World Academy of Science, Engineering and Technology 48 2008
Manufacture of Alkyd Resin from Castor Oil
Nway Nay Hlaing1, Mya Mya Oo2
 endless use of the article of manufacture. The industrial
Abstract— Oil-modified alkyd resin was prepared from
crude castor oil. The experiment started with investigating the
optimum conditions for neutralization of crude castor oil and
bleaching of neutralized oil. Then the characteristics (iodine
value, viscosity, acid value, refractive index and color) of oils
were determined. Refined oil has iodine value of 90,
kinemetic viscosity of 4 St, free fatty acid value of 1,
refractive index of 1.474 and color number of 8. These results
showed that the refined oil was qualified to prepare
dehydrated castor oil. Dehydration of refined oil was carried
out at 210-220˚C under 600-640mmHg with the help of 1%
(wt%) NaHSO4 catalyst. The dehydrated castor oils were
analyzed for iodine value, viscosity and its set to touch time
and drying time were also investigated. Dehydrated castor oil
has iodine value of 140, kinemetic viscosity of 1.6 St, set to
touch time of 4 hr and drying time of 5 days. And then , oil
modified alkyd resin (acid value 6.6) was prepared from
dehydrated castor oil by alcoholysis method in excess of
glycerol and phthalic anhydride in the presence of 0.3% (wt%)
NaOH catalyst. The obtained resin was characterized by
Fourier Transform Infrared Spectrophotometer (FTIR) and the
properties were determined.
Keywords— Alcoholysis method, Alkyd resin, Castor oil,
Dehydrated castor oil, Polymerization
I. INTRODUCTION
Polymerization is one of the most important
industrial processes. Resins and emulsion are two main classes
of polymer. Alkyd resins are by far the most important class
of coating resins. It is estimated that alkyd resins contribute
about 70% to the conventional binders used in surface coating
today. The popularity of alky resins as vehicle for coatings is
largely due to their unique properties such as film hardness,
durability gloss and gloss retention, resistance to abrasion, etc.
impacted on them through modification with drying oil [1].
Alkyd resins are used in both clear and pigmented,
industrial and trade coating to protect and decorate a wide
variety of substances. The industrial coatings or finishes
generally are applied during the manufacturing process of the
item which they cover. Often they are specifically formulated
to meet both conditions desired for their application and the
1.Department of Chemical Engineering, Mandalay technological
University, Patheingyi Township, Mandalay, Myanmar, Myanmar 11011, e-
mail: nway.nay5@gmail.com
2.Yangon Technological University, Gyongone, Insein, Yangon, Myanmar
11011, e-mail : most7@gmail.com
155
finishes include primers and top coats for refrigerators,
furniture, and electrical equipment. In view of the
development of these items and sectors, the positive growth is
expected for paint industry [2].
Further the paint industry envisages a future
expansion in view of development in Automobile Industry,
utility in Nuclear Power Station, development in Corrosion
Resistant Coatings, expansion in housing activity and other
industry uses. The demand of alkyd resin being an ingredient
in Paint, Varnish and Printing ink industry would be linked
with the Paint industry.
There are many significant efforts that have been
made to increase alkyd resin production. Many researchers
have attempted to search the different sources for alkyd resin
preparation. Airegumen I Aigbodion et al [3] studied
enhancing the quality of alkyd resins using methyl esters of
rubber seed oil in 2004.
A lot of alkyd resins were imported to Myanmar
Paint Industries every year. In order to save foreign currency
outflow, it is needed to produce alkyd resin in Myanmar.
The oils that are mostly employed for alkyd resin
synthesis are linseed oil, soybean oil, dehydrated castor oil,
fish oil and tall oil. Myanmar being rich in aquatic and
terrestrial resources, every state and division is pursuing the
target of putting 500,000 acres under physic nut (castor oil) in
three years. Rural development tasks are included in the
national development endeavors that are being carried out by
the Nation target.
Castor oil is useful directly in protective coatings as a
plasticizer in alkyd systems, and blown castor oil is an
important nitrocellulose plasticizer. In commercial
manufacture of dehydrated castor oil, the aim is to produce the
most valuable material for use as a drying oil. By far the most
important coatings use of castor oil is in the form of
dehydrated castor. Dehydrated castor oil is now recognized as
an individual drying oil with its own characteristic properties
and advantages. The drying oils owe their value as raw
materials for decorative and protective coatings to their ability
to polymerize or “dry” after they have been applied to a
surface to form tough, adherent, impervious, and abrasion
resistance films. The advantages claimed in surface coating
applications include excellent odor and heat bleachability,
good drying properties, more uniform polymer structure, and
