Fuel 196 (2017) 102–109

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Full Length Article

Chemical demineralization of high ash Indian coal by using alkali and

acid solutions
Sushanta K. Behera a, Sudipto Chakraborty a, B.C. Meikap a,b,⇑
a
Department of Chemical Engineering, Indian Institute of Technology (IIT) Kharagpur, West Bengal 721 302, India
b
Chemical Engineering, School of Engineering, Howard College, University of Kwazulu-Natal, Durban, South Africa

h i g h l i g h t s g r a p h i c a l a b s t r a c t

Adequate demineralization of high

ash coal obtained by acid and alkali
treatment.

Degree of demineralization depends
on coal particle size and process
conditions.

More than 50% minerals present in
coal are leached out by acid/alkali
treatment.

The sodium complex formed restrict
the demineralization at higher alkali
solution.

The calorific value increased with the
degree of demineralization.

a r t i c l e i n f o a b s t r a c t

Article history: In the present work an attempt have been made to upgrade the low grade Indian coal to high grade coal
Received 15 January 2016 by using caustic (NaOH) leaching followed by acid (H2SO4) treatment. The experimental works aimed at a
Received in revised form 25 February 2016 selective attack on in situ MCL (Mahanadi Coal Limited) coal, Odisha, India with some fluxing agents like
Accepted 27 January 2017
NaOH and H2SO4. The leaching experiments were carried out in a stainless steel batch reactor of 2.5 L
Available online 4 February 2017
capacity with controlled heating facility. Initially, the coal sample with 16+100 mesh particle size
was leached with 50–150 g/L of NaOH solution at 100 °C for one hour and then subjected to leach further
Keywords:
with 20% sulfuric acid. The maximum demineralization from the level of 26% ash with NaOH (100 g/L)
Coal
Leaching
leaching 27.5% is achieved and with combined chemical treatment method (100 g/L NaOH followed by
Demineralization 20% H2SO4) was obtained 48% effectively. In addition, the results showed that the percent of demineral-
Particle size ization improved adequately by decreasing the particle size also with rise of the leaching time and tem-
SEM perature. Coal characterization of raw and treated coal was done by Scanning Electron Microscopy (SEM)/
EDS Energy Dispersive Spectroscopy (EDS) analysis and also showed that the calorific value of coal was
increased with increase the percent of demineralization of coal.
Ó 2017 Elsevier Ltd. All rights reserved.

1. Introduction

The low cost and availability of low grade coal are best feed
⇑ Corresponding author at: Department of Chemical Engineering, Indian Institute
materials for fuel and energy production. The high ash coals are
of Technology (IIT) Kharagpur, Kharagpur Technology, Paschim Medinipur, West
Bengal 721 302, India.
unsuitable for use in combustion, gasification, carbonization or liq-
E-mail address: bcmeikap@che.iitkgp.ernet.in (B.C. Meikap). uefaction process. However theses coals have several drawbacks

