Mineral Processing and Extractive Metallurgy Review

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Removal of ash from low grade Indian coal by

chemical leaching technique

Sushanta K. Behera, Sudipto Chakraborty & B. C. Meikap

To cite this article: Sushanta K. Behera, Sudipto Chakraborty & B. C. Meikap (2018) Removal of
ash from low grade Indian coal by chemical leaching technique, Mineral Processing and Extractive
Metallurgy Review, 39:1, 59-67, DOI: 10.1080/08827508.2017.1391247

To link to this article: https://doi.org/10.1080/08827508.2017.1391247

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 MINERAL PROCESSING AND EXTRACTIVE METALLURGY REVIEW
2018, VOL. 39, NO. 1, 59–67
https://doi.org/10.1080/08827508.2017.1391247

Removal of ash from low grade Indian coal by chemical leaching technique
Sushanta K. Beheraa, Sudipto Chakrabortya, and B. C. Meikapab
a
Department of Chemical Engineering, Indian Institute of Technology (IIT), Kharagpur, India; bDepartment of Chemical Engineering, School of
Engineering, Howard College Campus, University of Kwazulu-Natal (UKZN), Durban, South Africa

ABSTRACT KEYWORDS
In this work leaching of low grade Indian coal was investigated. Coal samples of pre-treated and treated Low grade coal; removal of
were characterized to quantify the quality of coal. An attempt has been made in this work to reduce the ash; leaching; mineral
mineral matter from low grade coal of particle size 250 μm by leaching with H2SO4, HCl, Na2CO3 and matter; chemical leaching;
up-gradation of coal
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NaOH solution as leaching agent at a temperature of 100°C for 3 h. It was found that the final ash
content of treated coal was 22% from 38% of ash of feed raw coal by NaOH treatment alone compared
to rest of the solvents.

Introduction and inorganic) more effectively than physical methods

(Ryberg et al. 2015). Usually, less than 30% ash content in
It is necessary to explore chemical leaching of low rank coal
coal which is achieved by coal cleaning may avoid problems
(LRC), because of the depletion of high rank coal and crude
connected to efficiency of combustion, gasification and to
oil in earth crust, which is the major source of energy in the
minimize the emission of airborne pollutants in the environ-
world. The use of LGCs is the major cause of environmental
ment (Meshram et al. 2015).
pollution due to the generation of large amounts of fly ash,
The main purpose of chemical cleaning of coal is to
bottom ash, and other pollutants. The common pollutants
remove the mineral matters without affecting the organic
associated with the activity of coal power stations are different
structure of the coal matrix. During the leaching process
sizes of particulate matter (PM), ozone (O3), SO2, NOx, car-
the major minerals in the coal like kaolinite, silica, carbo-
bon monoxide (CO), metals and volatile organic compounds.
nate, and sulphur bearing minerals are removed from the
It is therefore important to clean the coal before using it in
coal and then dissolute in the acid or alkali solution. The
thermal power stations, steel plants, cement industries etc.
effective demineralization depends on the type and amount
The low-grade coals are inherent characteristic with limited
of mineral constituent present in the coal (Sharma and
utilization, because it contains high mineral matters and
Gihar 1991; Yang et al. 1985). The coal demineralization
moisture content. The presence of high minerals in the coal
(ash removal) by treatment with aqueous fused sodium
has detrimental effect of combustion, gasification, carboniza-
hydroxide alone or followed by minerals acids has been
tion, and liquefaction processes (Bolat et al. 1998 Mukherjee
reported by many researchers (Kumar and Shankar 2000;
and Borthakur 2003; Dash et al. 2013). Although the low
Balaz et al. 2001; Mukherjee and Borthakur 2001, 2004;
grade coal are low cost fuel and help to improve the energy
Ratanakandilok et al. 2001; Shakirullah et al. 2006; Nabeel
security issue, their use in existing coal preparation units is a
et al. 2009; Saydut et al. 2011; Wijaya et al. 2011; Behera
great challenge. Therefore, prior to utilization of such coal,
et al. 2017). The chemical cleaning of coal is applicable to
beneficiation by different methods is essential. The drift origin
LGCs or high-ash coal which removes ash bearing minerals
of the Indian coal possesses high ash content of the order of
of both organic and inorganic minerals more efficiently as
30 to 40%. Commercially the beneficiation method of coal is
compared to physical methods. Due to this, chemical clean-
done by the physical methods and the magnitude of the
ing of coal is an alternative technique to physical cleaning,
cleaning depends on specific gravity and surface properties
allowing for achieving the efficient ash removal method
of minerals associated in the coal structure. Generally the
that cannot be achieved in the physical cleaning.
physical methods like gravity separation and froth flotation
Literature survey revealed that chemical cleaning of coal
which are relatively low ash removal techniques. In spite of
has a great potential for better mineral matters ash removal
the physical properties of minerals, these methods are not
from the coal. Chemical cleaning methods have not widely
suitable to remove the organic minerals and the inherent
employed at a commercial scale due to huge cost related to
ash in the coal matrix. In contrary, the chemical cleaning
the requirements of chemicals and the need for dewatering
using acid, alkali or acid-alkali leaching techniques are applic-
of the post-demineralization and regeneration of reagents
able to low grade coal which removes minerals (both organic

