Journal of Environmental Chemistry and

Ecotoxicology

Vol. 5(7), pp. 181-189, July, 2013

DOI:10.5897/JECE2013.0275
ISSN 2141-226X 2013 Academic Journals
http://www.academicjournals.org/JECE

Full Length Research Paper

Influence of starch addition on properties of urea

formaldehyde/starch copolymer blends for application
as a binder in the coating industry
S. A. Osemeahon1, O. N. Maitera1, A. J. Hotton2 and B. J. Dimas1*
1

Department of Chemistry, Modibbo Adama University of Technology, Yola, Nigeria.

National Agency for Food and Drug Administration and Control (NAFDAC) Jalingo, Nigeria.

Accepted 2 July, 2013

Urea formaldehyde resin was reactively blended with various concentrations (10 to 70%) of cassava
starch in order to develop a paint binder for emulsion paint formulation. Some physical properties and
formaldehyde emission of the blended resin were investigated. Viscosity initially decreased before a
gradual increase was noted with increase in starch concentration. Refractive index and elongation at
break increased initially but gradually decreased with cassava starch content in the blend. Gel time,
density, melting point, moisture uptake and formaldehyde emission decreased with increase in starch
inclusion. The interaction between the two different polymers shows that 50% starch was the optimal
loading inclusion. This new system has advantages of low brittleness, low formaldehyde emission and
water reduction characteristics. Therefore the polymer blend can be recommended as binder for
coating industry.
Key words: Urea formaldehyde, starch, copolymer, binder.

INTRODUCTION
The development of reliable high performance coating
materials with excellent thermal and mechanical
properties is the focus of modern technology. Waterborne coatings are finding more application due to
increased legislative restrictions on the emission of
volatile organic materials to the atmosphere (Motawie et
al., 2010). Depending on the type of binder, paints are
classified into 2 main categories; that is, oil paint which is
oil based, and emulsion paint which has synthetic resin
as the binder, and its water soluble as against oil paint
which is solvent (organic solvent) soluble. Although oilbased paints display a lot of advantages such as water
resistance, durability and flexibility, its major drawback is
its use of organic compound as solvent, which is
threatened by growing proliferation of Volatile organic

compounds (VOC) regulations imposed worldwide.

Water-borne resins are polymeric materials whose
composition enables them either to dissolve or to swell in
water. Most buildings are protected and decorated using
water-borne paints due to their ease of applications, fast
drying, non-odour, good wash-ability and finish. However,
although most household paints are water based, this is
not true of industrial paints because of the special
requirement of the industrial coatings. Hence, satisfactory
water based polymers with the required properties have
not yet been developed thus leading to emphasis on
sustainable commercial production of water-borne paints
(Hasmukh and Sumeet, 2010; Motawie et al., 2010;
Osemeahon, 2011). Developing nations however, will
need to put more effort into the development of local

*Corresponding author. E-mail: blesseddimas@yahoo.com.

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J. Environ. Chem. Ecotoxicol.

technologies for the purpose of achieving the above

target. Polymer blends has grown tremendously in leaps
and bonds over the past few decades (Oluranti et al.,
2011).
Blending could be a simple process for
developing new composites for coating systems.
Polymer blend is one of the most useful approaches to
prepare new materials with specially tailored and
improved properties that are often absent in a single
polymer. The performance of a polymeric material can be
improved by selection of suitable ingredients and their
ratios, leading to the formation of a new material with
enhanced physical, chemical and mechanical properties
(Kaniappan and Latha, 2011; Hwang et al., 2012). The
synthesis of a new class of urea formaldehyde (UF) resin
through a one step process was reported by Osemeahon
and Barminas (2007). Although this new class of resin
showed much improvement in terms of formaldehyde
emission and moisture uptake (water resistant),
compared with the traditional urea formaldehyde (UF)
resin, its brittleness and hardness remains a source of
concern (Osemeahon and Archibong, 2011). Hence the
need to modify this new class of urea formaldehyde (UF)
resin in order to address the problem of brittleness and
further reduce both formaldehyde emission and moisture
uptake.
This work seeks solution to the problem, by the
copolymerization
reaction
between
urea
formaldehyde/cassava starch (UF/CS). Starch is one of
the most abundant natural polymers, used in a wide
range of products including binders, sizing materials,
glues and pastes. Inexpensive materials such as starch,
are biodegradable additives, which are appropriate for
blending with synthetic polymers (Amine et al., 2010;
Borghei et al., 2010). The cassava starch has a high
purity level, excellent thickening characteristics, a neutral
(bland) taste, desirable textural characteristics, relative
cheapness and contains a high concentration of starch
(dry-matter basis) which is an advantage over other
grains or root crop. Its high paste viscosity, clarity, freezethaw stability and renewability are advantageous to many
industries.
The Nigeria government cassava project is aimed at
increasing the utilization of cassava for industrial
purposes, which is why recently, many research has
focus on conversion of cassava into industrial products
and raw materials (Akpa, 2012).
MATERIALS AND METHODS
Urea formaldehyde, sodium di-hydrogen phosphate, sulphuric acid,
sodium hydroxide pellets, sucrose, were reagent grade products
from the British Drug House (BDH). The materials were used as
received. Cassava tubers were collected from a farm in Yola,
Nigeria.

