Optimal prediction of PKS: RSO modified

alkyd resin polycondensation process using

discrete-delayed observations, ANN and
RSM-GA techniques

Chigozie F. Uzoh & Okechukwu

D. Onukwuli

Journal of Coatings Technology and

Research

ISSN 1547-0091

J Coat Technol Res

DOI 10.1007/s11998-016-9881-6

1 23
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1 23
 Author's personal copy
J. Coat. Technol. Res.
DOI 10.1007/s11998-016-9881-6
Optimal prediction of PKS: RSO modified alkyd resin
polycondensation process using discrete-delayed observations,
ANN and RSM-GA techniques
Chigozie F. Uzoh, Okechukwu D. Onukwuli
 American Coatings Association 2017
Abstract Alkyd resins are widely used in the paint
industry and although they have a long history about
70–100 years, today the developments in alkyds are
still welcome and innovations are still needed. Artifi-
cial neural network (ANN) and response surface
methodology based on a 251 fractional factorial design
were used as tools for simulation and optimization of
the polycondensation process for autooxidative drying
alkyd resin from palm kernel stearin: rubber seed oil
blend of 70:30 ratio. A feed forward neural network
model with Levenberg–Marquardt back propagation
training algorithm was adapted to predict the responses
(conversion Y1, viscosity Y2, and molecular weight
average Y3). The studied input variables were reaction
time, temperature, catalyst concentration, oil ratio, and
stirring rate. The performance of the RSM and ANN
model showed adequate prediction of the responses in
terms of the process factors, with MRPD of ±4.47%
(Y1), ±2.08% (Y2), ±8.92% (Y3) and ±6.50% (Y1),
±3.31% (Y2), ±10.20% (Y3), respectively. The sensi-
tivity analysis showed that while reaction time is the
most effective process parameter, the interaction of the
five process variables produced the most significant
effect on the studied responses with the overall
minimum MSE of 0.079. The optimization task per-
formed using a genetic algorithm linked to the RSM
model gave a viable, nondominated optimal response
and optimum operating conditions regarding the route
to high-quality resin at reduced material and opera-
tional costs. Overall, coupled RSM-GA was found to
be a better tool for modeling and optimization of the
alkyd resin production.
Keywords Multivariate system, Response surface
C. F. Uzoh (&), O. D. Onukwuli
Chemical Engineering Department, Faculty of Engineering,
Nnamdi Azikiwe University, Awka, Nigeria
e-mail: cf.uzoh@unizik.edu.ng
methods, Genetic algorithm, Artificial neural network,
Alkyd resin
Introduction
Alkyd resins are polyester polymers of fatty acids which,
when spread over a surface in a thin coat, form a solid,
cohesive, and adherent film. They are the polymer-
binding materials in paints responsible for the formation
of continuous film that adheres to the substrate and
holds the other substances together.1 The global paints
and coatings market was worth USD 121.9 billion in 2013
and is expected to reach an estimated value of USD
176.5 billion by 2020.2 The raw materials, energy and
labor contribute approximately 60% to the final value of
each liter of paint.3 The major hindrances to industrial
alkyd resin production are their relative high solvent
content and economic viability. Therefore, much cur-
rent research interest is geared toward the development
of a new approach that will guarantee the decrease in
alkyd resin production cost.
Vegetable oils, green renewable sources, are common
raw materials in the organic coating industry, especially,
for alkyd resins. About one million tons of vegetable oils
have been used in surface coatings each year.4 Applica-
tion of vegetable oil for production of alkyd resin
requires the use of an alcoholysis-polyesterification
technique along with fusion process. This process may
use waste or by-products of oil plant industries and
consumes lower energy compared to the solvent process
of synthesizing alkyds, which uses expensive oil fatty
acids instead of oils and consumes more energy. More-
over, the solvent process produces environment pollu-
tion due to aromatic solvent entering the air.5
Oil palm (Elaeis guineensis) is native to Africa and
remains a source of the most abundant and widely used
plant oils in the world, grown in mass in tropical
countries. Palm oil and palm kernel oil are edible plant
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J. Coat. Technol. Res.
oils derived from the fruit of trees. It differs from its
major competitors (soybean, sunflower seed, and rape
seed) in that it is obtained from perennial tree crops and
drought impacts are less severe in comparison with oil
seed crops. Palm stearin is the more solid fraction of palm
and palm kernel oils. It has not been commercially
utilized and barely used in most parts of the world. The
fatty acid composition of palm kernel stearin is approx-
imately 60% saturated and 40% unsaturated fatty acid.
The main unsaturated fatty acids compositions of palm
kernel stearin are 33% oleic and 7% linoleic acid.4
Therefore, palm kernel stearin is classified as saturated
fatty acid due to its very low degree of unsaturation and
alkyd resins, which are based on palm kernel stearin
alone, and cannot be air-dried.5 In order to air-dry, palm
kernel stearin-based alkyd resin, an unsaturated C–C
bonds, must be introduced into the main or pendant
chains of the alkyd resin. In a previous work, it was
established that 2/3 of the total palm kernel stearin (PKS)
content is needed with 1/3 of rubber seed oil (RSO) for
autooxidative drying.6 Azimi et al.7,8 investigated the
effect of conventional and nano zinc pigments and
modification with ketone on air-drying properties of
palm stearin-based alkyd resin paints. They reported that
palm stearin can be utilized in the synthesis of alkyd resin.
Uzoh et al.9 synthesized and optimized the polyesterifi-
cation process for palm oil-based alkyd resin using
response methodology. They reported that optimum
fractional conversion of 97.28% was predicted at reaction
temperature of 240.61 8C, reaction time of 150 min,
catalyst concentration of 0.03%, and PA: MGO ratio of
0.38:1, for the process. Due to the stringent industrial
specifications that today’s alkyd resins must meet, the
need for fine-tuning their properties through a more
effective optimization technique is more acute than ever.
For instance, in order to produce alkyd resin offering a
combination of both desired drying time and chemical
and mechanical properties, the molecular weight, viscos-
ity, conversion and some instances, undesirable side
product concentration, must be controlled within limits
that would not damage the industrial or end-use require-
ments. These alkyd resin property variables, in most
instances, are difficult or impossible to measure online,
specifically, viscosity. Thus, it is very difficult to control
the alkyd resin product quality when all that is available is
infrequent and delayed-offline laboratory measurements.
Apart from work presented in reference (9), there is no
reported literature on any alkyd resin system optimiza-
tion in which the response of interest directly relates to
the end-properties using statistical screening paradigm.
Mathematical and statistical techniques such as
response surface methodology (RSM) and artificial
neural network (ANN) can assist in analyzing exper-
imental data, finding optimum situation, and predicting
results. Statistical design, first applied in industry in the
1930s, was promoted by Box and Wilson10 with the
development of the response surface methodology
(RSM). RSM can be defined as a group of mathemat-
ical and statistical techniques used to model and
analyze results/data in which the response/property of
interest is affected by numerous factors, and the aim is
to obtain an optimal response.11 Once a system is fully
characterized, the objective of process design may be
pursued further by formulating a model that may
permit a rough local approximation to the actual
surface. Such predictive models are usually developed