CONTACT B. C. Meikap bcmeikap@che.iitkgp.ernet.in Department of Chemical Engineering, School of Engineering, Howard College Campus, University of
Kwazulu-Natal, Durban, South Africa.
Color versions of one or more of the figures in the article can be found online at www.tandfonline.com/GMPR.
© 2017 Taylor & Francis Group, LLC
 60 S. K. BEHERA ET AL.
from spent solution (Wu and steel, 2007; Meshram et al.
2015; Ryberg et al. 2015; Sriramoju et al. 2017). The che-
mical leaching process is unattractive because the cost of
the chemicals is more although the leaching process is
simple and it operates under mild temperature and atmo-
spheric pressure. The different methods have been devel-
oped for regeneration, recovery, and recycling of both alkali
and acid spent solution. In the chemical leaching methods,
the spent alkali solution can be regenerated by reacting
with lime, whereas acid can be regenerated by treating
with gypsum. The reactions (1), (2) and (3) occur during
the regeneration of chemical reagents.
Na2 SiO3 þ H2 SO4 ! H2 SiO3 þ Na2 SO4 (1)
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Na2 SiO3 þ CaðOHÞ2 ! 2CaSiO3 þ 2NaOH (2)
H2 SiO3 þ CaSO4 ! CaSiO3 þ H2 SO4 (3)
Regeneration of spent alkali and acid reduces the cost of
chemicals in the cleaning method. The spent solution which
contain not only silicate and aluminates but also contains Fe,
Al, and trace elements of Zn, Cr, Mn, Ni, Cu, Ba, Ti etc.
(Nabeel et al. 2009; Sriramoju et al. 2017). In addition to the
chemical leaching, other method also used for demineraliza-
tion or desulphurization that is bioleaching can remove the
inorganic sulphur bearing minerals from coal. However, this
method is very complex in nature (Malik et al. 2001).
The literature review revealed that the ash was removed
efficiently by the chemical treatment method. The novelty of
the present research is to enhance the coal quality and finding
the effect suitable chemical solvent which can efficiently
remove the mineral matter from LGCs. Therefore, the LGCs
were treated with various aqueous solutions of sodium hydro-
xide, sodium carbonate, sulphuric acid and hydrochloric acid,
which subsequently reduce the ash contents. In addition to
this, characterization of the pre and post treated coal was
performed by XRD, FTIR and FESEM to identify the presence
of minerals phases, changes in mineral bands, coal composi-
tion and the modification of exposure coal surface during
leaching process.
Materials and method
Materials
For the leaching study, the coal sample was selected from
Jagannath mines of Mahanadi Coalfield Limited (MCL),
Odisha, India. The coal sample was crushed and sieved in
British Standard Sieve (BSS) mesh size to collect 250 µm size
of coal particles and preserved in desiccators before the start
of experiments to avoid environmental contaminates. The
commercial grade chemical was used for leaching study. The
standard chemical reagents or solvent was Sulphuric acid
(98%), Hydrochloric acid (35%), Na2CO3 and Sodium hydro-
xide (NaOH). These solvents were diluted with distilled water
as per requirements for leaching study.
Table 1. Chemical analysis of Jagannath Coal.
Proximate analysis (wt%, on dry basis)
Moisture 2.3
Volatile matter 28.6
Fixed carbon 30.8
Ash 38.3
Ultimate analysis (wt%, on dry ash free basis)
C 42.25
H 3.105
N 2.1
Sa 0.82
Ob 51.725
Calorific value (kcal/kg) 4450
a
Combustible Sulphur, bBy difference
Chemical analysis of coal
The pre and post treated coal samples were analyzed for
physicochemical characterization. The ultimate analysis of
coal (C, H, N, and S) samples was carried out using elemental
(CHNS/O) analyzer (EL Vario MICRO Cube, Elementar TM)
according to ASTM D5291 standard technique. The free oxy-
gen contents of samples were calculated by difference.
Similarly, the proximate analysis was examined using
American Society for Testing and Materials (ASTM) D3173,
D3174 and D3175 standard techniques for moisture, volatile
matter and ash content respectively and fixed carbon was
determined by difference. The chemical analysis of raw coal
was shown in Table 1.
Experimental method
The leaching experiments were carried out in the laboratory
scale as well as bench scale experimental set-up. The labora-
tory leaching setup assembly consists of a three necked round
bottom flask with capacity 1000 ml, where a stirrer is fitted
with the motor at the center of the reactor assembly. The
speed of the stirrer up to 500–600 rpm is regulated by the
motor. A condenser is connected to one of the other two
necks which are connected to a conical flask for collecting
condensate formed by trapping the volatile gases generated
during the reaction. During the leaching process reflux must
be recycled to avoid evaporation loss of the solvent. The third
neck is used for adding the reagents using a dropping funnel
and also the monitor temperature of the reaction bath using a
thermometer. The rotamantle (heating element) is the source
of heat input to the system to raise the reaction temperature
and the temperature was controlled through a variable power
regulator.
The bench scale leaching experiments were conducted in a
batch reactor of capacity 2.5 L with heating facilities, condenser
provision for reflux and temperature measured by a thermo-
meter. The batch reactor made up stainless steel reactor (SS-
316) with inside teflon coating. The reactor is heated with
heating coils, which fitted outside circumference of the reactor.
According to respective chemical characteristics of reagents, a
stainless steel or teflon stirrer is fitted with the motor. The
propellers are placed at 0.06 m from the bottom of the reactor.
A motor rotate the stirrer and its speed is measured by a sensor
that mounted in front of the motor. The stirrer usually operates
at 600–900 rpm. The photographic view of fine coal samples
 MINERAL PROCESSING AND EXTRACTIVE METALLURGY REVIEW 61