http://dx.doi.org/10.1016/j.fuel.2017.01.088
0016-2361/Ó 2017 Elsevier Ltd. All rights reserved.
 S.K. Behera et al. / Fuel 196 (2017) 102–109
like lower specific energy due to low carbon content, highly min-
eral and moisture contents and also low calorific value [1–6]. Coal
contains variable amounts of largely incombustible mineral matter
co-existing with the organic matrix called as impurity. Mineral
matter is consist of all the inorganic minerals (discrete phases),
as well as all elements (apart from C, H, O, N and S) that are in,
or associated with, coal. The mineral matter in coal exists in differ-
ent forms such as the coal discrete crystalline particles, amorphous
mineral phases, inorganic elements chemically bound to the
organic material and compounds dissolved in the pore or surface
water of the coal [7]. Clay minerals are the most abundant mineral
species and quartz is the second most abundant mineral phase in
the coal [8,9]. Except this, other mineral matters are also found
in the original coal that includes silicas or shales (kaolinite type),
calcite, gypsum, siderite, carbonates, pyrites, disulfides, sulfides,
sulfates, feldspars and trace elements [5,10].
The presence of mineral matter in the coal has adverse affects
on coal utilization and processing. Mineral matter is the inert solid
material in the coal which form ash during combustion [11]. The
effects of treatments on different forms of the mineral matters
may be different from coal to coal. It is difficult to reduce ash con-
tent to a minimum limit by physical method because the ash form-
ing mineral are intermixed to the organic part of coal. In the
physical method the coal is crushed into fine particles and the
removal of mineral matter based on their physical properties like
surface phenomena (wettability) and specific gravity [12–14]. It
is only possible in the chemical method for removal of associated
mineral and bound to coal matrix or structure. The mineral species
is dissolute in water acid or alkali solution in the chemical method.
The method used in the chemical cleaning of coal include acid
leaching or alkali leaching and or followed both acid and alkali at
varying physical parameters. It is more expensive than physical
methods concerning of total cost (fixed and operating cost). Chem-
ical cleaning of coal is using simple equipment and an aqueous
solution of common industrial chemicals and operation is easier
when it operate under mild condition but the cost of chemicals
needed [15].
A review of the literature on the chemical leaching of coal
reveals that the methods of acid and aqueous alkali or combined
leaching under moderate temperature and pressure conditions to
demineralize and desulfurize from various coals is suitable tech-
nique. Sharma et al. reported the method of chemical leaching of
low grade coals through alkali-acid leaching under mild condition
at atmospheric pressure resulting 75% demineralization [4]. Araya
et al. observed demineralization of sub bituminous coal from the La
Union are treated with aqueous alkali, and the elimination of ash
increases with reaction time, temperature and concentration of
solution [16]. Various organic acids and aqueous alkali used in
the demineralization studies for production of ultra clean from dif-
ferent types of coal reported by (Steel and Patrick, steel et al.,
Nabeel et al.) and also the removal of mineral matter during chem-
ical leaching depend on the coal characteristics, types and quantity
of mineral matter, size of coal particle, and solvent concentration
and contact time of leaching [17–20]. Culfaz et al., observed from
investigation the effect of temperature, caustic concentration and
time on the degree of demineralization of Turkish low and high
grade lignite coal (Beypazari 35.6% ash, and Soma 7% ash) are trea-
ted with Caustic and after washed with HCl solution. In the effect
of caustic treatment, most of silica (SiO2) and calcium oxide
(CaO) in the ash were removed. However, most of iron oxide
(Fe2O3) and Sodium oxide (Na2O) remained in the coal matrix.
The degree of demineralization was obtained 90% for both coal
seams [21]. Karaca et al. studied the leaching effect of hydrogen
peroxide (H2O2) on Turkish two lignites (Beypazari and Tuncbilek
103
seam) and Investigated the effect of concentration, contact time
and temperature on the removal of ash and sulfur. They reported
maximum demineralization was achieved from 30 to 70% from lig-
nite coal type [22]. Onal et al. studied six Turkish lignite coal were
treated with HCl or CH3CH2ONa solution at 150 °C. They concluded
from the investigation, HCl treatment was effective demineraliza-
tion but not CH3CH2ONa while effective desulfurization by CH3-
CH2ONa treatment but not HCl [7]. Adeleke et al. reported the
effect of multistage caustic leaching of Nigerian Lafia-Obi coal.
The average ash reduction was achieved 38.66% at low molar con-
centration 1:20 mass reagent (H2O-Na2CO3-H2O) to coal in the
absence of stirring [23].
A literature review revealed that the demineralization of coal
can be improved by chemical leaching process. Several authors’
has been studied the demineralization with low ash coals to gener-
ate ultra clean coal while, in the present investigation we select
high ash Indian coal. Since the Indian coals are high ash content
and the nature of low ash coal is completely different from Indian
coal. In the present communication, an effort has been made to
investigate the effect of alkali concentration and followed by acid
treated on the demineralization of high ash coal by varying leach-
ing temperature and contact time and also particle size. The char-
acterization of raw and leached coal was analyzed by SEM-EDS and
XRF analysis.
2. Material and methods
2.1. Materials
In the present investigation, the coal sample were collected
from Bhubaneswari OCP (Open Cast Project) of Mahanadi Coal
Field (MCL), Orissa. The coals were crushed in a ball mill and sieved
to 16+100 British standard sieves (BSS) mesh size particle, was
used for conducting the experiments. Before the actual start of
the experiment, the coal sample was characterized by using stan-
dard proximate (ASTM D3172 – 13) and ultimate (ASTM D3176 –
15) analysis method. The results are summarized in Table 1. The
chemical reagent used in the present work is the commercially
available sulfuric acid (98% concentration by wt.%) and sodium
hydroxide pellets.
2.2. Experimental set up and procedure
The leaching experiments were conducted in a bench scale unit
consist of a batch reactor of capacity 2.5 L with heating facilities,
condenser provision for reflux and temperature measured by a
thermometer. The batch reactor made up stainless steel reactor
(SS-316) which consist of 0.11 m diameter and 0.22 m height with
Teflon coating inside. The reactor is heated with four heating coils
Table 1
Chemical analysis of coal sample.
Bhubaneswari coal seams
Proximate analysis (wt%, dry basis)
Ash 26.3
Volatile matter 38.7
Fixed carbon 35.0
Ultimate analysis (wt%, daf)
Carbon 52.9
Hydrogen 4.5
Nitrogen 1.5
Sulfur 1.3
Oxygen (by difference) 39.8
Calorific value (kcal/kg) 4632
104 S.K. Behera et al. / Fuel 196 (2017) 102–109