from design of experiment to provide analytical solu-
tion(s) for the desired response, obviating the need for
experimenting in an ad hoc manner in search of
optimal setup. RSM and other designs spread through-
out several industries over the next 30 years. The use
of experimental design was expanded by Taguchi
et al.12–14 However, the Robust Parameter Designs
(RPD) approach initially proposed by Taguchi, caused
a great deal of controversy among statisticians.15 With
the emergence of response surface methodology
(RSM), many efficient approaches which could effec-
tively handle RPD problems are available.
Most of the traditional optimization techniques
based on gradient methods have the possibility of
getting trapped at local optima, depending upon the
degree of nonlinearity and the initial guess. Hence, it
does not ensure the global optimum and also has
limited application. Nontraditional search and opti-
mization methods based on natural phenomena, neural
networks, and evolutionary computation (simulated
annealing, genetic algorithm (GA), and differential
evolution) have been developed to overcome this
problem.16 Artificial neural network (ANN) is a highly
simplified model of the structure of a biological
network.17 The fundamental processing element of
ANN is an artificial neuron (or simply a neuron). A
biological neuron receives inputs from other sources,
combines them, performs generally a nonlinear oper-
ation on the result, and then outputs the final result.18
The basic advantage of ANN is that it does not need
any mathematical model since an ANN learns from
examples and recognizes patterns in a series of input
and output data without any prior assumptions about
their nature and interrelations.17 ANN is a good
alternative to conventional empirical modeling based
on polynomial and linear regressions.19 In recent years,
the genetic algorithms (GA) have been successfully
applied in a variety of fields where optimization in the
presence of complicated objective functions and con-
straints abounds. The reasons for the wide use GAs are
their global search ability and independence of initial
value. Genetic algorithm (GA) is a stochastic general
search method which proceeds in an iterative manner
by generating new populations of individuals from the
old ones. GA uses stochastic operators such as selec-
tion, crossover, and mutation on an initially random
population in order to compute a new population.20
The search feature of the GA is in contrast with those
of the gradient descent and LM in that it is not
trajectory-driven, but population-driven. The GA is
expected to avoid local optima frequently by promot-
ing exploration of the search space, in opposition to the
exploitative trend usually allocated to local search
algorithms like gradient descent or LM.21
 Author's personal copy
The current article deals with the study of ANN and
RSM-GA models for optimization of the alcoholysis-
polyesterification blend of PKS: RSO for alkyd resin
synthesis. A 251 fractional factorial array was used to
generate the data for all the models. The objectives of
the study are: to investigate whether ANN can
adequately predict and simulate those discrete-delayed
measurements/responses which directly affect the end-
use properties (i.e., viscosity, conversion, and molecu-
lar weight average); to compare the performance of the
developed ANN and RSM models as tools for predic-
tion and simulation of the alcoholysis-polyesterification
process; to optimize the responses and conduct sensi-
tivity analysis using RSM-GA and ANN, respectively.
Materials and methods
Materials
The palm kernel stearin was collected from the Upglobal
Agro oil mill, Isiakpu village Nise, Anambra State. The
refined rubber seed oil was purchased from the Rubber
Research Institute of Nigeria, Iyanomon, Benin city, and
was used without further purification. The analytical
grade phthalic anhydrides, maleic anhydride, glycerol,
calcium oxide, sodium bisulfate (NaHSO4), and xylene
were obtained from Eddy Chemical Shop in Onitsha,
and were used without further purification.
Synthesis of alkyd resin from modified palm kernel
stearin
Seventy grams of palm kernel stearin were blended with
30 g of rubber seed oil and labeled as oil. The mixture
was charged into a reactor with 2% sulfuric acid in the
presence of 2% pumice for the dehydration process. It
was heated to 260–298C at a constant reaction time of
20 min in an inert atmosphere of nitrogen. The water
generated from the reaction was collected through a
Dean-Stark apparatus. The iodine value was measured
to determine the unsaturation level of the dehydrated
blended oil. Alkyd resin was prepared with dehydrated
PKS-RSO blend, glycerol, phthalic anhydride, using
lithium hydroxide as catalyst. The reactions were
carried out in a four-necked round-bottom flask titled
with a motorized stirrer, a Dean-Stark trap titled with
water-cooled condenser and nitrogen inlet tube at a
temperature of 220–260C. Xylene was employed as an
azeotropic solvent. During alcoholysis, the triglycerides
of the oil blends were converted to monoglycerides by
reaction with glycerol, catalyzed by lithium hydroxide at
180–200C. Phthalic anhydride, glycerol, and xylene
were then added, and polymerization was carried out at
220–250C for about 6 h as shown in Fig. 1. The
concentrations of the alkyd solutions were determined
and finally diluted to 70–75% by addition of xylene. The
progress of reaction was monitored by measuring the
J. Coat. Technol. Res.
evolved water of reaction and periodically checking the
acid number by titration in accordance to ASTM
D1980-87 (1998) with some modifications.
System prediction via RSM
The RSM study was implemented on model-based
calibration tool (MBC v2.0) found in MATLAB 7.1
tool box. The steps involved are discussed as follows;
Design of experiments (DOE)
System analysis via MBC tool requires initial coding of
the independent variables into the solution algorithm.
This involves using unique notations (or codes), such as
A, B, C…, x1, x2, x3…, to represent the variables, and
specifying the actual range of values of the variables
using a suitable DOE template. In the current study, five
process variables including temperature, time, oil ratio,
catalyst concentration, and stirring rate coded A, B, C, D,
and E, respectively, were considered as major operating
factors affecting reaction progress and product quality in
a typical alkyd polycondensation process. A useful DOE
template which minimizes the required number of
system iterations for full system assessment is the
classical central composite design (CCD). However,
considering the number of independent variables in the
present study, fractional factorial design (251) was
implemented at the factorial levels of a standard CCD
to further reduce the required number of iterations. This
results in a useful experimental design template called
combined array (CA) which is also known to give
reliable results with minimized number of system itera-
tions in studying multivariate systems.22,23 The proposed
CA for the current design problem requires performing
sixteen distinct system iterations at the factorial points,
ten iterations at the axial points, and four iterations at the
center points, giving a total of thirty different iterations
of the system. This step was accomplished for the current
study using the following codes and data ranges:
A:½a; a ! Temperature (C): [230, 270]
B:½a; a ! Time (min): [60, 180]
C:½a; a ! Oil ratio: [0.1, 0.5]
D:½a; a ! Catalyst conc.: [0.02, 0.1]
E:½a; a ! Stirring rate (rpm): [500, 700].
Sensitivity analysis and system prediction via
artificial neural network (ANN) model
Sensitivity analysis was first conducted to determine
the effectiveness of the parameters by the constructed
neural network model. In the analysis, the effects of
different interactions of the variables on the recorded
conversion of acid functional group were studied and
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Total condenser