lack of after-yellowing. The dehydrated castor oil is non-
yellowing oil and so this can give requirements of coating
industries [2,4,5,6,7].
2. Materials and Methods
2.1. Neutralization of Crude Castor Oil
 World Academy of Science, Engineering and Technology 48 2008
Oil (100g) was heated to 55˚C. Then, the calculated
amount of strong (45˚Be, 2N NaOH) lye was added to
neutralize the free fatty acids exactly, with constant stirring.
Completion of neutralization reaction was determined by
testing the mixture with phenolphthalein indicator. When the
indicator color of the sample mixture turned to pink,
neutralization was completed. Then NaCl solution was heated
to 90˚C and 20ml of hot NaCl solution was added to the
mixture to ensure adequate salting or graining out of
soapstock. After that the mixture was poured into separating
funnel. Three hours later, the mixture was separated into two
distinct layers. Then the lower layer or soap layer was drain
out. The upper layer or oil layer was washed with hot water.
Washing was carried out until color of phenolphthalein
indicator did not change to pink. After complete washing, the
oil was dried at 100˚C in oven to evaporate the moisture.
Drying and cooling was carried out until the weight of dried
oil remained unchanged.
The neutralized oils were weighed to calculate oil
loss and then their free fatty acid content (FFA) were
determined [8]. The characteristics of crude oil and
neutralized oil were determined by American Society of
Testing and Materials (ASTM) standard methods.
2.2. Bleaching of Neutralized Oil
The neutralized oils were heated to 100˚C and different
amounts of activated charcoal were added. After the mixture
was stirred for 45 minutes, the mixture was cooled to room
temperature and activated charcoal was removed by filtering
with filter paper.
The neutralized oils were also bleached with different
amounts of bentonite and a mixture of activated charcoal and
bentonite (1:1 ratio). Then the process was carried out above
procedure.
The colors of bleached oil samples were determined
by a spectrophotometric method [11]. In this method, optical
densities were measured at the wavelength of 460nm, 550nm,
620nm and 670nm. Then the photometric colors were
calculated by the following equation.
Photometric color = 1.29D460 + 69.7D550 + 41.2D650 –
56.4D670 [4]
2.3. Dehydration of Castor Oil
Bleached oil (50g) and 2% (wt%) of NaHSO4 catalyst were
placed into round bottom flask and the apparatus was set up as
shown in figure (1). The system was heated to 210-220˚C for
dehydration time were taken for 15, 30, 45, 60, 75 minutes.
Dehydration was also carried out under 600-640
mmHg (vacuum) as described in the above process. In this
process, the effect of NaHSO4 catalyst amount on the
properties of dehydrated castor oil was also investigated.
Then, the iodine values of dehydrated castor oil were
determined by ASTM D1541-86 and viscosities were
determined by ASTM D 1545-63 method. The drying time
and set to touch time were also determined by ASTM D 1953-
70 [9].
156
Figure 2.1.Dehydration of Castor Oil
2.4. Preparation of Alkyd Resin
Oil modified alkyd resin was prepared with
dehydrated castor oil, glycerol and phthalic anhydride using
NaOH catalyst. The preparation was done in a 4-neck round
bottom flask fitted with a motorized stirrer, a nitrogen inlet, a
thermometer pocked and a hold for sampling. The system was
shown in Fig. 2. In the preparation of alkyd resin, two stages
were involved. The first stage was alcoholysis stage and the
second stage was esterification stage.
Raw material Weight (g) Weight (%)
Dehydrate castor oil 114.27 60.437
(DCO)
Phthalic anhydride (PA) 43.364 22.935
Glycerol (G) 31.44 16.63
Total 189.074 100
Stage 1 (alcoholysis): In this stage, monoglyceride was first
prepared by reacting the oil with glycerol. Alcoholysis of oil
was carried out with different percentages of (0.03%, 0.05%,
0.1%) (by weight) PbO catalyst and (0.1%, 0.2%, 0.3%)(by
weight) NaOH catalysts.
In alcoholysis reaction, the oil was heated with
agitation speed of (700 rpm) and N2 sparging rate of about
(0.06ft3/sec) to 230-240˚C. Glycerol and selected catalyst was
added and alcoholysis reaction was carried out at 230-240˚C.
The reaction was continued until a sample of the reaction
mixture became soluble in two to four volumes of anhydrous
methanol. After alcoholysis reaction was completed, the
reaction mixture was cooled to 140˚C.
Stage 2 (esterification): In this stage, phthalic anhydride was
added to the monoglyceride mixture. The temperature was
maintained at the range of 230-240˚C and maintained at this
temperature. The sparging rate of N2 was increased to
(0.1ft3/sec). The reaction was monitored by periodic
determination of the acid value of the mixture until acid value
dropped to nearly 5.
The acid value of alkyd resin was determined by ASTM D
1639-90 and the chemical resistances also determined. The
prepared resin was standardized by FTIR [12, 13].
Fig.3.3.Alkyd Resin Preparation
 World Academy of Science, Engineering and Technology 48 2008