Treatment/preparation of starch
The cassava tubers were washed, dried and grounded into

powder. It was treated by dispensing in cold water and filtering. The

filtrate was heated using hot plate with occasional stirring of 5 min
intervals, until colloidal suspension was observed which formed a
gel on cooling. The method used for the resin synthesis, blend/film
preparation and determination of the film properties was according
to Osemeahon and Archibong (2011).

Resin synthesis
Urea formaldehyde (UF) resin was prepared by reacting one mole
(6.0 g) of urea with three moles (24.3 ml) of 37% (w/v)
formaldehyde using 0.2 g of sodium dihydrogen phosphate as
catalyst. The pH of the solution was adjusted to 6, using 0.5 m
H2SO4 and 1.0 m NaOH solution. The reaction was then allowed to
proceed for 2 h in a thermostatically control water bath at 70C,
after which the sample was removed and kept at room temperature
(30C).

Blend/film preparation
Blending of urea formaldehyde resin with cassava starch was
carried out by preparing 10% cassava starch in urea formaldehyde
at room temperature (30C). The solution was mixed thoroughly
using a magnetic stirrer. The above procedure was repeated at
different cassava starch concentrations (10, 20, 30, 40, 50 and
70%) respectively and the resulting blends analyzed. Copolymer of
the different resins obtained with various cassava starch
concentrations were introduced into a glass Petri dish for casting.
The resins were then allowed to cure and set for seven days at
30C and the physical properties of these copolymers were
carefully investigated.

Determination of viscosity and gel time

A 100 ml Phywe made graduated glass macro-syringe (Phywem,
Gottingen, Germany) was utilized for the measurement. The
apparatus was standardized with a 20% (w/v) sucrose solution
whose viscosity is 2.0 mPa.s at 30C. The viscosity of the resin was
evaluated in relation to that of the standard sucrose solution at
30C. Five different readings were taken for each sample and the
average value calculated.The gel point of the resin was determined
by monitoring the viscosity of the resin with time until a constant
viscosity profile was obtained.

Determination of density, melting point and refractive index

The density of the different resins was determined by taking the
weight of a known volume of resin inside a density bottle using
Mettler Model, AT400 (GmbH, Greifensee, Switzerland) weighing
balance. Five readings were taken for each sample and average
value calculated. The turbidity of the resin samples was determined
using Hanna microprocessor turbidity meter Model, H193703
(Villafranca Padovana, Italy). The melting points of the different film
samples were determined using Galenkamp Melting apparatus
Model, MFB600-010F (Loughborough, UK). Different copolymer
samples were grounded into powder and some quantity of each
sample was introduced into different capillary tubes. The melting
point was then taken one after the other for all samples. The
refractive indices of the resin samples were determined with Abbe
refractometer (Bellinglam and Stanley, Tunbridge Wells, Kent, UK).
Five readings were taken for each sample and the average value
calculated for each of the aforementioned parameters. The
properties of the blends were also determined according to
standard methods (AOAC, 2000).

Osemeahon et al.

183

60

Viscosity (Sec)

50
40
30
20
10
0
0

10

20

30

40

50

60

70

80

Cassava Starch Concentration (%)

Cassava Starch Concentration (%)

Figure 1. Effect of cassava starch concentration on viscosity of methylol urea resin.

Determination of moisture uptake

The moisture uptake of the resin film was determined
gravimetrically as known weights of the sample were introduced
into desiccators containing a saturated solution of sodium chloride.
The increase in weight (wet weight) of each sample was monitored
until a constant weight was obtained. The difference between the
wet weight and dry weight of each sample was then recorded as
the moisture intake by resin. Triplicate determinations were made
for each sample and the average value recorded.