Automatic
Solvent decanter
return line

Heat-transfer
fluid outlet Water overflow
to receiver

Heat-transfer
fluid inlet

To thin tank
Fig. 1: Alkyd reactor

the results were used as a basis for evaluating the considered appropriate for correlating the experimen-
sensitivity of the neural network model. The perfor- tal data and predicting the general system behavior.
mances of the five interaction groups of (one, two,
three, four, and five) variables were examined using   X
k X k
the LM (Levenberg–Marquardt) algorithm. Artificial Y Xj ; Xj ¼ b0 þ b j Xj þ bjj Xj Xj
neural network (ANN) model from Toolbox V7.12 of Xj¼1
X j¼1
MATLAB mathematical software is also constructed þ bij Xi Xj þ e ð1Þ
for prediction of the system response. The effort is i\ j¼2
intended to compare the performances of the two
popular functional approximation methods in yielding where Y is the predicted system response, b0 is the
adequate prediction of the studied alkyd polyconden- model intercept, k is the number of design variables,
sation process. The implementation followed the basic and Xj ; Xj Xj ; Xi Xj represent the first-order term(s), the
procedure for ANN model.24,25 The performances of second-order term(s), and the interaction term(s) of
ANN and RSM models were statistically measured and the model, respectively.
compared by mean relative percent deviation bj ; bij and bjjbjjj are the respective coefficients of the
(MRPD). model terms, and e is the random error. The coefficient
terms were calculated using the MBC algorithm such
Results and discussion that the predicted error sum of squares (PRESS) is
minimized. This leads to the specific RSM model for
Predictive model for system response conversion, viscosity, and MWA written as (2), (3), and
approximation via RSM (4), respectively:
 
