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Application of articial neural networks to predict

chemical desulfurization of Tabas coal
E. Jorjani *, S. Chehreh Chelgani, Sh. Mesroghli
Department of Mining Engineering, Research and Science Campus, Islamic Azad University, Poonak, Hesarak, Tehran, Iran
Received 26 May 2007; received in revised form 25 January 2008; accepted 29 January 2008
Available online 27 February 2008

Abstract
This paper presents a neural network model to predict the eects of operational parameters on the organic and inorganic sulfur
removal from coal by sodium butoxide. The coal particle size, leaching temperature and time, sodium butoxide concentration and
pre oxidation time by peroxyacetic acid (PAA) were used as inputs to the network. The outputs of the models were organic and inorganic
sulfur reduction. Feed-forward articial neural network with 5-7-10-1 arrangement, were capable to estimate organic and inorganic sulfur reduction, respectively. Simulated values obtained with neural network correspond closely to the experimental results. It was achieved
quite satisfactory correlations of R2 = 1 and 0.96 in training and testing stages for pyritic sulfur and R2 = 1 and 0.97 in training and
testing stages, respectively, for organic sulfur reduction prediction. The proposed neural network model accurately reproduces all the
eects of operational variables and can be used in the simulation of Tabas coal desulfurization plant.
2008 Elsevier Ltd. All rights reserved.
Keywords: Articial neural networks; Coal; Chemical desulfurization

1. Introduction
Articial neural network (ANN) is an empirical modeling tool, which is analogous to the behavior of biological
neural structures [1]. Neural networks are powerful tools
that have the ability to identify underlying highly complex
relationships from inputoutput data only [2]. Over the last
10 years, articial neural networks (ANNs), and particularly feed-forward articial neural networks (FANNs),
have been extensively studied to present process models,
and their use in industry has been rapidly growing [3].
The use of such networks can now be found for number
prediction such as modelling the greenhouse eect [4], simulation N2O emissions from a temperate grassland ecosystem [5], modelling of rare earth solvent extraction [6],
bioleaching of metals [7] and coal microbial desulfurization
[8].

Corresponding author. Tel.: +98 912 1776737; fax: +98 21 44817194.

E-mail address: esjorjani@yahoo.com (E. Jorjani).

0016-2361/$ - see front matter 2008 Elsevier Ltd. All rights reserved.
doi:10.1016/j.fuel.2008.01.029

The use of neural networks to predict coal nal sulfur

content, after desulfurization with Acidithiobacillus bacteria, was reported by Acharya et al. [8]. Type of coal, initial
pH, pulp density, particle size, residence time, media composition and initial sulfur content of coal were fed as inputs
to the network and output of the model was nal sulfur
content (about 0.26.6 (%) for the tested samples) after
desulfurization.
The aim of the present work is the assessment of Tabas
coal with reference to the organic and inorganic sulfur
removal by sodium butoxide, as leaching agent, and possible variations with change of coal particle sizes, leaching
temperature and time, sodium butoxide concentration
and duration time of peroxyacetic acid (PAA) pretreatment
of coal (to enhancing of coal desulfurization by sodium
butoxide), using experimental data obtained at a laboratory level and simulated data by means of a neural network, MATLAB software package. To our knowledge,
this is the rst time that ANNs have been used to predict
both of organic and inorganic sulfur removal from coal
in a chemical desulfurization process.