of 1KW capacity each, which fitted outside of the circumference of
the reactor. A stainless steel stirrer is firmed in motor and whose
propeller placed at 0.06 m above from the bottom of the reactor.
A motor moves the stirrer and its speed measured by the sensor
that mounted in front of the motor. The stirrer usually operate at
600–900 rpm. The layout of bench scale experimental setup is
shown in Fig. 1.
For each test, 50 gm of coal (16+100 mesh size) sample was
added to 500 ml NaOH solution of known concentration (50–
150 g/L) in stainless steel reactor at temperature 100 °C for one
hour. The coal slurry was heated from a room temperature to
leaching temperature and maintained constant time. In the second
set of experiments, 50 gm of coal (-16+100 mesh size) was treated
with 50 g/L NaOH concentration of 500 ml solution for 60–120 min
at reaction temperature 65–150 °C. In both stages, the caustic lea-
ched coal is followed by 20% sulfuric acid similar reaction time and
respective leaching temperature. After leaching the hot coal slurry
is cooled, filtered and washed with distilled water for diluting the
concentration of alkali and acid treated coal. The sample is then
dried at 75–85 °C for 3–4 h and weighed. Finally, the ash content
of treated coal was determined by using standard methods (ASTM
D3174 - 12).
3. Results and discussion
3.1. Effect of concentration on demineralization of coal
The caustic concentration has the direct effect on the deminer-
alization of coal and the result depicted in Fig. 2. Up to 100 g/L
NaOH, as the concentration of NaOH increases the percent dem-
ineralisation of the coal increases. Above 100 g/L NaOH increased
concentration of NaOH decreases the percent demineralisation. In
the alkali leaching, the coal containing silica and alumina and other
silica alumina clay bearing minerals may dissolve and formed
sodium silicate and sodium aluminate, which is leached out to
the solution. The following reaction as shown in (1), (2) and (3).
While at higher concentration of alkali solution, the dissolution
of silica and alumina decreases because formation complex sodium
compound called sodium-aluminosilicate. The decrease in percent
demineralization with the increase in alkali concentration is
because the concentration of silicate and aluminate ions exceeds
the solubility product of sodium-aluminosilicate. Several author
also observed similar case as decrease demineralization with
increases alkali concentration [4,15]. In the investigation maxi-
mum percent demineralization was obtained 27% at 100 g/L NaOH

1 Legends

5
1. Fixing Stand
3
2. Batch Reactor
3. Motor and stirrer assembly
6 7 4. Heating Coil
5. Temperature Controller
2
6. Feed Inlet
4 7. Condenser Line
8. Outlet Valve of Reactor
9. Filtration Equipment
8 10. Filtering Plate(Mesh)
11. Filtrate Outlet Valve

10

11

Fig. 1. Experimental setup of bench scale operation for leaching process.