Fitting a suitable approximation function usually linear Y1 A2 ; B2 ; C2 ; D2 ; E2 ¼ 2830:22 þ 18:53A þ 5:21B
polynomial (of quadratic, cubic or quartic order) to the þ 827:47C  0:033A2  0:01AB  2:28AC
experimental data followed the standard statistical
method. From preliminary evaluation of the system þ 3:31AD þ 0:0012AE  0:0032B2  4:85BD
achieved through the steepest ascent technique, a  0:002BE  339:91C2 ð2Þ
quadratic polynomial of the general form (1) was
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Table 1: Summary of statistics for the constructed RSM models

Response models Observations Parameters Box–cox Press RMSE RMSE R2 Adj R2 PRESS R2

Y1 30 13 1 6.481 4.275 0.9576 0.9276 0.8278

Y2 30 18 1 20.17 9.736 0.9777 0.9462 0.761
Y3 30 13 1 553 384.1 0.955 0.9232 0.8354
Target – – – 0 0 1 1 1

(a) (b)
100
Y1 [Conversion (%)]

Y1 [Conversion (%)]
80 90

60 70
40 50
20 30
0 10
280 280
200 0.5
260 150 260 0.4
240 100 240 0.3
0.2
[Temperature (°C) ] 220 50 B [Time (min)] A [Temperature (°C)] 220 0.1 C [Oil ratio]

(c) (d)
110 100
Y1 [Conversion (%)]

Y1 [Conversion (%)]

90
80
70
60
50

30 40
280 280
260 0.1 700
0.08 260 650
240 0.06 240 600
0.04 550
A [Temperature (°C)] 220 0.02 220 500
A [Temperature (°C)] E [Stirring rate (rpm)]
D [Catalyst concentration (w/w)]

(e)
(f)
100
100
Y1 [Conversion (%) ]

Y1 [Conversion (%)]

80
80
60 60

40 40
80
60 20
20 40
200
0
700 200
150 650 0.1
150 0.08
100 600 0.06
550 100 0.04
B [Time (min)] 50 500 E [Stirring rate (rpm)] 50 0.02
B [Time (min)]
D [Catalyst concentration (w/w)]

Fig. 2: Interaction effects between: (a) A and B, (b) A and C, (c) A and D, (d) A and E, (e) B and D, (f) B and E on conversion
of acid functional group
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Y2 A2 ; B2 ; C2 ; D2 ; E2 ¼ 11679:24 þ 65:69A Y3 A2 ; B2 ; C2 ; D2 ; E2 ¼ 264287:30 þ 1784:30A
þ 19:68B þ 3919:51C þ 6971:56D þ 4:66E þ 436:60B þ 42722:91C  3:25A2  0:91AB
2 ð4Þ
 0:099A  0:04AB  7:58AC  0:01AE ð3Þ þ 288:48AD  0:26B2  402:64BD  0:15BE
 0:008B2  2:42BC  18:11BD  0:007BE  28326:20C2  34:88CE þ 0:025E2
 900:09C2  2015:63CD  1:57CE  6:08DE

(a) (b)
300 300
Y2 [Viscosity (cP)]

Y2 [Viscosity (cP)]
200 200

100 100

0 0
280 280
260 200 260 0.5
150 0.4
240 240 0.3
100 0.2
[Temperature (°C)] 220 50 A [Temperature (°C)] 220 0.1
B [Time (min)] C [Oil ratio]

(c) (d)
300
300
Y2 [Viscosity (cP)]

250
Y [Viscosity (cP)]

200
200

150 100

100 0
280 200
260 700 0.5
650 150 0.4
240 600 0.3
550 100
220 0.2
A [Temperature (°C)] 500 E [Stirring rate (rpm)] B [Time (min)] 50 0.1
C [Oil ratio]

(e) (f)
300 400
Y [Viscosity (cP))

Y2 [ Viscosity (cP)]

250
300
200
200
150

100 100
200 200
150 0.1 700
0.08 150
100 0.06 100 600
0.04
B [Time (min)] 50 0.02 B [Time (min)] 50 500
E [Stirring rate (rpm)]
D [Catalyst concentration w/w]

Fig. 3: Interaction effects between: (a) A and B, (b) A and C, (c) A and E, (d) B and C, (e) B and D, (f) B and E, (g) C and D, (h)
C and E, (i) D and E on viscosity
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(g) (h)
300 300
Y2 [ Viscosity (cP)]

Y2 [ Viscosity (cP)]
250 250

200 200

150 150
0.5 0.5
0.4 0.1 0.4 700
0.3 0.08 0.3 650
0.06 600
0.2 0.04 0.2 550
0.1 0.02 0.1 500
C [Oil ratio] C [Oil ratio]
D [Catalyst concentration (w/w)] E [Stiring rate (rpm)]

(i)
300
Y2 [ Viscosity (cP)]

280

260

240

280
220
260
240
200 220
0.1
700
650
0.05
600
550
D [Catalyst concentration (w/w)] 0 500 E [Stirring rate (rpm)]