Determination of formaldehyde emission

Formaldehyde emission test was performed by using the standard
2 h desiccators method. The evaluation of the absorbed
formaldehyde by the 25.0 ml water was obtained from standard
calibration curves derived from refractometric technique using Abbe
refractometer. In brief, the prepared resin was aged for 2 days. At
the end of this period, the resin was poured into a mold made from
aluminium foil with a dimension of 69.6 126.5 mm and thickness
of 1.2 mm. The mold and its content was then allowed to
equilibrate for 24 h in the laboratory after which it was then placed
inside a desiccator along with 25 ml of water, which absorbed the
formaldehyde emitted. The set up was allowed to stay for 2 h after
which the 25 ml water was removed and analyzed for formaldehyde
content. Triplicate determinations were made for each sample and
mean value recorded.

Elongation at break
Elongation at break was measured, using Inston testing machine
(model 1026). Resin films of known dimension 50 mm long, 10 mm
wide and 0.15 mm thick were brought to rapture at a clamp rate of
20 mm/min and a full load of 20 kg. A number of five runs were
done for the sample and the average elongation evaluated and
expressed as the percentage increased in length.

RESULTS AND DISCUSSION

Viscosity and gel point
The viscosity of a substance (liquid, gas or fluid) is its

resistance to flow. Studying rheological properties of

fluids and gels are very important, since operation
processes design depends on the way the product flows
through a pipe, stirring in a mixer and packaging into
containers. Emulsion lattices has many sensory attributes
which are related to their rheological properties,
examples are creaminess, thickness, smoothness,
spread- ability, flow -ability, brittleness and hardness
(Hussain and Nasr, 2010; Akpa, 2012).
Because of the presence of functional groups in the
polymeric backbone, inter-polymeric specific interactions
have long been known to result in unusual behavior and
material properties that are dramatically different from
those of the nonfunctional polymers. These interactions
include ion-ion Coulombic interaction, hydrogen bonding
and transition metal complexation of the component
polymer chains, resulting in solution viscosity variation.
Rheological properties such as the viscosity can be
directly correlated to the evolving physical and
mechanical properties during resin cure (Derkyi et al.,
2008; Osemeahon, 2011). The effect of cassava starch
on the viscosity of urea formaldehyde resin is observed
(Figure 1). At low concentration of 10% cassava, the
viscosity decreased slightly and then increased with
increase in cassava starch concentration. This
phenomenon can be explained in terms of specific
interactions between urea formaldehyde and cassava
starch.
In a dilute system, there are strong specific interactions
and the complexes are isolated from each other with the
formation of compact structure, which reduced the
viscosity of the blend solution. However, as the blend
concentration increases, the isolated complexes
combined, lead to the formation of a gel-like
intermolecular complex structure leading to increase in
viscosity of the copolymer blend system, since the
variation is linear, it indicates the miscibility of polymer
blend (Osemeahon and Barminas, 2007; Reddy et al.,
2008).

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J. Environ. Chem. Ecotoxicol.

450

(h)
time
Gel
(hr)
Time
Gel

400
350
300
250
200
150
100
50
0
0

10

20

30

40

50

60

70

80

Cassava Starch Concentration (%)

Figure 2. Effect of cassava starch concentration on gel time of methylol urea resin.

Viscosity also increases with increase in solid content

as a consequence of higher surface interactions among
the particles. Concentrated polymer shows a great deal
of interaction between the macromolecule. The higher the
concentration, the higher the viscosity observed (Palma,
2007; Taghizadeh and Toroutan, 2005). The gel time or
pot life is the maximum length of time the system remains
in sufficiently fluid condition to be applied to a substrate.
The dry time of any paint is a function of its binders gel
time among other factors. On the technical front, gel time
enable paint formulator to ascertain the optimum storage
period of a binder before its utilization for Paint
formulation. The gel time is an important kinetic
characteristic of curing because it describes the
attainment of certain critical conversion responsible for
the transition from liquid to solid state of the curing
process. The gel point is characterized by the
appearance in the reactive system of macromolecule with
an infinitely large molecular weight (Desai et al., 2003;
Derkyi et al., 2008). Figure 2 shows the effect of cassava
starch concentration on gel time. It can be observed that
the gel time decreases with increase in cassava starch
concentration. The reaction between monomers leads to
the formation of network, hence gelation. Both molecular
weight and poly-dispersity increase until one single
macromolecule is formed. At this point, the behavior of
the system changes from liquid-like to rubber- like thus
the reactive system becomes a gel (Gonzalez et al.,
2012).
Density
Density is a physical property of matter that expresses a
ratio of mass to volume. It is very useful for identification
and characterization of substances. The density of a