and the laboratory experimental set-up and bench scale leaching
experimental set-up is shown in Figure 1 and Figure 2. For the
leaching study, each experiment was carried out with 20 g coal
of 250 μm particle size treated with 200 ml of 5, 10, 20, and 30%
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by wt% of NaOH, Na2CO3, and above concentration range by
vol% of H2SO4 and HCl solution at 100°C for 3 h. After sub-
sequent leaching, the treated coal sample was washed with
distilled water for diluting the solvent and filtered in

Figure 1. Schematic diagram of experimental set up for leaching study.

5 3
Legends

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

10

11

Figure 2. Experimental setup of bench scale operation for leaching process.

 62 S. K. BEHERA ET AL.

polypropylene funnel by using Whatmann filter paper. The
residual wet coal dried in a hot air oven at 90ºC for 2–3 hrs.
Finally the ash analysis of coal has been carried out.
XRD analysis of coal
The coal samples were collected from the samples generated
during the experimentation. The coal samples were analyzed
by X-ray Diffraction (XRD) using PANalytical High
Resolution X-ray Diffractometer and a Cu k-alpha radiation
from 10 to 85°, 2θ, with a 0.02 step. This instrument works on
the principle of Bragg’s law, nλ = 2d sinθ. After X-ray scan-
ning of the samples, mineral peaks were identified using
X’Pert High Score Plus software.
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acid powder and 4 gm of powder coal sample was filled in. The
mixture was then pressed into a pellet on a hydraulic pelleting
machine. Finally, the pellet used for determined the composition
of mineral matters present in the coal by spectrometer.
Results and discussion
Effect of concentration of acid and alkali on ash removal
from the coal
The effect of different acid and alkali concentration on ash
removal from coal as shown in Figure 3. The caustic concen-
tration has significant effect on the de-mineralization of coal
rather than acid treatment. Sodium carbonate was less reac-