2728

E. Jorjani et al. / Fuel 87 (2008) 27272734

2. Area description
2.1. Desulfurization of coal with sodium butoxide
The use of high-sulfur coals for energy production
requires a cleaning stage to meet environmental regulations. Sulfur in coal occurs in organic and inorganic forms.
The organic form is about 50% of the total sulfur that cannot be removed by physical coal cleaning methods [9].
Removal of organic sulfur requires chemical desulfurization techniques that can remove inorganic sulfur and
ash-forming minerals too. Generally, cleaning is carried
out over the ue gases, but chemical desulfurization has
also received attention. Physical and microbial methods
were also used. Although chemical desulfurization of coal
is not protable in the current economic conditions, it
may become economical in the future, as SO2 emission regulations are tightened and low sulfur coal reserves are
depleted.
Well known desulfurization processes include: caustic
treatment [10], pyrolysis [11,12], oxidation [1315], IGT
hydrodesulfurization [9], magnex process [16] and chemical
comminution [17]. Oxidation is the most often applied
chemical method of coal desulfurization [18]. Hydrogen
peroxide, sodium hypochlorite, nitric acid, potassium permanganate, air, and many other oxidants are used in this
method. Oxidation of coal is a very complex process,
dependent on a number of parameters such as temperature,
pressure, time, reagent concentration, type of coal and its
grain size distribution. Oxidation can change coal characteristics such as caloric value, free swelling index, sinter
ability and extractability [19,20].
The use of PAA as oxidative reagent for the desulfurization of coal has been reported by Palmer et al. [21,22], Sonmez et al. [23] and Aelst et al. [24]. PAA is believed to
produce hydroxyl cations, which are strong electrophiles
and react with sulfur atoms because they are considerably
more nucleophilic than carbon atoms. It was also found
that selective oxidation of coal with PAA was a very eective pretreatment for enhancing desulfurization of coal
with various hydroxide and carbonate bases.
The structural properties of coal, such as porosity, surface area and pore size, play an important role in chemical
desulfurization. Coal contains moisture in its pores and
this moisture can be removed by heating at 100 C. Moisture removal is accompanied by a substantial increase in
porosity [25].
Borah et al. [26] have shown that coal oxidation by
heating, as a pretreatment process for coal desulfurization
by the process of electron transfer, decomposes the large
organic sulfur molecules to low molecular weight products. These smaller molecules are much more prone to
attack by the leaching solution in subsequent stages for
the rupture of CS as well as SS bounds. They also found
that low temperature oxidation converts coal organic
sulfur to compounds containing S@O and SO2 [26]. In
these aerial oxidized samples, besides aliphatic sulfur,

aromatic disulde compounds can also be leached out

[25].
Pietrzak and Wachowska [27] have studied the eect of
oxidants such as PAA and air on the oxidation of the coal
organic structure by FTIR. They found that during oxidation with atmospheric oxygen at 125 C for 7 days, hydrocarbon groups are more susceptible to oxidation than
sulfur groups; whilst PAA can convert organically bound
sulfur to oxidized forms such as sulphones (SO2) and sulphoxides (S@O).
The other chemical method of coal desulfurization is
leaching with straight-chain aliphatic or aromatic organometallic compounds [28,29]. The mechanism of pyritic sulfur removal from coal is not clear but the reactions for
organic sulfurs are:
RONa R1 SSR2 ! Na2 S ROR1 ROR2

RONa R1 SH ! Na2 S ROR1

R can be benzyl, methyl and n-butyl. During previous

studies the reduction of sulfate, pyritic, organic and total
sulfur for sodium benzoxide was found to be about 91,
68, 33 and 45.9%, respectively, and 75, 60, 11 and 28%
for sodium butoxide [29].
In this work the optical microscopy investigation shows
that pyrite is present in forms of discrete grains, fracture
and cavity lling, regular and irregular framboidal with particle size ranging from 1 to 40 lm. Scanning electron
microscopy studies show that some of pyrite particles are
distributed on ner than 1 lm. Fine grinding is needed for
the removal of this ne distributed sulfur from coal and is
impossible using the conventional methods in practice.
Therefore it was applied the chemical desulfurization
method. PAA + air oxidation was used as suitable pretreatment processes, for the subsequent desulfurization of coal
with sodium butoxide that was reported on previously published work [30]. The eects of other parameters such as
sodium butoxide concentration, leaching temperature and
time, and particle size, on the extent of dierent forms of
sulfur removal from Tabas coal were investigated.
3. Materials and methods
3.1. Coal sample
The bulk sample 600 kg in mass was collected from all
operating mine workings of C1 seam the Tabas coal
deposit in Iran. The sampling methods similar of Jones rifes, coning, and coning-and-quartering were used. Proximate and ultimate analyses were performed according to
standard techniques. In all samples, the content of total,
pyritic, and sulfate sulfur were determined by the methods
ISO 334 and 157 in replication [31,32]. For pyritic sulfur,
the iron concentration in nitric acid solution was determined by colorimetry. The dierence yielded the amount
of organic sulfur. The mineralogical composition of the
sample was also established (Table 1).

