Energy Sources, Part A: Recovery, Utilization, and

Environmental Effects

ISSN: 1556-7036 (Print) 1556-7230 (Online) Journal homepage: http://www.tandfonline.com/loi/ueso20

Agglomeration of Makarwal coal using soybean oil

as agglomerant

Asad Mustafa, Toqeer Ahmad, Javaid Akhtar, Khurram Shahzad, Naseer

Sheikh & Shahid Munir

To cite this article: Asad Mustafa, Toqeer Ahmad, Javaid Akhtar, Khurram Shahzad, Naseer
Sheikh & Shahid Munir (2016) Agglomeration of Makarwal coal using soybean oil as
agglomerant, Energy Sources, Part A: Recovery, Utilization, and Environmental Effects, 38:24,
3733-3739, DOI: 10.1080/15567036.2016.1141268

To link to this article: http://dx.doi.org/10.1080/15567036.2016.1141268

Published online: 01 Nov 2016.

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ENERGY SOURCES, PART A: RECOVERY, UTILIZATION, AND ENVIRONMENTAL EFFECTS
2016, VOL. 38, NO. 24, 3733–3739
http://dx.doi.org/10.1080/15567036.2016.1141268

Agglomeration of Makarwal coal using soybean oil as agglomerant

Asad Mustafa, Toqeer Ahmad, Javaid Akhtar, Khurram Shahzad, Naseer Sheikh,
and Shahid Munir
Centre for Coal Technology University of the Punjab Lahore, Pakistan

ABSTRACT KEYWORDS
The study was carried out for beneficiation of Makarwal coal using soybean Agglomeration; ash; gross
oil as agglomerant. The effect of six parameters – pH, mesh size of coal calorific value; Pakistani coal;
particles, slurry ratio, stirring speed, soybean oil concentration, and time of soybean oil; sulfur
agglomeration – was investigated to reduce ash and sulfur from Makarwal
coal and to enhance the gross calorific value. In the cleaned product obtained
after the agglomeration process, the gross calorific value was increased from
4900 to 7115 Kcal/kg. The ash of agglomerates was reduced from 30% to
7.5% and sulfur was reduced from 5.4% to 2.0% The optimum operating
conditions were concentration of soybean oil 10 mL, pH 9, stirring speed
2800 rpm, mesh size 200, coal to water ratio of 15:450 (W/V), and time of
agglomeration 20 min. Significant reduction in ash and sulfur showed the
effectiveness for agglomeration of Makarwal coal using soybean oil as the
agglomerant. The final product thus obtained may be used efficiently in
various energy recovery schemes.

Introduction
Pakistan is blessed with 185 billion tons of coal reserves across all of its provinces. The majority of coal
deposits exist at Thar, Lakhra, Chamalang, Loralai, Khushab, Mianwali, Makarwal, Kotali, and Narran.
Coal from Chamalang, Kotli, and Narran regions and a few other locations in Baluchistan lie in the
range of high volatiles bituminous-C (Wahab et al., 2015). The majority of coal reserves located in
Punjab and Sindh region contain high ash and high sulfur contents. It is often essential to wash off
unnecessary ash and sulfur from coal to increase its calorific value. Makarwal coal deposits, estimated
at 22 million tons, occur in the province of the Punjab. The reserves are in the vicinity of many cement
plants; however, due to the high ash and high sulfur contents, Makarwal coal cannot be decisively used
as a fuel source. The mineral matter including pyrite is very finely disseminated in the coal matrix. The
process of agglomeration appears to be applicable for the upgradation of Makarwal coal. Moreover,
agglomeration is a useful beneficiation technique that can deal with fines in finely ground coal
(Sahinoglu and Uslu, 2008; Aslan and Ünal, 2009; Chary and Dastidar, 2012).
Agglomeration converts coal fines into lumps using a suitable bridging liquid. A large variety of
bridging liquids have been investigated for the agglomeration of coal fines such as jatropha oil, sunflower
oil, canola oil, xylene, n-heptane, and diesel oil (Baruah et al., 2000; Sahinoglu and Uslu, 2008). The effect
of some important processing variables is significant on the efficiency of the agglomeration process,
including coal particle size, stirring speed, pH of coal water slurry, type and quantity of the agglomerant,
and to a lesser extent on the residence time of agglomerate formation. The existing literature on the
agglomeration of coal mainly focuses on the cleaning of lignite and sub-bituminous coals using a
variety of agglomerants, mainly fossil oils, vegetable oils, and organic solvents (Cebeci and Eroglu,
1998; Alonso et al., 1999; Baruah et al., 2000; Valdés and Garcia, 2006; Sahinoglu and Uslu, 2008).