Bleaching time = 45 minutes

3. Results and Discussion *Photometric color = 1.29D460 + 69.7D620 + 41.2D650 í
3.1. Results Sample Bleaching (wt%) of Photometric Wt. of
3.1.1. Characterization of Crude Castor Oil no. agents bleachin color Refined oil
The characteristics of crude castor oil are shown in g agent number (g)
Table 3.1. A1 Activated 3 7.25 57.437
Table 3.1. The Characteristics of Crude Castor Oil A2 charcoal 5 6.35 57.400
Characteristics Crude castor oil A3 (A) 7 7.16 57.36
Free fatty acid value 19 A4 9 8.32 57.254
A5 11 9.29 57.217
Color, photometric - B1 Bentonite 3 3.80 58.118
Refractive index - B2 (B) 5 3.40 57.386
B3 7 4.40 57.380
Specific gravity 0.9633 B4 9 4.47 57.311
Viscosity(Stroke) 4.5 C1 Activated 3 4.0 57.405
C2 charcoal 5 3.0 57.342
Iodine value, wiji’s 89.5
C3 and 7 4.46 57.254
bentonite
3.1.2. Neutralization of Crude Castor Oil (1:1 ratio)
Table 3.2 show the FFA content of neutralized oil. (C)
Initial weight of crude castor oil = 100g 56.4D670 [4].
FFA (%) of crude oil = 19%
Neutralization temperature = 55˚C 3.1.5. Dehydration of Refined Castor Oil
20% NaCL solution = 40ml Table 3.5 present the yield of dehydrated castor oil at
Sr. 2N Neutralization FFA (%) Weight of different dehydration conditions. The changes of iodine value
no NaOH time(minutes) of Neutralized and viscosity by dehydration of castor oil at different
Neutralized oil (g) dehydration conditions are shown in Fig. 3.1 and Fig. 3.2.
oil
1 15.2 5 8.448 65.09 Table 3.5. Yield of Dehydrated Castor Oil at Different
2 30 10 0.987 60.43 Dehydration Conditions
Initial weight of sample C2 = 50g
3 30 10 0.988 51.79

4.1.3. Characterization of Refined Castor Oil

The characteristics of refined castor are described in
Table 3.3 by comparing with ASTM standard castor oil.
Table 3.3.Characteristics of Refined Castor Oil
Characteristics Refined Castor oil
castor oil (ASTM D 960-79)
Free fatty acid value 1 1.00
Color, photometric 8 -
Refractive index 1.474 1.476 to 1.4778
Specific gravity 0.9614 0.957 to 0.961
Viscosity(Stroke) 4 6.3 to 8.9
Iodine value, wiji’s 90 83 to 88
Source [6]
3.1.4. Bleaching of Neutralized Castor Oil
Effect of bleaching on color and yield of neutralized castor
oil is shown in Table 3.4. Oil was bleached with 0-11% of
activated carbon, 0-9% of bentonite and 0-7% of 1:1 mixture
of activated charcoal and bentonite
Table 3.4. Effect of Bleaching On Color and Yield of
Neutralized Castor Oil
Initial weight of neutralized oil = 100 g
Bleaching temperature = 100˚C