Fig. 3: continued

The performance of the constructed RSM models in uncertainties associated with every interaction of the
predicting the experimental data was tested using process variables. The observed trends suggest that by
RMSE, Press RMSE, R2, Adj R2 and PRESS R2 proper adjustment of the system variables within the
criteria as shown in Table 1. sampled space, a valid optimal could be attained. The
From the summary of statistics presented for the results conform largely to what is already known for
RSM models in Table 1, it seems that the RMSE and alkyd polycondensation processes.9,26–29
Press RMSE values are not as close to the targeted Nevertheless, one noticeable unusual result may be
value zero. However, the resulting coefficient of the apparent linear (one-directional) response observed
determination (R2 > 0.95) and Adjusted R2 > 0.92 are in the system response with respect to D and E axes. This
sufficiently close to their ideal value 1. This implies that does not reflect a typical behavior of batch alkyd
the models were sufficiently adjusted to yield adequate polycondensation processes. Particle congestion which
prediction of the actual system behavior and more than occurs at high catalyst concentration in the reactor and
95% of the overall system variability could be increased turbulence associated with high stirring rate is
explained by the predictive models. formally expected to introduce significant nonlinearities
or at least quadratic behavior in the system response.
The consistent linear behavior (in which increasing the
Interaction effects of process variables input value leads to a corresponding increase in output
with respect to D and E axes) implies that no definite
The combined effects of adjusting the process variables optimal solution could be obtained for the two variables.
within the design space were monitored using 3D surface If such an optimal condition exists for the present case,
plots. All significant interaction effects on the system then it definitely lies in a range outside the sampled
response between two independent variables were space. The selection of a useful optimal condition for the
analyzed in phases. The results are presented in Figs. 2, two variables would thus be guided strictly by a balance
3, and 4. The overall system behavior is characterized by of compromise between their effects on system response
various degrees of curvature which reflect the levels of and economic implication.
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J. Coat. Technol. Res.

(a) (b)
6000
6000
4000
Y3 [MWA (g/mol)]

Y3 [ MWA (g/mol.)]
2000
4000
0

-2000 2000

-4000
0
280
280
260 200
260 0.1
150 0.08
240 240 0.06
100
0.04
A [Temperature (°C)] 220 50 B [Time (min)] A [Temperature (°C)] 220 0.02
D [Catalyst concentration (w/w)]

(c) (d)
6000
6000
4000
Y3 [ MWA (g/mol.)]

Y3 [ MWA (g/mol)]
4000
2000

0 2000

-2000
0
200
200
150 0.1
0.08 150 700
0.06 650
100 100 600
0.04 550
B [Time (min)] 50 0.02 50
B [ Time (min)] 500 E [Stirring rate (rpm)]
D [Catalyst concentration (w/w)]

(e)

5000
Y3 [ MWA (g/mol)]

4000

3000
4000
2000
3000
2000
1000
0.5
0.4 700
0.3 650
0.2 600
C [Oil ratio] 550
0.1 500 E [Stirring rate (rpm)]

Fig. 4: Interaction between: (a) A and B, (b) A and D, (c) B and D, (d) B and E, (e) C and E, on molecular weight average

Figures 2a and 2b reveal some basic routes to their mean values, while either catalyst concentration
optimum progress of reaction for the studied alkyd (see Fig. 2c) or steering rate (see Fig. 2d) is reviewed
polymerization process which requires tuning the key upwards. By and large, the latter solution may be less
control variables including reaction time, temperature economically viable since it possibly leads to increased
or oil ratio to some values well above their center material/operational cost.30 The most economically
points while catalyst concentration and stirring rate are viable solution in terms of achieving optimal progress
fixed at their mean values. This framework stands as a of reaction may be traced to the possibility of reaching
viable solution, especially where oil as a major raw optimum conversion of the acid functional group either
material is relatively available. Alternatively, optimum with low catalyst concentration demonstrated in Fig. 2
conversion of the acid functional group could be e or with low stirring rate presented in Fig. 2f by
achieved by setting reaction time and temperature at merely allowing a relatively high reaction period.
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J. Coat. Technol. Res.

Table 2: Performance evaluation of the interaction of the process variables for the LM algorithm with 5 neurons in
the hidden layer for sensitivity analysis
No. Interaction MSE R2 Gradient BLF

Group of one variables

1 A 0.736 0.24 1.38 9 1009 Y1 = 0.217T + 51.9
2 B 0.546 0.42 4.30 9 1008 Y1 = 0.413T + 38.6
3 C 0.766 0.14 7.80 9 1004 Y1 = 0.15T + 56.9
4 D 0.836 0.09 3.40 9 1004 Y1 = 0.092T + 60.3
5 E 0.857 0.07 1.56 9 102 Y1 = 0.069T + 61.8
Group of two variables
6 AB 0.299 0.67 2.77 9 1000 Y1 = 0.682T + 20.5
7 AC 0.436 0.33 7.47 9 1009 Y1 = 0.377T + 39.9
8 AD 0.758 0.28 1.30 9 1010 Y1 = 0.179T + 55.6
9 AE 0.625 0.27 8.60 9 1008 Y1 = 0.211T + 52.9
10 BC 0.386 0.54 1.59 9 1009 Y1 = 0.475T + 37
11 BD 0.444 0.51 1.84 9 1003 Y1 = 0.51T + 32.9
12 BE 0.439 0.48 9.23 9 1012 Y1 = 0.597T + 26.9
13 CD 0.581 0.16 4.98 9 1009 Y1 = 0.18T + 54.5
14 CE 0.629 0.13 2.35 9 1011 Y1 = 0.167T + 58.2
15 DE 0.790 0.11 3.15 9 1011 Y1 = 0.075T + 62.2
Group of three variables
16 ABC 0.165 0.82 5.91 9 1010 Y1 = 0.81T + 11.7
17 ABD 0.217 0.76 8.86 9 1009 Y1 = 0.746T + 17
18 ABE 0.236 0.73 1.35 9 1010 Y1 = 0.632T + 24
19 ACD 0.410 0.46 1.05 9 1001 Y1 = 0.49T + 32.9
20 ACE 0.584 0.37 5.42 9 1012 Y1 = 0.336T + 42.9
21 ADE 0.613 0.30 2.11 9 1013 Y1 = 0.311T + 46.3
22 BCD 0.330 0.64 8.28 9 1010 Y1 = 0.601T + 26.4
23 BCE 0.385 0.58 9.01 9 1009 Y1 = 0.586T + 26.6
24 BDE 0.419 0.57 1.06 9 1011 Y1 = 0.541T + 30.4
25 CDE 0.642 0.20 1.42 9 1012 Y1 = 0.204T + 52
Group of four variables
26 ABCD 0.095 0.86 1.35 9 1011 Y1 = 0.823T + 11.7
27 ABCE 0.186 0.76 3.23 9 1012 Y1 = 0.663T + 23.1
28 ABDE 0.152 0.77 8.42 9 1011 Y1 = 0.752T + 15.4
29 ACDE 0.475 0.29 1.69 9 1010 Y1 = 0.173T + 63.1
30 BCDE 0.166 0.69 1.52 9 1012 Y1 = 0.717T + 19.1
Group of five variables
31 ABCDE 0.079 0.88 1.16 9 1011 Y1 = 0.853T + 10.1