tive to the minerals in the coal while the caustic treatment is

FTIR analysis of coal more effective to remove the minerals like kaolinite, calcite
and inorganic sulphur minerals. Similarly, the sulphuric acid
FTIR (Fourier Transform Infrared) spectroscopy is a powerful
and hydrochloric acid leaching effect of coal minerals was
tool for the characterization of coal and its products which sig-
significant. Both the acid reduces the ash content of the coal
nifies the comprehensive view about the structure/composition of
after treatment. It has been observed that in the leaching
the minerals in the coal matrix. Infrared (IR) spectroscopy is the
process, with increase in reagent concentration, the de-miner-
study of interactions between the mineral matters and electro-
alization of coal increases. The leaching effect of sulphuric
magnetic fields in the IR region. The probability of a particular IR
acid alone is less reactive to silica and clay minerals while the
frequency being absorbed which depends on the actual interac-
hydrochloric acid was significantly recitative and reduces the
tion between the frequency and the molecule. The spectrum in
mineral constituents from the coal. The minerals matter such
the FTIR analysis mainly presented as transmittance versus wave
as carbonates, Fe2O3, and sulfides are removed during the
number (cm−1). The presence of functional group and bonding
acid leaching. Removal of mineral matters from coal by acid
characteristic of the raw and leached coal were determined
treatment is not much effective. This is due to the fact that,
through FTIR measurements using a Nicolet NEXUS-670 FTIR
the major minerals (kaolinite, quartz) are not effectively react-
instrument. The measuring region within the range of
ing with acidic solution. As these are less soluble in the acidic
4000–400 cm−1 wave number. In the presence of baking lamp,
treatment. NaOH pretreatment alone has extensive effect on
approximately 1 mg of ground coal sample was properly mixed
removal of mineral matters from the raw coal. It is interesting
with 100 mg of dried KBr powder, and then it was grounded by
to note that in comparison with raw coal sample, the de-
pestle with mortar to avoid moisture absorption. The mixture was
mineralization of coal is enhanced with increase in the con-
pressed into a pellet on a hydraulic pelleting machine. The soft-
centration of chemical solvents. The maximum ash reduction
ware used for data processing and spectral analysis are obtained.
by the caustic leaching effect from original coal was found to
about 42% (deashing, 22%) than the acidic treatment. The ash
FESEM/EDS analysis of coal content of leached coal reduced to 24% and 26% for hydro-
The Scanning Electron Microscopy coupled with Energy
Dispersive X-ay (SEM-EDX) analysis were used to determine
the nature of mineral matter present in the pre and post-treated
coal samples by Field Electron Scanning Electron Microscope
(FESEM) model JEOL JSM-7610F, Japan. SEM samples were
prepared by sprinkling powdered coal sample on to a carbon
coated metallic holder followed by gold coating. The reason
behind for gold coating due to the conducting behavior of coal
samples.

XRF analysis of coal

X-ray fluorescence (XRF) spectrometry is a rapid technique for
accurate and precise elemental analysis of solid and liquid sam-
ples. The elementary composition of mineral matter in the coal
was analyzed by XRF spectrometer (PANalytical Axios FAST XRF
spectrometer, Japan). A sample was prepared by thoroughly mix-
ing 4 gm of coal mixing with 2 gm of boric acid powder in a
cylinder type dies. The pelletization was done by hydraulic pressed
powder method. In an aluminum cylindrical die, 2 gm of boric Figure 3. Effect of reagent concentration on the removal of coal ash.
 MINERAL PROCESSING AND EXTRACTIVE METALLURGY REVIEW 63

chloric and sulphuric acid treated coal while limited ash was
reduced to during the sodium carbonate treated coal.
The mineral matters is reduced at higher concentration
caustic leaching may be due to the high affinity of hydroxyl
(OH−) ion, which attack the mineral rich materials of coal.
Major constituents of alumina and silica from clay and other
silica bearing minerals reacted during alkali leaching, which
formed soluble sodium compounds of silicate and aluminate
as per following reaction mechanism as shown in equations
(4) and (5). In addition, the alkali (Baruah and Khare, 2007)
and acid (Onal and Ceylan, 1995) also react with sulphur
minerals. The sulphur present in the coal react less with alkali
in comparison to acidic treatment. The alkali react with sul-
phur minerals (pyrite) forming soluble sulfates and which also
react with organic sulphur was shown in reactions (6), (7), (8)
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and (9). The following reactions occur during the leaching

process.
2NaOH þ SiO2 ! Na2 SiO3 þH2 O (4)