E. Jorjani et al. / Fuel 87 (2008) 27272734

2729

Table 1
Characterization of Tabas coal representative sample
Proximate analysis (wt% as received)
Moisture
Ash
Volatile matter
Fixed carbon

0.75
32.3
20.12
46.83

Ultimate analysis (wt% daf)

C
H
N
S
Odi

86.25
4.31
2.45
0.67
6.32

Forms of sulfur (wt% db)

Total
Pyritic
Sulfate
Organic

1.44
0.77
0.0
0.67

Mineralogical composition
Illite, quartz, kaolinite, goethite, feldspar, calcite, pyrite, hematite

3.2. Oxidation of coal with PAA + Air

PAA oxidation was carried out by dispersing 8 g of coal
in 240 ml of glacial acetic acid and warming it to the
desired temperature, followed by adding 80 ml of H2O2
solution (30% w/v) [33]. The experiments were carried
out in a 750 ml Pyrex reactor equipped with a thermometric tube and stirrer. Reaction times of 10, 20, 30 and 40 min
were used, and the reaction temperature was maintained at
40 C. After oxidation, the reactor was cooled and ltered
to recover the oxidized coal. The ltrate was washed with
hot water and dried at room temperature for 24 h. The
samples which oxidized using PAA (dried at room temperature), were used for further oxidation with air in an oven,
at 100 C for 1 h. It also helps to evaporate liquids from
coal pores and increasing the accessibility of sodium butoxide to the oxidized sulfurs.
3.3. Preparation of sodium butoxide
Sodium butoxide was prepared by adding the requisite
amount of sodium to 1-butanol (0.8 kg/l) in a ask tted
with a water condenser, and then placed in a cooling bath
to decrease the heat of the reaction. A 17% solution was
prepared by adding 42.84 g of sodium to 1000 ml of 1-butanol. This solution was then diluted with 1-butanol to prepare the other concentrations of sodium butoxide that
were needed.
3.4. Desulfurization procedure
The desulfurization experiments were carried out in an
80 ml microreactor (Fig. 1) heated in an oven. When the
oven reached the reaction temperature, the reactor, containing 40 ml of sodium butoxide and 7 g of oxidized coal, was
placed in it. The experiments were carried out using sodium

Fig.1. Reactor assembly.

butoxide concentrations of 5 and 10%, reaction times of 30,

60, 90 and 120 min, particle sizes of 8501400, 300850 and
<300 lm, and temperatures of 90, 120, 150 and 190 C. Following the reaction, the reactor was cooled in cool water
and ltered to recover the leached coal. The ltrate was
washed with hot water, dried in a vacuum oven at 60 C,
and analyzed for forms of sulfur. Percentage changes in
the sulfur in comparison to their original values were calculated as described in the literature [10]. The results for the
optimization of sodium butoxide concentration, leaching
temperature and time, particle size and PAA oxidation pretreatment time are shown in Table 2.
3.5. Articial neural networks
Since the 1940s, articial neural networks (ANNs) have
been used in various applications in engineering and science [3441]. ANNs are generally the software systems that
imitate the neural networks of the human brain [42]. It is
also possible to accept the ANNs as a parallel distributed
data process system. The ANNs can be applied successfully
in learning, relating, classication, generalization, characterization and optimization functions. Because ANNs have
the ability to work with incomplete data, posses error tolerance, and show graceful degradation, they can easily
form models for complex problems. Especially in the development of solutions for semi-structural or non-structural
problems, articial neural network (ANN) models can
have very successful results. Moreover, they can be
cheaper, faster and more adaptable than traditional methods [43].
The main advantages of the ANN models are: (1) no
particular knowledge is needed about the system being
modeled, unknown eects could be involved through a
proper design of the inputoutput patterns; (2) relative simplicity of neural network architecture [44]; (3) ANNs are
also very powerful to eectively represent complex non-linear systems [45].
These application processes of an ANN model design
include the steps below [42]:
1.
2.
3.
4.

Collecting the whole data in one place.

Determining the train and test sets.
Converting the data into the ANN inputs.
Determining, training and testing the network topology.

2730

E. Jorjani et al. / Fuel 87 (2008) 27272734

Table 2
Results of experiments for sulfur removal by sodium butoxide in dierent operational conditions
Test
number

PAA oxidation
pretreatment time
(min)

Leaching
temperature
(C)

Leaching
time (min)

Sodium butoxide
concentration (%)

Particle size (lm)

((upper limit + lower
limit)/2)

Organic sulfur
reduction (%)

Inorganic sulfur
reduction (%)

1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36

0
10
20
30
40
40
40
40
40
40
40
40
40
40
40
40
40
40
40
40
40
40
40
40
40
40
40
40
40
40
40
40
40
40
40
40