Hence, reaction time seems to be a very important
process variable whose overall effects on the system
responses must be investigated in detail to enhance
selection of the most desirable optimal solution.
In a typical alkyd monitoring scheme, reactor
performance is usually measured in terms of the
commercial values of the resulting molecular proper-
ties of the product including cold-viscosity and/or
molecular weight average. Thus, these molecular
properties are usually monitored (preferably online)
such that the final product lies substantially within
specifications.31–34 As part of the present reactor
modeling and optimization scheme, data obtained for
cold-viscosity and MWA at various reactor conditions
were analyzed and the effects of every significant
interaction of the variables on system response were
evaluated systematically. The results of this study are
presented in Fig. 3 for cold-viscosity and Fig. 4 for
MWA.
In the coating industry, alkyd resin whose cold-
viscosity and MWA values lie in the range (243–
600 cP) and (4000–10000 g/mol.) satisfies most com-
mercial needs.35 The results presented in Fig. 2 high-
light various ways to achieve this target. Figures 3a, 3b,
3d, and 3g represent a typical behavior in which
increasing the value of the system variables initially
leads to a corresponding increase in the value of the
observed response before an optimum value is
attained, after which the trend is reversed. In Figs. 3c,
3f, 3h, and 2i, high viscosity response is recorded at low
stirring speed by reviewing upwards the temperature,
the reaction time, the oil ratio, and the catalyst
concentration, respectively. For some economic rea-
sons, it is usually more elegant to pursue a good result
 Author's personal copy
J. Coat. Technol. Res.

(a) 100 (b)

4
ANN predicted conversion (%) 90

80 3

70

MSE
2
60
Training
50 Validation
1
Data points Test
40 Best linear fit
A=T
30 0
20 40 60 80 100 0 5 10 15 20
Experimentally measured conversion (%) Epoch

Fig. 5: (a) Predicted vs actual values of conversion and (b) performance of the constructed NN model in predicting the
actual conversion of acid functional group

with low catalyst concentration and mean oil ratio

Best linear fit: A = (0.911) T + (25.2)
300 presented in Figs. 3c and 3e by merely allowing a
R = 0.962 relatively increased reaction time. This point again
highlights the reaction time as an important factor that
250 must be monitored closely to control both reaction
progress and product quality without unnecessarily
increasing the cost of operating the batch.
A

200
The results obtained for MWA properties of the
system at various operation conditions are presented in
Data points
150 Best linear fit
Fig. 4. Figure 4a highlights the futility of operating the
A=T reactor for a short reaction time using low reactor
temperature. With mean reaction time and moderate
100 temperature, a good result in MWA properties could
100 150 200 250 300
T be achieved, either with increased catalyst concentra-
tion as described in Fig. 4b or with high oil ratio as
Fig. 6: Predicted (A) vs actual (T) values of (a) the viscosity shown in Fig. 4e. However, both options may lead to
increased material cost making them less economically
viable. Some good alternative routes to desirable
Best linear fit: A = (0.938) T + (188) response are demonstrated in Figs. 4c and 4d where
5000 good MWA properties are instead obtained with low
R = 0.96 catalyst concentration and low stirring rate, respec-
4000 tively, by merely increasing the reaction time.
3000
A

Sensitivity analysis and reaction prediction via

2000
1000
0 ined using the LM (Levenberg–Marquardt) algorithm.
0 2000
T
Fig. 7: Predicted (A) vs actual (T) values of the molecular
weight average
with moderate oil ratio and reduced catalyst concen-
tration. Thus, an important observation made in this
regard is the possibility of obtaining high viscous resin
ANN
Data points
Best linear fit The performances of the five interaction groups of
A=T
(one, two, three, four, and five) variables were exam-
4000 6000
The results are presented in Table 2. The results show
that while B (i.e., reaction time) is the most effective
parameter in the group of one variable, the interaction
of A and B which shows relatively low MSE value
(0.299) has the greatest effect in the group of two
variables. Similarly, the interaction of five variables
produced the most significant effect on the studied
response with the overall minimum MSE of 0.079. This
 Author's personal copy
J. Coat. Technol. Res.