157
 World Academy of Science, Engineering and Technology 48 2008

NaHSO4 V.P Dehydration time (minutes)/Yield (%)

catalyst (mm
(%) Hg)
15 30 45 60 75
um
) 2 760 0.5 90.37 89.88 89.56 89.55
cu
, va
m Hg
140 0m 2 600- 90.9 90.11 89.5 89.13 89.06
-6 4
(60
0
u m) 640 5
acu
135 O
HS
4
,v
Na Hg
130 2% 0 mm 1 600- 90.2 90.035 89.67 89.39 89.28
0 -6 4
125 (60
SO 4
640
Iodine Value

H
Na
120 1%

115
1
110 ho ut vac
uu m) dehydration with 1% NaHSO4 catalyst for 60 minutes
S O 4(w it 2
2 % N aH dehydration with 2% NaHSO4 catalyst for 45 minutes
105

100
3.1.7. Preparation of Alkyd Resin
Reaction condition of alcoholysis reaction condition
10 20 30 40 50 60 70 80
Dehydration Time(min) in alkyd resin preparation is described in Table 3.7. Fig. 3.3
shows the acid value control of esterification reaction. Yield
of dehydrated castor oil-modified alkyd resin and the
Fig. 3.1.Change of Iodine Value with Reaction Time calculation for percentage of reaction complection are
for Dehydration Temperature at 210-220˚C presented in Table 3.8. The appearances of gel type resin,
dehydrated castor oil-modified alkyd resin are shown in Fig.
3.4.
Table 3.7. 1st Stage Alcoholysis Reaction Conditions
Reaction temperature = 230-240˚C
2%
Na
Agitation speed = 500 rpm
= 0.06 ft3/minutes
4 .6
4 .4
HS
O 4 (w
it h
N2 sparging rate
4 .2 ou
4 .0
tv
ac
uu
Alcoholysi Catalyst Reaction Completion of
3 .8 m
3 .6
) s catalysts % (wt%) time (hr) alcoholysis
Viscosity(Stroke)

3 .4
3 .2
2%
N
reaction*
3 .0 aH 1%
2 .8
SO
4 (6
00
Na
HS
PbO 0.03 4 Not complete
-6 O (6
2 .6
2 .4
40
m
4
00
-6
40
0.05 4 Not complete
m m
2 .2
2 .0
Hg
,v
m
Hg
,v
0.1 4 Not complete
a cu ac
1 .8
1 .6
um
)
uu
m
)
NaOH 0.1 4 Not complete
1 .4
10 20 30 40 50 60 70 80 0.2 4 Not complete
D e h y d r a t io n T im e ( m in )
0.3 2 complete
*It was determined by testing the solubility of alcoholysis
Fig.3.2. Change of Viscosity with Reaction Time mixture in anhydrous methanol.
for Dehydration Temperature at 210-220˚C

4.1.6. Characterization of Dehydrated Castor Oils

100
The characteristics of typical dehydrated castor were
presented in Table 3.6 by comparing with ASTM standard
acid value

dehydrated castor oil.

10
Table 3.6.Characteristics of Typical Dehydrated Castor Oils
Vacuum pressure = 600-640 mmHg
Characteristics Dehydrated Dehydrated Standard 1
castor oil1 castor oil 2 dehydrated 30 60 90 120 150
castor oil
(ASTM reaction time (minutes)
D961-86)
Iodine value 140.01 139.05 125-145 Fig.3.3. Acid Value Control of Esterification Reaction
Viscosity 1.600 1.686 1.5-1.8
Table 3.8. Yield of Dehydrated Castor Oil-Modified Alkyd
(Stroke)
Resin
Set to touch 4 3.5 2.5,approxi
time (hour) mately
Drying time 5 5 -
(hour)

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 World Academy of Science, Engineering and Technology 48 2008

I.W-initial weight DCO I..W(g) F.W Y IAV FAV P

F.W-final weight alkyd (g) (%) (%)
Y-yield resin
IAV-initial acid value (100% 6.6 97.72
FVA-final acid value solid) 189.58 140 73.85 298.58
P-degree of reaction complection 2 8
5
1125.26 1150-1060

