-up for Equilibrium Moisture Content Determination

Esterification of Hydrolyzed Copra (Cocos nucifera) Meal for the Production of

B-6. Data and Results

B-7. Sample Calculation

𝐷𝑖𝑓𝑓𝑒𝑟𝑒𝑛𝑐𝑒 = 𝑀𝑎𝑠𝑠(𝑡−1) − 𝑀𝑎𝑠𝑠𝑡

For equilibrium moisture content,

II. PRETREATMENT OF COPRA MEAL

Esterification of Hydrolyzed Copra (Cocos nucifera) Meal for the Production of

Materials and Apparatus

Figure 3.5. Laboratory Set-up for Drying of Copra Meal

Esterification of Hydrolyzed Copra (Cocos nucifera) Meal for the Production of

A. Determination of Optimum Drying Temperature of Copra Meal

Figure 3.6. Dried Copra Meal under Different Drying Temperatures

Esterification of Hydrolyzed Copra (Cocos nucifera) Meal for the Production of

A-5. Sample Calculation

𝐹𝑖𝑛𝑎𝑙 𝑀𝑜𝑖𝑠𝑡𝑢𝑟𝑒 𝐶𝑜𝑛𝑡𝑒𝑛𝑡 (%)

B. Determination of Optimum Drying Time of Copra Meal

Esterification of Hydrolyzed Copra (Cocos nucifera) Meal for the Production of

B-4. Data and Results

Figure 3.7. Dried Copra Meal under Different Drying Time