paint binder in the coating industry has a profound

influence on factors such as pigment dispersion, brushability of paint, flow, leveling and sagging (Kazys and
Rekuviene, 2011; Osemeahon and Archibong, 2011).
Figure 3 shows the effect of cassava starch on the
density of urea formaldehyde resin. The gradual
decrease observed in density with increase in cassava
starch concentration can be as a result of differences in
the molecular features and morphology which influenced
the packing nature of resin molecules as the
concentration of starch increases (Osemeahon and
Barminas, 2007). This result is similar to the findings of
Barminas and Osemeahon, 2007 when natural rubber
was blended with methylol urea resin.
Melting point
The melting point of a polymer has a direct bearing on its
thermal property. Melting point of polymer varies
depending on molar mass, intermolecular van der Waal
interactions and intrinsic structures that affect the rigidity.
In the case of coating industries, the melting point of a
binder is related to its thermal resistance as well as to the
brittlity. Urea formaldehyde resin is known to compose of
molecules that cross-link into clear hard plastics (Afsoon
et al., 2011; Osemeahon et al., 2010). Figure 4 shows the
effect of cassava starch on the melting point of methylol
urea resin where the melting point decreased slightly at
the beginning up to 10% cassava starch. Thereafter, a
sharp decrease in melting point was observed. The
melting points of the two monomers are very different
which probably result from different contributing factors.
At a certain domain of concentrations of the two
copolymers, their melting point decreased even below the
melting point of each monomer. The melting point of the

Osemeahon et al.

185

1.17
1.16
(h)3 )
Gel Time
(m/cm
Density

1.15
1.14

1.13
1.12
1.11
1.1
1.09
0

10

20

30

40

50

60

70

80

Concentration (%)
CassavaCassava
StarchStarch
Concentration
(%)
Figure 3. Effect of cassava starch concentration on the density of methylol urea resin.

Melting Point oC

Melting Point (C)

300
250
200
150
100
50
0
0

10

20

30

40

50

60

70

80

Cassava Starch Concentration (%)

Figure 4. Effect of cassava starch on the melting point of methylol urea resin.

blended films shifted due to interaction of the two

biopolymers as influenced by the lower melting
temperature of cassava starch (Afsoon et al., 2011;
Wirongong et al., 2011). This decrease in melting point is
due to increase in molecular mobility which is a positive
result.
Refractive index
Gloss is a measure of the ability of the coated surface to
reflect light. Reflection of light from surfaces can be
classified according to the diffuse component or the
specular component, which is expressed as a function of

the incidence angle and refractive index of the material,

the surface roughness and a geometrical shadowing
function. Gloss is a necessary coating property when the
purpose is for surface aesthetics or decoration (Kaygin
and Akgun, 2009; Yumiko et al., 2010). Figure 5 presents
the effect of cassava starch on the refractive index of
urea formaldehyde resin. Initially, the refractive index
increased from 0 to 20% cassava starch inclusion after
which a gradual decrease in refractive was observed with
increase in cassava starch concentration. This result is
due to differences in the level of specific interaction
between the two polymers resulting in molecular weight,
molecular features and molecular orientations depending
on morphology and crosslink density (Qi et al., 2002).

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J. Environ. Chem. Ecotoxicol.

1.43
Refractive Index

Refractive Index

1.42

1.41
1.4
1.39
1.38
1.37
1.36
0

10

20

30

40

50

60

70

80

Cassava Starch Concentration (%)

Figure 5. Effect on cassava starch concentration on the refractive index of methylol urea.

Moisture Uptake (g)

Moisture Uptake (%)

3.5
3

2.5
2
1.5
1
0.5
0
0

10

20

30

40

50

60

70

80

Cassava Starch Concentration (%)

Figure 6. Effect of cassava starch on the moisture uptake of methylol urea resin.

This suggests that from 0 to 20% cassava starch

inclusion in the gloss property especially on a smooth
surface increases after which a decrease is observed.
Moisture uptake
Polymeric binders play a major role in moisture transport
properties of paint because it is one of the major
constituent. Susceptibility to durability issues pertaining
poor water resistance is one of the draw-backs of waterborne resin. The functional groups on polymers that are
used can undergo hydrogen bonding. A detailed
knowledge of moisture transport is essential for
understanding the resistance of a material against

attacks from its environment (Emile, 2003; Bharath and

Swamy, 2009).
Figure 6 shows the effect of cassava starch on the
moisture uptake of methylol urea resin. It can be
observed that moisture uptake drastically dropped at the
beginning and decreased steadily after 10% blend until
after 40% blend. The different levels of interactions gave
rise to polymers with different morphology and crosslink
density. From 0 to 10% blend, the molecular size holes in
the copolymer structure were rapidly reduced. After this
period, the size of the molecular size holes might have
slowly decreased with increase in cassava starch
loading; hence the steady reduction in moisture uptake.
After the steady decrease in moisture uptake between 10
to 40% blend, a sharp decrease in moisture uptake was

Osemeahon et al.