 S.K. Behera et al. / Fuel 196 (2017) 102–109
Fig. 2. Effect of NaOH concentration (g/L) on the coal demineralization.
concentration then it further decreases to 23% with increasing up
to 150 g/L caustic concentration.
2NaOH þ Al2 O3 ! 2NaAlO2 þ H2 O
2NaOH þ SiO2 ! Na2 SiO3 þ H2 O
At higher concentration of alkali solution the following reaction
NaOHðaqÞ þ NaAlO2ðaqÞ þ Na2 SiO3ðaqÞ ! NaX ðAlO2 ÞY ðSiO2 ÞZ NaOH  H2 O
ðSodium-aluminosilicate complex compoundÞ
ð3Þ
The decrease in the extent of demineralization at above 100 g/L
concentration may be due to the adsorption the complex sodium
compound on the reactive site of coal surface and forms film coat-
ing on the coal surface. Although during the leaching process in the
stirred batch reactor, the film layer limited formation and disap-
pear by stirring at desired concentration (up to 100 g/L in this
investigation) but at higher concentration the thickness of film
appear was more important which inhibit the diffusion of leaching
agent to the reactive site of coal and resist the demineralization
process. The mechanism of resistance to diffusion of leaching agent
mainly as shown in Fig 3. It may be also possible during diffusion of
leaching agent up to 100 g/L, then after remaining un-leached min-
erals drifted from the pores and become trapped where resist to
diffusion of leaching agent.
Fig. 3. Mechanism of reaction during leaching process.
105
Most of the insoluble minerals from alkali treated coal, and
residual alkali leached coal was acidified with 20% H2SO4 solution.
As from Fig. 2 revealed that the coal demineralization was
increased from 27.62% to 48%. That may be due to the dissolution
of carbonates, hematite group and sulfide and some insoluble min-
eral from alkali treated coals.
3.2. Effect of contact time and temperature on coal demineralization
The effect of time and temperature is one of the most important
parameters for leaching process. The leaching effect of time and
temperature on percent demineralization of coal for 16+100
mesh size particle with caustic leach and then followed with 20%
sulfuric acid solution as shown in Fig. 4. The graph reveals, the per-
cent demineralization of coal increases with time and temperature
up to the studied range. In the investigation, the maximum dem-
ineralization was obtained 23% and 45% at 150 °C for alkali and fol-
lowed acid leach coal respectively, while less demineralization was
achieved at the lower temperature. The reason for demineraliza-
tion is due to the rise in temperature which enhance the rate of
reaction between the ash bearing mineral matter particles and
leaching agent. The magnitude of demineralization was increased
with temperature while less at low temperature with similar con-
tact time. The reason may be at the higher temperature, the rate of
leaching is faster and lesser time required to the dissolution of
mineral matters.
3.3. Effect of particle size on demineralization
The particle size also affects the demineralization of coal. In this
ð1Þ
investigation, the different coal particle sizes (0.11, 0.181, 0.23,
0.37, 0.75 mm) were treated with 50–150 g/L NaOH solution con-
ð2Þ centration and then acidified with 20% sulfuric acid solution for
one hour at 120 °C. The ash content of raw coal varies with particle
size and the results were shown in Fig. 5. The ash content of raw
coal decreases with increased the particle size while it increased
for treated coal. The reason might be the finer particle size have
larger surface area and easily expose to the leaching agent. The
ash forming mineral matters of finer particles were less gap to dif-
fuse in the leaching agent but in the case of the larger size particles
have minimum exposed surface area and mineral matters itself
trapped in the cavity or pores in the coal matrix. So the liberation
of the mineral is difficult for larger particle size and the exposed
minerals of raw coals directly forming ash after combustion. There-
fore, the decreased the ash percent of raw coal with the increase in
the size of coal particle while the ash content of leached coal
increases with the rise of particle size. It is evident from Fig. 5,
the percent demineralization increases with the decrease particle
size. Fig. 5 consists of two type of plots i.e. for leached coal and
another is for raw coal. For leached coal the demineralization is
slightly increases with increase in particle size, which is due to
the fact that for fine coal less quantity of mineral matters are pre-