O=C-O-C-
3.1.8. Characterization of Alkyd Resin
The physico-chemical properties of alkyd resin are
presented in Table 3.9. The chemical resistances of alkyd resin
film are shown in Table 3.10. Table 3.11 show FTIR
absorption band of dehydrated castor oil-modified alkyd resin. 3.2. Discussion
3.2.1. Discussion on Characteristics of Crude Castor Oil
Table 3.9. Characteristics of Dehydrated Castor Oil-modified According to Table 4.1 FFA content of crude castor oil
Alkyd Resin was high and it was not within the ASTM specification limit.
Properties DCO RSO alkyd DCO The color and refractive index of crude oil can not be
alkyd resin* alkyd determined because the transparency of crude oil was very
resin resinŠ poor. The viscosity of crude oil was slightly lower than that of
Acid value 6.6 12.7 4-11 ASTM standard oil [6]. Even though, the specific gravity and
Iodine 80.24 66.3 - iodine value of crude oil were in the range of ASTM
value specification limit, the FFA content of crude oil was differed
Color Yellow Brown - from ASTM standard. The only reason to reduce the FFA
Refractive 1.477 1.5050 - content of oil was to neutralize the crude oil.
index
Gouge HB HB - 4.2.2. Discussion on Neutralization of Crude Castor Oil
hardness In neutralization process, it was found that 30 ml of 2
Scratch F H - N NaOH per 100g of oil was required to obtain neutralized oil
hardness with an acceptable FFA content and to be a minimum of oil
RSO- rubber seed oil loss. The neutralization time of 10 minutes was sufficient to
Source [1, 14] reduce FFA content from 19% to 1%. In neutralization of oil,
free fatty acid content of oil was converted in oil soluble
Table 3.10. Chemical Resistances of Alkyd Resin Films soaps. Small amount of impurities such as phosphotides,
Media Immersion Appearance of proteins or protein fragments, and gummy or mucilaginous
time (hours) film* substances were also removed by neutralization process.
Therefore, the initial weight of oil was decreased as well as
Distilled water 18 Not effect
the yield of oil was decreased. In neutralization process, there
8 Whitening
was a difficulty to separate the soap and oil layer because FFA
3 N NaOH 16 Blistering
content in crude oil was very high. The two layers can be
24 Removal
easily separated when NaCL solution was added to the
*It was examined after the films were air dried for 30 minutes. neutralized mixture because NaCL can help to ensure
adequate salting or graining out of the soapstock. Other
Table 3.11. FTIR Absorption Band of Dehydrated Castor Oil- impurities in oil were removed by washing with hot water. In
Modified Alkyd Resin washing step, there has a little loss of oil. So, the average
Band Experimental Literature Remark yield of oil was 64%.
No. frequency frequency
(cm-1) (cm-1) 3.2.3. Discussion on Characteristic of Neutralized Castor Oil
1 3008.99 Near 3030 =C-H From Table 3.3., it can be seen that the neutralization
2926.74 process can reduce the FFA content of crude oil from 19% to
2 3514.21 3570-3200 O-H 1%. Then, it can give the refined oil color of 8 and refractive
1169.21 Near 1100 O-H index of 1.474. Therefore, neutralization process can offer
3 2855.67 2926-2850 C-H great effect on FFA content, color and refractive index of oil.
1460.43 1485-1440 CH2 Moreover, the refined oil has specific gravity of 0.9614,
4 1738.64 1750-1735 CH3COOCH3 viscosity of 4 and iodine value of 90. These results were
nearly the same as that of the crude oil. Although the
1730.30 1730-1717 COO
neutralization technique reduced significantly FFA content in