CONTACT Shahid Munir [email protected] Centre for Coal Technology University of the Punjab Lahore, Pakistan.
Color versions of one or more of the figures in the article can be found online at www.tandfonline.com/ueso.
© 2016 Taylor & Francis Group, LLC
3734 A. MUSTAFA ET AL.

The present study investigates the agglomeration of Makarwal coal (Punjab, Pakistan) using
soybean oil as agglomerant. The effect of six parameters – pH of agglomeration slurry, coal to water
ratio, particle size of coal feed, stirring speed, soybean oil concentration, and residence time –was
investigated on gross calorific value (GCV), and proximate contents of agglomerates formed.

Experimental
Refined soybean oil was purchased from the local market. About 40 kg representation bulk coal was
obtained from the operating Makarwal mine (Mianwali, Punjab). The coal was crushed to obtain the
desired size of 1–2 inches using a standard laboratory roller crusher. The crushed coal was then subjected
to disc grinding mills and subsequent sieving. For agglomeration test work, the ground sample was sieved
to obtain four fractions with mesh sizes of 60 (0.25 mm), 100 (0.15 mm), 200 (0.074 mm), and 300
(0.053 mm). The ground coal samples were sealed in airtight plastic bags before use. Volatile matter,
moisture, ash, and sulfur of the bulk product and test products were analyzed using standard ASTM
methods, D3175, D3173, and D3174, respectively. Total carbon and sulfur contents were measured using
a carbon sulfur analyzer (LECO SC-144 DR). The gross calorific value was determined using a LECO AC
500 calorimeter. The results of proximate analysis of the Makarwal coal sample are shown in Table 1.
The agglomeration tests were carried out in covered glass beakers of 500 mL capacity equipped with an
overhead stainless steel stirrer. In each experimental run, the weighed amount of coal was added to a beaker
and water was added according to the coal water ratio. The slurry was agitated for 3 min. Next, 1 mL of
soybean oil was poured into a test tube and 10 mL of distilled water was added. The test tube was agitated
vigorously and the emulsion was poured to the coal water slurry. The mixture was agitated for 10 min at the
desired agitation speed. After 10 min, the agitation was stopped and the contents were allowed to stay for
10 h to achieve the distinct phases of agglomerates and tailings. The sample was sieved through a 100 mesh
sieve and washed with 2 L of distilled water. Efforts were taken to minimize the breakage of the obtained
agglomerates during the wet sieving process. After washing the agglomerates were dried in a drying oven at
55°C for 24 h. The proximate analysis of the dried agglomerates was carried out using standard ASTM
methods. Sulfur and calorific value of the agglomerates were determined using a carbon sulfur analyzer and
a digital bomb calorimeter, respectively. The results are shown in Table 2.

Results and discussion

Effect of pH
Figure 1 represents the composition of agglomerates obtained at pH 7–11. It was observed that there
was a gradual increase in volatile matter, fix carbon, and GCV from pH 3.7 to 9, but on exceeding
this pH range there was insignificant increase in the above-referred components. The ash and sulfur
contents decrease gradually up to pH 9. It was found that there was no significant change in the
composition of agglomerates beyond pH 9. It was therefore concluded that pH 9 may be taken as the
optimum for the production of agglomerates. At pH 9, the composition of agglomerates was 46%
volatile matter, 36% fixed carbon, 15% ash, 2.8% sulfur, and 6485 kcal/kg GCV.
The reason for the good grade of agglomerates at pH 9 is that the pyrite, which floats well at
acidic pH, has depressed at basic pH along with the rest of the mineral matter, resulting in sufficient
reduction in sulfur and ash contents. The hydration energy of the mineral surfaces increased due to
hydrogen bonding with water, making the mineral matter hydrophilic, whereas the carbonaceous
matter having good floatability favorably improved the total carbon and GCV of agglomerates.

Table 1. Proximate analysis of Makarwal coal.

Moisture (%) Volatile matter (%) Ash (%) Fixed carbon (%) Sulfur (%) GCV Kcal/kg
4 34 30 30 5.4 4900
 ENERGY SOURCES, PART A: RECOVERY, UTILIZATION, AND ENVIRONMENTAL EFFECTS 3735

VM, % FC, % Ash, % Sulfur, % GCV (Kcal/kg)

50 6800
45 6600
% Content in agglomerates 40 6400
35
6200

GCV (Kcal/kg)
30
6000
25
5800
20
5600
15
10 5400

5 5200

0 5000
3.7 7 9 11
pH

Figure 1. The influence of pH on GCV and proximate contents of agglomerates. Conditions: coal to water ratio 20:80 (W/V),
RPM 2520, mesh size 100, soybean oil concentration 10% of coal weight, time 10 min.