sent as a result, demineralization is less. Once the particle size
106 S.K. Behera et al. / Fuel 196 (2017) 102–109
Fig. 4. Effect of leaching temperature and time on the percent demineralization of
coal.
Fig. 5. Leaching effect of particle size on coal demineralization.
increases the surface area is less than smaller particle as a result
demineralization gradually decreases. But for size fraction little
bigger than fines has both high surface area and reasonable
amount of mineral matters, that’s the reason it is showing a peak
for maximum demineralization. Fig. 5 is revised to clearly indicate
which plot is for leached coal.
In this investigation, 60 and 72 mesh particle size was
obtained the maximum percent demineralization around 53%
and 54% for acid followed alkali treated coal while in the case of
the alkali treated coal only 72 mesh particle size was maximum
demineralized. Throughout the investigation, 60 and 72 mesh
particle size is the best demineralization of coal. However, very
fine ground particle (over 100 mesh particle size) were inhibited
to extent of the demineralization. The reason might be the very
finer particles were stick to each other due to greater cohesive
force between the particles (above 100 mesh) and it is difficult to
handling. It also reduces the rate of diffusion of the leaching agent
to the reactive part of the coal and very less yield and also more
time to take for filtration.
3.4. Studies the observation and identification of minerals by SEM-EDS
analysis
The observation and quantification of minerals in the raw and
chemical leached coals was carried out using scanning electron
microscope with energy dispersive X-ray analyzer (SEM-EDS
model JSM5800 from JEOL Company in Japan). SEM sample were
prepared by sprinkling powdered coal sample on to a carbon
coated metallic holder followed gold coating. In this investigation
the surface morphology and the elementary composition of the
mineral group in the raw coal and leached coal was studied. The
SEM micrograph and the EDS analysis of raw and leached sample
were provided in Fig. 6 and Table 2. In the chemical leaching, most
of the minerals are removed and also enrich the carbon content.
Fig. 6 (1) represents the SEM image of the raw coal sample contains
large amount quartz and alumina and the lesser percentage of car-
bon content as well as the small proportion of elements such as
calcium, potassium and sulfur. The SEM micrograph Fig. 6. (2),
(3), and (4) revealed that the carbon content in the coal has been
improved with the percent demineralization. The carbon content
increases from 48% to 68% during the alkali leaching. It also noticed
that the liberation of mineral content drastically changes and the
‘Fe’ content increases with in the caustic treated coal. The libera-
tion of ‘Fe’ increases from the pyrite and hematite group of miner-
als during leaching. The maximum amount of silica (Quartz),
alumina and minerals associated in clay particles were leached
out during alkali leaching. The reason may be due to the presence
of OH (hydroxyl ions) is the high affinity towards the silica and
aluminas. The SEM micrograph Fig. 6. (5), (6), and (7) revealed that
the percentage carbon content improved to 71% (100 g/L NaOH fol-
lowed 20% H2SO4) and silica, alumina and clay bearing minerals
were increased that may be insoluble during acid leach. However,
the surface layer in the SEM image still showing bright and lumi-
nous, that indicating maybe presence of mineral phases.
3.5. Ash composition
The composition of mineral matter as a fraction of oxide was
analyzed by XRF spectrometer (PANalytical Axios FAST XRF spec-
trometer, Japan). The analysis results are summarized in Table 3.
The Fe2O3, Na2O, SO3 content of treated coal was increased in caus-
tic treatment but it is better dissolute in the acid followed alkali
treated coal. On the other hand the SiO2 and Al2O3 content were
increased in combined treated coal while it reduced to above 50%
by alone with caustic treatment by dissolution and formation of
sodium silicate (Na2SiO3) and sodium aluminate (NaAlO2) in the
leaching process. Most of quartz (SiO2) and alumina (Al2O3) were
dissolved during caustic treatment. During the ash analysis, the
red colored ash was found in the caustic treated coal, that may
be due to the presence of Fe2O3 (Hematite) and Na2O and other
minerals while white colored ash was found due to presence of
large content of silica and alumina in the combined treated coal.
 S.K. Behera et al. / Fuel 196 (2017) 102–109 107