120
120
120
120
120
90
90
90
90
120
120
120
150
150
150
150
190
190
190
190
150
150
150
150
150
150
150
150
150
150
150
150
150
150
150
150

90
90
90
90
90
30
60
90
120
30
60
120
30
60
90
120
30
60
90
120
30
60
90
120
30
60
90
120
30
60
90
120
30
60
90
120

5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
10
10
10
10
5
5
5
5
5
5
5
5
5
5
5
5

700
700
700
700
700
700
700
700
700
700
700
700
700
700
700
700
700
700
700
700
700
700
700
700
1125
1125
1125
1125
575
575
575
575
150
150
150
150

13.21
20.31
23.54
27.89
33.58
8.49
18.4
24.59
30.21
14.59
24.89
37.2
20.48
28.94
38.79
41.6
24.5
31.7
41.59
44.6
17.79
32.97
40.78
45.7
17.45
27.26
35.3
39.29
22.12
29.13
40.12
42.13
25.18
33.12
45.17
49.17

52.17
64.27
65.89
66.91
67.41
28.45
45
56
62.8
38.64
57.3
71.6
44.27
60.6
71.1
76
47.56
64
74.56
80.7
46.19
55.76
72.01
77.55
28.45
44.04
54.25
61.36
40.12
58.16
71.77
78
45.31
61.84
78.45
84.36

5. Repeating the 1st, 2nd, 3rd and the 4th steps as long as it
is required to determine the optimal model.
6. Application of the optimal ANN model.
An ANN can be considered as a black box (hidden layers) consisting of a series of complicated equations for the
calculation of outputs based on a given series of input values [44]. It is able to develop a model relating the networks output to existing actual data used as inputs.
After determining the number of input variables by statistical means, the most appropriate architecture for the network should be determined. In this stage, several networks
should be created, trained and tested. The number of layers, the optimum number of neurons per layer and the
transfer function(s) in the hidden layer(s), obtain by trial
and error. Care was taken to avoid overtraining. Therefore
it was ensured not to include more weights and biases in
both networks than the number of data in the training
set [44].

A parameter wij (known as weight) is associated with

each connection between two cells. Thus each cell in the
upper layer receives weighted inputs from each node in
the layer below and then processes these collective inputs
before the unit sends a signal to other layers [46]. One of
the major advantages of ANN is ecient handling of
highly non-linear relationships in data, even when the exact
nature of such relationship is unknown [47].
The most popular ANN is the feed-forward multi-layer
ANN which uses back-propagation learning algorithm.
This type of network consists of three layers of nodes
namely an input layer, hidden layers and an output layer.
Feed-forward neural network usually has one or more hidden layers, which enable the network to model non-linear
and complex functions. Scaled data are introduced into
the input layer of the network and then is propagated
from input layer to hidden layer and nally to the output
layer [48]. Each node in hidden or output layer rstly acts
as a summing junction which combines and modies the

E. Jorjani et al. / Fuel 87 (2008) 27272734

inputs from the previous layer using the following

equation:
yi

i
X

xi wij bj

j1

where yi is the net input to node j in hidden or output layer,

xi are the inputs to node j (or outputs of previous layer), wij
are the weights representing the strength of the connection
between the ith node and jth node, i is the number of nodes
and bj is the bias associated with node j. Each neuron consists of a transfer function expressing internal activation level. Output from a neuron is determined by transforming
its input using a suitable transfer function. Generally, the
transfer functions for function approximation (regression)
are sigmoidal function, hyperbolic tangent and linear function, of which the most widely used for non-linear relationship is the sigmoidal function. The general form of this
function is as follows [49]:
zj 1=1 ey y

zj, the output of node j, is also an element of the inputs

to the nodes in the next layer.
The values of the interconnection weights are determined by a neural network training or learning procedure
using a set of data. The objective is to nd the value of
the weight that minimizes dierences between the actual
output and the predicted output in the output layer in
order to minimize the mean square errors (MSE), the average squared error between the network predicted outputs
and the target outputs [1]. In the learning process, there
are several variables that have an eect on the ANN training. These variables are the number of iterations, learning