2NaOH þ Al2 O3 ! 2NaAlO2 þH2 O (5)

Na2 S þ 2H2 O ! 2NaOH þ H2 S (6)

Na2 S þ 2H2 O ! 2NaOHþH2 S (7)

RSH þ 2NaOH ! Na2 S þ 2H2 O þ R0 CH ¼ CH2 O (8)

30NaOH þ 8FeS2 ! 4Fe2 O3 þ14Na2 S þ Na2 S2 O3 þ15H2 O
(9)
Characteristic studies of coal
Qualitative analysis of feed and leached coal samples
using XRD technique
XRD patterns are presented in Figure 4a–4e for the pre and
post treated coal samples. A qualitative analysis of the var-
ious minerals present in the coal was identified in the XRD
plots. From the software, the diffraction peak was searched
and matched to identify the crystalline components like
quartz or silica (SiO2), Kaolinite (Al2Si2O5 (OH)4), and
Hematite (Fe2O3). The raw coal associated with major com-
ponents like silica, kaolinite minerals, and low hematite
(iron bearing) minerals; which revealed from the Figure 3a.
It has also been found that there are other minerals (very
low peak) bound to the coal structures which are concealed
in the pore. The concealed minerals are leached with the
treated solvents, which causes the liberation of minerals
from the coal matrix as shown in Figure 4b–4e. Several
author reported the various mineral phases present in the
coal sample and which considered as the basis for analysis
(Steel et al. 2001; Dash et al. 2015). Also in XRD, 2θ value of
the mineral phases like quartz and hematite refer to JCPDS
card number 46–1045 and 89–0597 respectively. From the
Figure 4a it has been observed the various minerals peaks
found in the raw coal. The major mineral peaks correspond-
ing to quartz, kaolinite and low peaks corresponding to
hematite mineral groups. The minerals species of original
raw coal sample of the peak corresponding kaolinite 2θ
value at 12.35°, 22.5°, 27°, for quartz 2θ value at 26.64°,
39.438°, 59.804°, 67.718° and for hematite 2θ value at
Figure 4. XRD analysis of (a) Raw coal and 30% of (b) Na2CO3 (c) H2SO4 (d) HCl
(e) NaOH.
39.935°, 55.17°, 62.377°. The leaching effect causes the lib-
eration of minerals which changes the 2θ values of the
mineral species. The mineral phases corresponding to hema-
tite, 2θ value at 39.935°, 55.17°, 62.377° of raw coal shifted
to 33.11° and 54° for treatment with 30% of Na2CO3. Raw
coal samples treat with 30% HCl and H2SO4 found to
develop very low intensity peaks. Similar observation was
also found in case of alkali treatment and it changes the 2θ
value to 43.47°. The shifting of 2θ value during acidic treat-
ment is due to the solubilization of hematite minerals pre-
sent in the raw coal. It has been observed from Figure 4e
that, after 30% caustic treatment of coal, the intensity of
peaks reduces, and develops new peaks of 2θ from 27° to
25°. The peak intensity of clay bearing mineral species
gradually decreases by the acid and alkali leaching process.
FTIR analysis of coal
To access the presence of functional groups in the raw and
leached coal sample, FTIR analysis was performed. The
respective transmittance value at particular wavelength sig-
nifies the presence of the functional groups. However, several
functional groups may absorb at the same frequency range,
and a functional group may have multiple-characteristic
absorption band, especially for 1500–650 cm−1, which is called
the fingerprint region. The detection of the most prominent
band of FTIR spectra of coal samples is presented in Table 2.
 64 S. K. BEHERA ET AL.