Table 3: RSM and ANN results compared with the experimental data
S/N Independent variables Y1 (%) Y2 (cP) Y3 (g/mol)
A B C D E Actual RSM ANN Actual RSM ANN Actual RSM ANN

1a 240 90 0.4 0.08 650 63.1 63.50 61.67 217 216.46 217.31 2438 2323.35 2712.2
2c 260 150 0.4 0.08 650 91.1 86.99 79.09 229.4 225.92 231.21 4890 4759.37 4046.9
3a 260 150 0.4 0.04 550 81.5 80.35 78.75 291 280.86 267.15 4995 4825.27 4903.0
4b 240 90 0.4 0.04 550 39.8 38.33 37.75 163.4 161.28 176.08 693.9 735.422 0795.6
5a 260 90 0.2 0.08 650 78.5 77.03 72.44 250.9 253.55 255.85 3620 3746.13 3571.1
6a 260 90 0.4 0.04 650 69.8 66.16 70.16 240.3 231.56 242.57 3088 3006.32 3062.8
7a 260 90 0.4 0.08 550 71.8 69.84 75.24 274.7 270.80 267.07 4436 4089.09 3507.7
8c 240 150 0.2 0.04 550 61.2 63.06 65.86 216.9 219.94 244.04 2533 2805.58 3041.3
9a 260 150 0.2 0.08 550 79.1 79.57 78.86 280 281.26 279.01 4292 4101.14 4199.7
10b 260 150 0.2 0.04 650 78.4 75.61 78.44 261.3 257.71 270.69 3790 3564.02 4067.7
11a 240 150 0.4 0.04 650 77.2 77.21 76.78 260.6 258.89 257.75 3886 3463.81 3808.5
12a 240 90 0.2 0.04 650 31.1 34.00 34.84 141 145.43 145.05 500 392.46 0340.5
13a 240 90 0.2 0.08 550 31.5 37.43 40.10 141.6 145.80 156.48 500 746.82 0715.3
14c 240 150 0.2 0.08 650 64.3 64.66 77.45 231.5 236.11 267.27 2993 3206.51 4066.0
15a 260 90 0.2 0.04 550 43.3 46.82 48.79 178.3 174.30 185.93 1270 1229.79 1441.0
16b 240 150 0.4 0.08 550 79.4 80.92 78.20 276.2 274.26 276.88 4640 4467.76 4280.6
17a 270 120 0.3 0.06 600 71.1 76.71 78.66 241.3 253.77 267.11 3336 3803.18 3864.0
18a 230 120 0.3 0.06 600 51.6 45.90 48.92 181.8 174.32 186.29 1200 1058.33 1302.8
19a 250 180 0.3 0.06 600 83.2 85.16 79.02 274.6 278.07 278.60 4445.5 4695.51 4552.0
20c 250 60 0.3 0.06 600 43.4 41.35 36.52 167.6 169.12 165.02 839 840.2 303.4
21a 250 120 0.5 0.06 600 66.5 71.75 77.50 229.4 243.19 232.06 2921 2956.50 3107.3
22b 250 120 0.1 0.06 600 55.8 50.46 63.60 200.5 191.70 205.72 1947 1637.01 1717.0
23a 250 120 0.3 0.1 600 81.5 84.50 77.97 271.8 275.22 268.14 4294 4681.99 4091.3
24a 250 120 0.3 0.02 600 61.1 64.90 59.73 215.4 231.67 214.85 2111.7 2777.61 2012.4
25a 250 120 0.3 0.06 700 78.7 80.81 76.22 259.1 255.59 248.96 3850 4140.83 3818.4
26c 250 120 0.3 0.06 500 75.2 68.60 69.22 251.2 251.31 242.95 3830 3825.56 4311.0
27a 250 120 0.3 0.06 600 75.4 74.70 73.63 256.1 253.45 264.17 3980 3729.80 3869.0
28b 250 120 0.3 0.06 600 75.1 74.70 73.63 256.4 253.45 264.17 3980 3729.80 3869.0
29a 250 120 0.3 0.06 600 75.4 74.70 73.63 256.5 253.45 264.17 3986 3729.80 3869.0
30a 250 120 0.3 0.06 600 75.3 74.70 73.63 256.1 253.45 264.17 3988 3729.80 3869.0
a b c
Training data set; validating data set; testing data set of the ANN mode