159
 World Academy of Science, Engineering and Technology 48 2008
oil, it gave slightly effect on specific gravity, viscosity and
iodine value of oil.
3.2.4. Discussion on bleaching of neutralized oil
In Table 3.4, it can be seen that the highest color removal
efficiency was obtained by bleaching with 5% of bleaching
agents. 5% of activated carbon, 5% of bentonite and 5% of
(1:1) mixture of activated charcoal and bentonite can give the
oil with photometric color of 6.35, 3.4 and 3.0 respectively.
Bleaching with (1:1) mixture of activated charcoal and
bentonite can offer better result. So, it can be chosen as
bleaching agents in bleaching of neutralized oil.
Beside decoloring, bleaching of neutralized oil served the
important function of largely removal of trace amount of soap.
After bleaching process, the average oil yield was 69%. The
oil yield was decreased during the bleaching process due to
the adsorption of oil on the surface of adsorbents and the
filtration of oil with filter paper.
4.2.5. Discussion on Dehydration of Castor Oil
According to the Table 3.5, the yield of dehydrated
castor oil decreased with increasing the dehydration time.
Then, there was a slightly different in yield of dehydrated
castor oil although the dehydration process was carried out
different dehydration conditions.
In Fig. 3.1 and 3.2, it was observed that the
dehydrated castor oil with a maximum iodine value and a
minimum viscosity could be obtained at the proper reaction
time. The iodine values of dehydrated castor oil increased
with the reaction time and reached a maximum value. Then, it
decreased because prolong heating leads to polymerization
with a consequence drop in iodine value and a step rise in
viscosity. The minimum viscosity occurs at or near the point
of maximum iodine value.
From Fig. 3.1, the dehydration of oil without vacuum
system could not give acceptable iodine value to qualify as
drying oil because the iodine value of oil was below 125 (the
lower limit of ASTM dehydrated castor oil) . In this process, a
lot of fumes were evolved during dehydration of oil and these
fumes were condensed and dripped back into the dehydrated
oil. It was undesirable effect. Therefore, it is required to use a
current of inert gas such as carbon dioxide or nitrogen in order
to remove the decomposition products. The most effective
way of removing of fume is by using the vacuum pressure. By
this means, the problem of condensing the fume into the
dehydrated oil was largely avoided. Therefore, dehydration of
refined castor oil was carried out under vacuum system.
When dehydration of oil was done by using 1% of NaHSO4
catalyst and vacuum pressure of 600-640 mmHg and the
optimum reaction time is 60 minutes, this system could give
dehydrated castor oil with iodine value of 140. When
dehydration of oil was done by using 2% of catalyst and
vacuum pressure of 600-640 mmHg and the optimum reaction
time is 45 minutes, this system could give the dehydrated
castor oil with iodine value of 139.05. Although the
dehydration time was decreased with increasing the amount of
catalyst percent, the refractive index of the dehydrated oil was
increased.
160
4.2.6. Discussion on Characteristics of Dehydrated Castor Oils
The iodine value and viscosity control the extent of reaction
and set to touch time and drying time show the drying
properties of dehydrated castor oil. Table 4.7 described that
the iodine value and viscosity of dehydrated castor oils were
in the limit of ASTM standard dehydrated castor oil. Then the
drying time and set to touch time also gave satisfactory result.
Therefore, these dehydrated castor oils were acceptable to
prepare drying oil-modified alkyd resin.
4.2.7. Discussion on Preparation of Alkyd Resin
According to the literature [3], the alcoholysis
reaction is usually completed within an hr or two hrs after the
batch had reached operating temperature. In Table 4.8, it was
found that the samples of the alcoholysis mixture did not
completely soluble in anhydrous methanol although the
alcoholysis reactions were carried out for 4hr by using
different amount of litharge catalysts (0.03%, 0.05%, 0.1%)
and NaOH catalysts (0.1%, 0.2%). It should not be tried to use
the amount of PbO catalyst more than 0.1% (wt%) because the
preferred PbO catalyst percent for alcoholysis reaction is 0.01-
0.1 in literature. Then, large quantities of catalyst lead to dark
the color of alkyd resin and detract from the water and alkali
resistances of alkyd resin. In alcoholysis of oil with 0.1%
(wt%) and 0.2% (wt%) NaOH catalyst, it cannot also give
complete alcoholysis mixture after reaction was carried out for
2 hrs. The degree of alcoholysis has an important bearing on