Table 2. Wave number assigned of most prominent corresponding band in the bands in between 400and1100 cm−1 wave numbers are mainly
FTIR spectra of coal samples. (Georgakopoulos et al. 2003; Dash et al. 2015;
Saikia et al. 2007).
assigned to inorganic minerals present in the coal. The major
minerals attributed in the band in between 1035 and
Band position (cm−1) Assignments of bands
1080 cm−1 are belongs to kaolinite, quartz, and montmorillo-
3619–3699 Clay minerals (Kaolinite and illite)
3400–3416 -OH stretching nite in the coal. These bands are less observed in case of alkali
3300 Stretching – OH groups treatment as shown in Figure 5e. Thus, FTIR studies revealed
2921–3392 Aliphatic C-H groups
1612–1622 C = C aromatic stretching and carboxyl groups the presence of major silica mineral like quartz, clay minerals
conjugated (aluminium silicates, illite, and kaolinite) in the coal samples.
1440–1450, 1500 Bending C-H aliphatic, stretching C-C aromatic The background of band intensity reduces for inorganic
1115–1118 C-O, C-O-R structure
1031–1095 Silicates (Si-O), Kaolinite Quartz, Montmorillonite minerals due to leaching effect. This signifies the removal of
779, 799 Quartz ash bearing minerals from coal during the leaching process.
528–536 and Clay and Silicates minerals
466–472
SEM-EDX analysis of coal
In order to find the elementary composition and surface
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Figure 5a–5e, represents the FTIR spectra for the leaching

morphology of coal before and after treatment SEM – EDX
effect on the coal mineral and organic macerals. The wave-
analysis was carried out as shown in Figures 6 and 7. The
number is in the range of 3618 to 3628 cm−1. The wavenum-
minerals are associated in the coal matrix in different forms
ber in the range of 3696 to 3699 cm−1 represents kaolinite and
such as dissolved salts, exchangeable ions, organometallic
other trace minerals. Similarly, the bands at 528–535 cm−1
complexes and discrete crystalline mineral particles. SEM-
and 466–472 cm−1 attributed clay and silicate minerals respec-
EDX study analyzing the composition of minerals, and iden-
tively. The bands at 3402–3416 cm−1 are corresponding to –
tify the different forms of minerals in the coal matrix. During
OH stretching group. The region of bands in between 3000
the experimentation, minerals like silica, kaolinite, montmor-
and 2800 cm−1 indicate aliphatic stretching C-H groups. In
illonite and pyrites (inorganic sulphur) are dissolved into the
between the bands at 1618–1622 cm−1 attributed the oxygen
alkali solution. The EDX results revealed from the Figure 7
containing functional groups. The wave number at
that, the silica, alumina and clay bearing mineral decreases
1032–1047 cm−1 related to silicate minerals (Si-O bonds).
significantly by the effect of alkali leaching as compared to
The band observed from the analysis corresponding to
acid leaching. The clay minerals are easily dissolute in sodium
1165 cm−1, 799 cm−1, and 779 cm−1 are for quartz. The
carbonate pretreatment, where as clay content increases dur-
ing the acidic treatment.
From the EDX analysis (Figure 7) it has been found that the
sulphur minerals like pyrite and organic sulphur was dissolute
with acid solution. The carbon content of leached coal increases
from 44% to 76% for alkali treatment and 70% for both sulphuric
acid and hydrochloric acid treatment. However, in case of
sodium carbonate treatment, there is not much change. The
sulphur content of coal drastically reduces during the leaching
process. Similarly, the hematite minerals in the original coal are
less dissolute in caustic leaching and it is soluble in acid solu-
tions. The SEM micrograph (Figure 6) shows the minerals were
uneven distributed and present in the cluster form. It has been
found from Figure 6 that, the leaching reagents react with the
minerals in the micropores as well as surface of the coal.
Therefore, the porosity of coal is increases which resulted in
liberation of mineral matters from raw coal due to leaching effect
of reagents. It has been also observed that the carbon content of
treated coal increases by the leaching effect that signifies the
leaching solvent dissociate the minerals by attacking the coal
matrix and concealed minerals in the coal structure. However,
The SEM micrograph of coal surface was still showing luminous
and bright which signifies may be the presence of mineral phases
coated with it.