Table 4: MRPD for RSM and ANN

MRPD (%)
RSM ANN

Conversion ±4.47 ±6.50

Viscosity ±2.08 ±3.31
MWA ±8.92 ±10.20

suggests that the most accurate prediction of the
system via ANN model could be achieved by using
the five independent variables in the formulation of the
model.
Reaction prediction via ANN
The performances of the constructed artificial neural
network model in yielding the conversion of acid
functional group (Y1), viscosity (Y2), and molecular
weight average (Y3) were evaluated considering the
highest order interaction of the system variables
(ABCD E), respectively. The results are presented in
Figs. 5a, 5b, 6, and 7 for Y1, Y2, and Y3, respectively.
The ANN results and that of equivalent RSM are
compared with experimental data in Tables 3 and 4.
From the comparative study, when looking at the
performances of the two functional approximation
models, it seems that greater overall prediction accu-
 Author's personal copy
J. Coat. Technol. Res.
Table 5: Optimal condition of input variables and reactor response obtained via coupled RSM-GA method
Obj. function
Temperature Time (min)
(C) A B (C)
Conversion 266.671 70.706
Viscosity 262.630 135.039
Molecular weight 268.425 155.236
average
Table 6: Global optimal values of process parameters for maximum responses
Temperature Time Oil ratio Catalyst
(C) A (min) B (C) con. (w/w) D
268 115 0.49 0.078
racy is guaranteed by the RSM model. Further analysis
of the predictive efficiency of models using MRPD as
shown in Table 4 clearly showed that RSM is a better
model for the alkyd resin polycondensation process.
This may be because of the limited number of
experimental data used in the analysis. ANN generally
performs better when very large number of data points
is used for training the network.24,36 Attempts to
compare this observation overtly with earlier work
from the literature did not provide the desired result.
This is because there is little or no study on the alkyd
resin polycondensation process modeling using ANN
and RSM. However, the result contained in this essay
is apparently different from the literature: methanol-
ysis of sunflower oil using ANN and RSM in which
there are 162 data points;36 RSM and ANN modeling
of electrocoagulation of copper from simulated
wastewater;37 optimization of recombinant of oryza
sativa nonsymbiotic hemoglobin using ANN and
RSM;38 optimization of biosorption process using
ANN and RSM;39 alkaline palm oil transesterification
of by RSM and ANN.40 From the previous, the
prediction accuracy was more prominent for ANN
possibly because it was built up from the experimental
results of RSM.
Optimization by coupled RSM-GA technique
In a typical coating manufacturing business, the need
for optimization arises where coating formulators
desire some obvious qualities like short drying time,
reduced material cost, improved color (appearance),
and weight. Of particular interest is the viscosity and
molecular weight average which affect the end-use
properties. We may recall that a major objective is to
design a route to high-quality resins with good poly-
merization properties for industrial coating processes
from a nondrying oil. Optimization problems may be
compounded when the process(es) pose multiple
Ind. variables
Oil ratio Catalyst con. Stirring rate Obj. function
(w/w) D (rpm) E optimum value
0.305 0.036 653.761 99.81%
0.229 0.076 655.135 640.91cP
0.469 0.067 505.981 5238.88 g/mol
Stirring rate Responses
(rpm) E
Y1 (%) Y2 (cP) Y3 (g/mol)
502 104 582 4814
desired responses which may be a combination of
two or more of above-stated conditions. A standard
approach to this problem is to formulate global
optimization criteria through which the necessary
trade-offs will help to achieve what may be considered
as the best combination for the desired result.
Considering the observed performance of the RSM,
the predictive models obtained for the three molecular
properties (including conversion, viscosity, and molec-
ular weight average) via RSM were separately linked
to GA (genetic algorithm) for evaluation of the specific
optimal conditions of the system variables and the
optimum response. The values of GA specific param-
eters used in the study were as follows: population
size = 2; cross-over probability = 1.0. The optimum
conditions were selected after evaluation of the GA for
10 iterations. The results of the optimization study are
presented in Table 5.
Following the GA multiobjective optimization pro-
cedure discussed in reference (41) the final global
optimal result obtained is given in Table 6.
No unique solution was found for the global
optimal. Thus, the selection of the data in Table 6 as
the global optimal conditions was based on a logical
trade-off among the parameters, guided by economic
considerations. Corresponding experiments conducted
at the global optimal conditions show that the actual
(99.2%, 579 cP, 4800 g/mol) were in reasonable agree-
ment with the statistical results (104%, 582 cP,
4814 g/mol) for Y1, Y2, and Y3. It is important to note
that no model is perfect. The model prediction of
104% in conversion (Y1) is an abstraction of reality as
conversion (Y1) cannot be more than 100%. This is a
result of possible overfitting in the model. However,
validation experiments using the established global
conditions gave 99.2%, indicating that they are realistic
conditions. Therefore, it is recommended that coating
formulators should operate at the given optimal
conditions in other to synthesize high-quality alkyd
resin in a most economical way.
 Author's personal copy
Conclusion
Artificial neural network (ANN) and response surface
methodology (RSM) based on a 251 fractional facto-
rial design were used to simulate and optimize the
polycondensation process for autooxidative drying
alkyd resin from palm kernel stearin (PKS): rubber
seed oil (RSO) blend of 70:30 ratio. The performance
of the RSM and ANN model showed adequate
prediction of the responses in terms of the process
factors, with MRPD of ±4.47% (Y1), ±2.08% (Y2),
±8.92% (Y3) and ±6.50% (Y1), ±3.31% (Y2),
±10.20% (Y3), respectively. The sensitivity analysis
showed that while reaction time is the most effective
process parameter, the interaction of the five process
variables produced the most significant effect on the
studied responses with the overall minimum MSE of
0.079. The optimization task performed using genetic
algorithm linked to the RSM model gave optimal
responses of conversion 104%, viscosity 582 cP, MWA
4814 g/mol at optimum operating conditions of tem-
perature 268, time 115 min, oil ratio 1:0.49, catalyst
concentration 0.78, and stirring rate 502. Correspond-
ing experiments at selected optimal gave viable results.
Coupled RSM-GA was found to be a better tool for
modeling and optimization of the alkyd resin produc-
tion.
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