2731

rate, the momentum coecient, number of hidden layers

and the number of hidden neurons. To nd the best set
of these variables and parameters, all of those must be varied and the best combination chosen [47].
In this work, the ANN model have been developed by
considering two hidden layer in MLP architecture and with
training using the EBP algorithm. The 5-7-10-1 ANN
model (Fig. 2), which adequately recognized the eects of
dierent operational conditions on the coal desulfurization,
can predict sulfur reduction for the inorganic and organic
forms.
4. Results and discussion
Neural network training can be made more ecient by
certain pre-processing steps [45]. In the present work all
inputs (before feeding to the network) and output data in
training phase, were used for pre-processing by normalizing the inputs and targets so that they have means of zero
and standard deviations of 1:
N p Ap  meanAps =stdAp

where Ap is actual parameter, meanAps is mean of actual

parameters, stdAp is standard deviation of actual parameter and Np is normalized parameter (input).
The mean and standard deviation for pre-processing of
input variables are given in Table 3.
A total of 36 sets of data were used in the predictions by
ANN; 25 data sets were used for training and 11 sets for
testing the network, for both organic and inorganic sulfur
reduction prediction. The training process was stopped
after 10 epochs (Figs. 3 and 4). In each epoch, the entire
training set is presented to the network, case by case; errors
are calculated and used to adjust the weights in the network using sigmoid transfer function. This method is based
on the BP error algorithm, which is an iterative supervisedlearning technique. A set of training examples is considered, and for each the desired output of the MLP is known.
The network learns the trends contained in the data set and
correlates the inputs and the outputs by nding the optimum set of weights that minimizes the dierences between
the predicted and actual output values. For each iterations,
an error between the predicted value and the actual value is
propagated backward from the output layer towards the
input through the hidden layers until the error is within
an acceptable limit [50]. The correlation coecient (R2) values in training stages were 1 (Figs. 5 and 6).

Table 3
Pre-processing parameters for ANN

Fig. 2. FANN architecture with two hidden layers and 5-7-10-1

arrangement.

Variables

Mean

Standard deviation

PAA oxidation time (min)

Leaching temperature (C)
Leaching time (min)
Particle size (lm)
Sodium butoxide con. (%)

36
146.8
80.4
675
5.8

10.41
25.12
34.34
247.07
1.87

2732

E. Jorjani et al. / Fuel 87 (2008) 27272734

Fig. 3. Parity plot for epoch and mean square error for training sets
(organic sulfur).

Fig. 4. Parity plot for epoch and mean square error for training sets
(inorganic sulfur).

Fig. 6. Inorganic sulfur removal predicted by neural network in training

process versus actual measured in laboratory.

Fig. 7. Organic sulfur removal predicted by neural network in testing

process in comparison to actual measured in laboratory.

Fig. 5. Organic sulfur removal predicted by neural network in training

process versus actual measured in laboratory.

Fig. 8. Inorganic sulfur removal predicted by neural network in testing

process in comparison to actual measured in laboratory.

The testing set which actually tests how good the model
is, shows that the models could estimate the sulfur reduction quite satisfactorily. The correlation coecient (R2)

values for testing sets were 0.97 and 0.96 in organic and
pyritic sulfur reduction predictions, respectively (Figs. 7
and 8). It was observed that organic and inorganic sulfur

E. Jorjani et al. / Fuel 87 (2008) 27272734

reduction from coal using ANN model could be predicted

satisfactory.

5. Conclusions

 The eects of time of oxidation with PAA, as pretreatment process, particle size, leaching agent concentration
and leaching temperature and time on coal desulfurization with an organo metallic compound, sodium butoxide, were investigated in laboratory.
 In the experiments, the pretreatment time of 40 min on
the temperature of 45 C by PAA, leaching temperature
and time of 150 C and 120 min, sodium butoxide concentration of 5%, and particle size <300 lm (with mean
particle size of 150 lm) were determined as the optimum
operational conditions for removal of organic (49%) and
inorganic sulfur (84%).
 The produced data, on laboratory optimization process,
were used to the simulation by means of articial neural
network. A feed-forward articial neural network with
5-7-10-1 arrangement was capable to estimate both of
organic and inorganic sulfur reduction.
 In testing process the used model could estimate the
sulfur reductions quite satisfactorily. The correlation
coecient (R2) values for testing sets were 0.97 and
0.96 in organic and pyritic sulfur removal predictions,
respectively.
 These studies on chemical removal of organic and inorganic sulfur from coal constitute new unexamined conditions that where ANN have never been used to
predict the amount of organic and inorganic sulfur
removal from coal.
 The used method and its related results can further be
used as an expert system in Tabas coal desulfurization
plant, in order to optimize the process parameters and
to evaluate the parameters interactions, for the expected
sulfur removal without having to conduct the new
experiments in laboratory.

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