Effect of particle size

Figure 2 represents the effect of mesh size on GCV and the proximate components of agglomerates
obtained at mesh sizes of 60#, 100#, 200#, and 300#. It was found that volatile matter increased from
45 to 47% and fixed carbon increased from 25 to 37% by increasing the mesh size from 60 to 300.
Ash was reduced from 27 to 13%, whereas sulfur was reduced from 5.1 to 2.5% by increasing the
mesh size from 60 to 300 meshes.

VM, % FC, % Ash, % Sulfur, % GCV (Kcal/kg)

50 8000
45 7000
% Content in agglomerates

40
6000
35
GCV (Kcal/kg)

30 5000

25 4000
20 3000
15
2000
10
5 1000

0 0
60 100 200 300
mesh size

Figure 2. Effect of mesh size on percentage content and GCV of agglomerates. Conditions: coal to water ratio 20:80 (W/V),
RPM 2520, soybean oil concentration 10% of coal weight, time 10 min, pH 9.
3736 A. MUSTAFA ET AL.

Regarding GCV, it was found that the GCV of agglomerates increased from 5310 to 6668 Kcal/kg by
changing the mesh size from 60# to 300#. At particle size of 200#, the ash rejection increased up to 50%
at 60#. The ash rejection further increased to 56% at 300#. However, recovery of agglomerates was
better for 200# at reasonable ash rejection. Therefore, the particle size of 200# may be regarded as
optimum for further experiments. The significant decrease of ash and sulfur in coal agglomerates is
due to the coalescing effect of coal fines. It is obvious that the smaller the size of the coal particles,
the more efficient would be the coalescing forces. For very fine particle sizes, the coal particle
coalescing dominates compared to coal ash particles coalescing. Due to this reason the ash particles
settle down easily, resulting in agglomerates of better quality. Therefore it is necessary to grind the coal
into fines for efficient agglomeration. The agglomerates obtained at 200 mesh size show high GCV and
low ash and sulfur contents. Although a slight increase in GCV was observed for 300 mesh size, it is
uneconomical to crush coal to extreme fineness.

Effect of slurry ratio

Figure 3 shows the effect of three slurry ratios 15:450, 20:180, and 40:160 on the proximate properties
and GCV of agglomerates. As the solid liquid ratio increases, volatile matter, fixed carbon, and GCV
progressively decreased, but ash and sulfur contents increased. Fixed carbon decreased to 38%, 36%,
and 33% and GCV decreased to 6684 kcal/kg, 6484 kcal/kg, and 6104 kcal/kg for slurry ratios of 15:450,
20:80, and 40:160, respectively. Ash contents increased to 13%, 15%, and 19% and sulfur contents
increased to 2.5%, 2.8%, and 3.4% for slurry ratios of 15:450, 20:80, and 40:160, respectively. If the
solids in pulp increase, the ash and sulfur contents also increase in agglomerates, suggesting
that the dilute slurries are appropriate to avoid entrapment of mineral matter in agglomerates. It is
evident from Figure 4 that a maximum ash reduction of 56.7% was observed when a slurry ratio of
15:450 was used, whereas at higher slurry ratio of 40:160, the ash reduction was 36.6%. This trend is in
agreement with the slurries already performed for using low and high solid liquid ratio used for the
agglomeration of coal.

VM, % FC,% Ash,% Sulfur, % GCV (Kcal/kg)

50 6800
45 6700
% Content in agglomerates

40 6600
35 6500
GCV (Kcal/kg)

30 6400
25 6300
20 6200
15 6100
10 6000
5 5900
0 5800
10:.90 20:.80 40:160
Coal to water ratio

Figure 3. Effect of coal to water ratio on proximate content and GCV of agglomerates. Conditions: RPM 2520, soybean oil
concentration 10% of coal weight, time 10 min, pH 9, mesh size 200.
 ENERGY SOURCES, PART A: RECOVERY, UTILIZATION, AND ENVIRONMENTAL EFFECTS 3737

VM.% FC,% Ash,% Sulfur,% GCV (Kcal/kg)

50 6600
45 6400
% Content in agglomerates
40
6200
35
6000

GCV (Kcal/kg)
30
25 5800
20 5600
15
5400
10
5 5200

0 5000
1960 2520 2800
RPM

Figure 4. The influence of RPM on GCV and proximate content of agglomerates. Conditions: coal to water ratio 14:450 (W/V),
soybean oil concentration 10% of coal weight, time 10 min, pH 9, mesh size 200.