the properties of the resulting resin. During the final reaction
with phthalic anhydride, esterification of the free hydroxyl
groups of the monoglyceride must compete with any
unreacted or excess glycerol. The latter reaction leads to
glyceryl phthalate which is insoluble in the oil-acid-glyceryl
phthalate and unreacted glyceride oil. Unless sufficient
monoglyceride is present prior to the addition of the phthalic
anhydride, the reaction product will be unsoluble gel of
glyceryl phthalate suspended in oily mixed glycerides. Such a
product is worthless.
In esterification reaction, it was observed that the
longer the reaction time, the more viscous the mixture is. In
this stage, adequate agitation was necessary for complete
mixing of monoglyceride mixture and phthalic anhydride.
Unless adequate mixing was supplied in this stage, the
unqualify alkyd resin would be resulted. So, the N2 sparging
rate was increased in order to remove liberated reaction
product and to increase the heat and mass transfer of chemical
reaction. In Fig. 3.3, the oil-modified alkyd resin with acid
number of 6.6 was obtained after the esterification reaction
was carried out for 150 minutes. It should not try to proceed
the reaction after the acid number of alkyd resin had dropped
to 6.6 because the reaction was closed to gel point.
In Table 3.8, it was observed that 97.72 % of reaction
was completed when the final acid number of alkyd resin was
6.6. Then, the yield of alkyd resin was 73.87%.
3.2.8. Discussion on Characteristics of Alkyd Resin
In Table 3.9, there is no common standard to compare
alkyds resins. Each alkyd resin has its own properties. The
alkyd resin that has acid number of less than 15 is suitable for
application of paint, according to literature [1, 7, 8]. The
scratch hardness of alkyd resin was F and gouge hardness was
 World Academy of Science, Engineering and Technology 48 2008
HB. The refractive index of alkyd resin was 1.447 and color
was yellow.
4.2.9. Discussion on Chemical Resistance of Alkyd Resin
Film
The resistance of alkyd film was determined in two media,
distilled water and NaOH solution. Table 3.10 described that
there was no effect on alkyd film after immersion in distilled
water for 18 hours. The immersion of alkyd film in water for
18 hours was sufficient time to examine the water resistance.
When the alkyd film was immersed in strong alkali solution,
3N NaOH, the film got whitening after immersion time for 8
hours, blistering after immersion time for 16 hours and
removal after immersion time for 24 hours. So, these results
show that the prepared alkyd resin has high chemical
resistance.
4.2.10. Discussion on FTIR Adsorption of Dehydrated Castor
Oil-Modified Alkyd Resin
The FTIR spectrum of prepared alkyd resin exhibits a
characteristic of straight chain ester band at 1738.64 cm-1 and
aromatic ring ester band at 1730.09 cm-1. The present of O=C-
O-C- also exhibit a characteristic ester band at 1125.26 cm-1.
The appearance of CH2, -CH- confirms the present of methyl
group at 1460.43 cm-1 and 2856.67 cm-1. The adsorption band
at 3008.99 cm-1 is characteristic of alkene carbon (=C-H)
according to literature [12, 13].
4. Conclusion
The characteristics of refined castor oils were found
to be standardized with ASTM standard castor oils and it was
suitable to carry out the next step. The refined castor oil was
done by using NaHSO4 catalyst to carry out the dehydration
process. Dehydration under vacuum pressure system was
effective processing method and this pressure influenced the
quality of dehydrated castor oil. A typical dehydrated castor
oil (iodine value 140, viscosity 1.6 stroke, set to touch time
3.5 hr and drying time 5 day) was prepared with 1% NaHSO4
catalyst under vacuum of 600-640 mmHg at 210-220˚C. In
alcoholysis of oil by using 0.3% (wt%) NaOH catalyst, it gave
complete alcoholohysis mixture to preceed the esterification
reaction after reaction time for 2 hrs. Dehydrated castor oil
has been used in the preparation alkyd resin. Dehydrated
castor oil-modified alkyd resin (acid value 6.6) was prepared
by alcoholysis method from dehydrated castor oil, glycerol
and phthalic anhydride with a help of 0.3% NaOH catalyst.
The physico-chemical properties and high chemical resistance
of alkyd resin film showed that they were promising in
formulating of paint.
Acknowledgements
The financial support of Ministry of Science and
Technology is gratefully acknowledged. The author wishs to
extend her gratitude to Prof. Dr. Mya Mya Oo for stimulating
discussion.
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161
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