Fig. 6. SEM analysis of (1) Raw coal (2) 50 g/L NaOH (3) 100 g/L NaOH (4) 150 g/L NaOH treated coal and 20% sulfuric acid followed by (5) 50 g/L NaOH (6)100 g/L NaOH (7)
150 g/L NaOH treated coal.

3.6. Calorific value
The calorific value of coal (moisture free basis) was deter-
mined by high pressure oxygen Bomb calorimeter (LECO AC
500). The calorific value (C.V) of coal is one of the most impor-
tant indexes in assessing the quality of coal. The calorific value
of coal increased ranging from 4631.5 kcal/kg to 5241.7 kcal/kg
for alkali leached coal which increases to 6733.3 kcal/kg for acid
treated coal. The increase these value found to be 13% and 45%
of the alkali and followed acid treated coal respectively. The
maximum calorific value was found in the acid followed by
alkali treated coal as compared to alkali treated and raw coal.
The reason might be soluble of non-carbonaceous mineral mat-
ters by the chemical treatment, which have no heating value.
The composition of calcite (Carbonaceous group) is the main fac-
tor for affect the calorific value of coal [24].
108 S.K. Behera et al. / Fuel 196 (2017) 102–109

Table 2
EDS analysis of coal samples.

Element (wt.%) Raw coal NaOH concentration (g/L) NaOH (g/L) followed by 20% H2SO4
50 100 150 50 100 150
C 48.95 65.23 68.38 65.85 67.24 71.13 70.1
O 36.48 24.24 22.69 16.51 18.72 20.24 19.0
Mg 0.13 0.38 0.42 0.51 0.7 0.01 0.05
Al 4.29 1.88 1.22 3.15 3.21 1.63 3.44
Si 9.16 5.78 3.35 8.51 7.73 4.23 5.7
S 0.22 0.27 0.62 0.4 1.35 1.46 1.05
K 0.2 0.12 0.2 0.96 0.02 0.41 0.12
Ca 0.08 0.32 0.08 0.69 0.23 0.12 0.01
Ti 0.3 0.37 0.12 0.99 0.16 0.16 0.24
Mn 0.04 0.06 0.09 0.03 0.06 0.07 0.06
Fe 0.15 1.25 2.65 2.4 0.08 0.54 0.21

Table 3
Ash analysis of coals.

Coal seams Coal type Ash composition (wt.%)

SiO2 Al2O3 Fe2O3 CaO MgO Na2O K2O SO3
Bhubaneswari Raw coal 44.51 20.12 3.67 1.45 0.98 0.15 0.97 0.741
NaOH 22.70 7.67 3.93 1.24 0.52 17.96 0.756 5.94
NaOH followed H2SO4 55.38 11.27 1.70 0.16 0.75 1.44 1.66 0.22

4. Conclusions solution at varying process conditions before such conclusions

The current study contains a detailed investigation of the effect
of concentration of alkali and acid followed alkali leached coal,
reaction temperature and time and the effect of coal particle size
on the percent demineralization for high ash coal. The observation
from the present investigation concludes following details.
1. The better generation of clean coal by leaching is possible when
the process conditions are properly selected. The extent of dem-
ineralization depends on the increasing the solvent concentra-
tion, temperature and leaching time and decreasing the size
of particles.
2. The extent of demineralization increased with increase alkali
concentration, and then it decreases with increase in alkali con-
centration due to the formation complex sodium compound,
which resist further demineralization process.
3. The combined treatment method depicted the maximum per-
cent demineralization of coal. In the investigation was shown
27% and 48% demineralization was achieved by alkali and acid
followed alkali treated coal from 26% ash of Bhubaneswari coal
seam.
4. The decreased in size of coal particles with increases the extent
of demineralization. Throughout in the investigation, 60 and
72 mesh size particle has been found the most effective dem-
ineralized by leaching process. The percent demineralization
was obtained up to 53% and 54% for these coal particle size by
the combined treatment methods.
5. The percent demineralization increases with increase in reac-
tion temperature and residence time up to the studied range
in the experiment.
6. It has been observed that in the SEM/EDS analysis, above 50%
minerals leached out in the present investigation.
7. The calorific value of coal increases with the extent of deminer-
alization. The reason behind the non-carbonaceous matter and
residual minerals were in eluate and also the increased the car-
bon content of the treated coal by the leaching method.
However, more investigations are required for upgrading the
low grade coal by leaching with other than NaOH and H2SO4
are can be generalized.
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