Effect of speed
Figure 4 represents the effect of speed ranging from 1960 to 2800 rpm on GCV and proximate contents
of coal agglomerates. It was found that the volatile matter increased from 44% to 46%, fixed carbon
increased from 29% to 36%, and GCV increased from 6542 Kcal/kg to 6485 Kcal/kg. The ash and sulfur
contents reduced from 24% to 15% and from 4.5% to 3.8%, respectively. At the higher speed of
2800 rpm, better interaction of coal particles and separation of ash and sulfur from agglomerates was
observed. From the figure it is evident that GCV was maximum at a high stirring speed; therefore,
2800 rpm is considered as optimum stirring speed for the agglomeration of Makarwal coal.

Effect of collector concentration

Figure 5 shows the effect of soybean oil concentration in the range of 5–30% on the proximate
properties and GCV of agglomerates. Volatile matter content increased continuously with an
increase of soybean oil concentration. Fixed carbon and GCV both decreased at higher oil concen-
tration. It was also observed that the higher concentration of oil was not helpful in lowering ash and
sulfur in agglomerates. From Figure 5, it is clear that a soybean oil concentration of 10% was the
optimum to produce maximum ash and sulfur reduction. Ash reduction at 10% concentration of
soybean oil was 56%. The sulfur reduction remained almost constant to the variations in oil
concentration, as evident in Figure 5. GCV sharply reduced from 6485 kcal/kg to 5498 kcal/kg by
increasing the soybean oil concentration from 10% to 30%. It was found in this study that a high
concentration of soybean oil was not recommendable. Excessive amount of soybean oil makes the
agglomerates pasty, making it difficult to wash with organic solvents (methanol in this study),
resulting in an increase in the volatile content of agglomerates. The increase in volatile content
and decrease in fixed carbon are mainly attributed to the unwashed oil from the recovered
agglomerates. Moreover, pasty agglomerates entrap more of mineral matter contents, thereby
imparting a negative influence on ash reductions. From the discussion, soybean oil concentration
of 10% is recommended for the cleaning of Makarwal coal.
3738 A. MUSTAFA ET AL.

VM. % FC, % Ash, % Sulfur, % GCV (Kcal/kg)

70 6600

60 6400
% Content in agglomerates
6200
50

GCV (Kcal/kg)
6000
40
5800
30
5600
20
5400
10 5200

0 5000
5 10 20 30
Soy bean oil concentration (W/W)

Figure 5. Effect of soybean concentration on GCV and proximate content of agglomerates. Conditions: coal to water ratio 14:450
(W/V), time 10 min, pH 9, mesh size 200, RPM 2800.

Effect of agitation time

Figure 6 shows the effect of agglomeration time on GCV and proximate contents of agglomerates.
Volatile matter, fixed carbon, and GCV increased with increase in agglomeration time. Longer residence
time was helpful in removing ash and sulfur from coal. At an agglomeration time of 30 min, reduction in
ash and sulfur was 76.6% and 55.5%, respectively. The GCV also increased to 7315 kcal/kg from

VM, % FC, % Ash, % Sulfur, % GCV (Kcal/kg)

60 8000

7000
50
% Content in agglomerates

6000
40
GCV (Kcal/kg)

5000

30 4000

3000
20
2000
10
1000

0 0
5 10 20 30
Time (min)

Figure 6. Effect of time on proximate content and GCV of agglomerates. Conditions: coal to water ratio 14:450 (W/V), time 10 min,
pH 9, mesh size 200, RPM 2800.
 ENERGY SOURCES, PART A: RECOVERY, UTILIZATION, AND ENVIRONMENTAL EFFECTS 3739

6485 kcal/kg by increasing the residence times from 5 to 30 min. Figure 6 shows better results for volatile
matter, ash, sulfur, and GCV when the agitation time was taken as 30 min.

Conclusions
Makarwal coal was subjected to agglomeration process by using soybean oil as agglomerant. The effect
of six variables (pH, particle size, slurry ratio, stirring speed, soybean oil concentration, and residence
time) was evaluated for proximate properties and GCV of agglomerates. According to the results, the
optimum parameters were found to be pH 9, particle size 75 µm, coal to water ratio 15:450 (V/W),
stirring speed 2800 rpm, soybean oil concentration 10 mL, and residence time of 30 min. The GCV of
clean agglomerates was increased from 4900 to 7115 Kcal/kg. The ash of agglomerates reduced from
30% to 7.5%, i.e. 75% ash reduction. The final product thus obtained may be used efficiently in various
energy-recovery schemes.

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