187

(ppm)
Formaldehyde Emission
Emission
Formaldehyde

0.06
0.05
0.04
0.03
0.02
0.01
0
0

10

20

30

40

50

60

70

80

Cassava Starch Concentration (%)

Figure 7. Effect of cassava starch on the formaldehyde emission of methylol urea resin.

noted. This might be as a result of the drastic decrease in

molecular size hole with increase in cassava starch
inclusion. Blending improves the resistance to moisture
susceptibility of mixtures as also seen in waste plastic
coating of aggregates (Bindu and Beena, 2010).
Formaldehyde emission
A serious drawback of urea formaldehyde resin is the
emission of the hazardous formaldehyde during cure.
The issue of formaldehyde exposure in homes is longstanding and has been studied overtime. Hydrolysis of
cured urea resins has been known to be responsible for
formaldehyde emission leading to sick building
syndrome. It is therefore important to determine the
formaldehyde emission from synthesized ureaformaldehyde resin (Derkyi et al., 2008; Park et al.,
2010). It is observed in Figure 7 that the level of emission
decreased with increase in the concentration of cassava
starch in the blend. This important promising trend is due
to the gradual decrease in the methylol urea content with
increase in the cassava starch content in the blend. The
blending process has succeeded in reducing the
emission lower than the permissible level of 0.1 ppm as
stated by Pizza et al. (2002). This agrees with the
findings of the copolymerization of urea formaldehyde
with acrylamide (Abdullah et al., 2010).
Elongation at break
The structure of thermosetting resins also leads to some
unwanted mechanical properties that limit their structural
applications. They are relatively brittle. Elongation at
break can be a propel tool to determine the adhesion

between phases because of its sensitivity for load

transfer between phases (Cakir et al., 2012; Hwang et al.,
2012).
Figure 8 shows the effect of cassava starch on the
elongation at break of methylol urea resin. A steady
increase in elongation at break was observed from 0 to
40% cassava starch and an abrupt increase at 50% due
to compatibilization effect and improved interfacial
adhesion, hence flexibility is improved and brittleness
reduced. Also, a decrease was observed after 50%. This
non-linear behavior in terms of the mechanical property is
caused by the difference in intimate physical interlocking,
and the extent of phase separation (Hwang et al., 2012).
The result is in consonance with the report of Cardona
and Moscou (2010) where resole phenolic resins were
modified by forming copolymer with cardanol (main
component of cashew nut shell liquid), the presence of
cardinol decreases the crosslink density and makes the
resole phenolic resins less brittle. Table 1 shows the
comparison of some physical properties of UF and
UF/CS resins.
Conclusion
The analyzed results obtained from the sample analysis
showed that the interaction between methylol urea and
cassava starch has remarkable synergistic properties
with 50% of cassava starch being the optimal inclusion
value. The values of moisture uptakes, formaldehyde
emission and melting point obtained from this experiment
are within the acceptable levels required in the coating
industry as shown in Table 1.
This results present cassava starch modified methylol
urea as a resin with relatively very low moisture uptake
and formaldehyde emission against the traditional hard

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J. Environ. Chem. Ecotoxicol.

(%)
Break
Elongation
Break
Elongationatat

1.8
1.6
1.4
1.2
1
0.8
0.6
0.4
0.2
0
0

10

20

30

40

50

60

70

80

Cassava Starch Concentration (%)

Cassava Starch Concengtration (%)

Figure 8. Effect of cassava starch on the elongation at break of methylol urea resin.

Table 1. Comparison of some physical properties of UF and UF/CS resins.

Parameter
Density (g/cm)
Refractive index
Formaldehyde emission (ppm)
Moisture uptake (%)
Viscosity (mpa.s)
Elongation at break (%)
Melting point ( C)

UF

UF/CS

1.168
1.410
0.0500
3.3000
3.1111
40
250.00

1.166 0.001
1.417 0.1000
0.0040 0.002
0. 6000 0.001
11.1000 0.1100
160.00 0.01
130.00 0.10

and brittle resin. The increase in elongation at break and

reduction in density is also a positive value to the coating
industry. Therefore, this work has shown that
biodegradable starch films could be used to produce
copolymer composite binder for the coating industry
especially in the formulation of emulsion paints.
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