XRF analysis of coal

The mineral matters present in the coal are not uniformly
distributed as a result chemical and physical properties (like
Figure 5. FTIR analysis of (a) Raw coal and 30% of (b) Na2CO3 (c) H2SO4 (d) HCl density, composition) are different. Mostly the trace element
(e) NaOH. content in the coal is associated with major minerals like
 MINERAL PROCESSING AND EXTRACTIVE METALLURGY REVIEW 65
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Figure 6. FESEM analysis of (a) Raw coal and 30% of (b) Na2CO3 (c) H2SO4 ((d) HCl (e) NaOH.

pyrites, kaolinite and illite. The ash forming behavior of

mineral phases in the coal varies with cleaning methods.
Trace elements (Zn, Cr, Mn, Ni, Cu, Br, Y, Zr, Nb, Ge, Ba,
Bi, Sr, Cs, Ga, Pb, Ce) present in coal and major elements (Na,
Mg, Al, Si, P, S, Cl, K, Ca, Ti, Fe) in coal were determined in
X-ray fluorescence spectrometry. The trace and major element
analysis reports are presented in Tables 3 and 4. Trace ele-
ments present in the coal plays an important role for forma-
tion ash clickers after burning. The degree of ash content
depends on the concentration of trace elements as well as
major minerals contents of the coal. It has been observed
that due to acid/alkali treatment, release of trace elements
found. The results of trace elements are presented in Table 3
and it has been observed from Table 3 that, the trace elements
Zn, Ba, Cu are increased in the treated coal due to leaching of
sodium carbonate, HCl and H2SO4 as compare to raw coal
while most of trace element reduced during the NaOH leach-
ing. It can be seen from Table 4 that, the major elements in
Figure 7. EDS analysis of coal. the raw coal increases or decreases by the leaching effect as
 66 S. K. BEHERA ET AL.

Table 3. Trace element concentrations (ppm) in coal samples. investigation shows the major minerals were removed by the
Elements Raw coal 30% Na2CO3 30% H2SO4 30% HCl 30% NaOH leaching effect. The minerals associated with the coal contain-
Zn 120 980 1270 2690 – ing carbon have been removed by the leaching effect, which
Cr 300 300 – – 150
Mn 480 460 – – –
increases from 44% to 76% by the caustic leaching effect.
Ni 380 270 0.041 – 60 FTIR results showed that, lowering band intensity of mineral
Cu 660 610 770 3730 120 bands of the leached coal with respect to raw coal which
Br 830 – – – –
Y 100 100 – – 50 represents the improvement of the coal quality. XRD analysis
Zr 890 930 450 1210 540 revealed that associated mineral groups in the pre and post
Nb 120 – – – 20
Ge – 430 – – – treated coal are of different phases. Chemical leaching tech-
Ba – 1620 1430 2970 – niques thus effectively reduce the minerals from LGCs which
Bi – 0 – – – minimizes the environmental pollutants and produce less
Sr – 340 – – 120
Cs – – – 730 – quantity of ash during its utilization in the boiler of coal
Ga – – 570 – – fired thermal power plants. Therefore, these methods can be
Pb – – – – 420
Ce – – – – 220 used as alternative methods to reduce the mineral matter from
the LGCs or thermal coal which can be upgraded to high
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quality coal.
Table 4. Major element concentration (wt %) in coal samples.
Elements Raw coal 30% Na2CO3 30% H2SO4 30% HCl 30% NaOH
O 42.720 43.7 50.516 45.382 49.52 Disclosure statement
Na 1.887 9.455 0.887 0.293 16.89
Mg 0.348 0.265 0.125 0.097 0.21 The authors report no conflicts of interest. The authors alone are
Al 11.429 10.69 7.864 7.726 5.31 responsible for the content and writing of the article.
Si 22.494 21.37 27.925 27.909 16.25
P 0.201 0.158 0.02 0.015 0.15
S 2.041 2.45 7.062 3.463 1.56
Cl 8.228 0.502 1.155 8.66 0.89 Funding
K 0.990 0.961 0.928 0.801 0.86
Ca 0.838 0.631 0.161 0.122 0.77 This work was supported by Chemical Engineering Department, Indian
Ti 1.342 1.449 1.807 1.77 0.829 institute of Technology, Kharagpur.
Fe 7.092 7.752 1.054 2.628 6.59

the coal samples are identical in mineral matter distribution
but not the same. The effective separation of specific elements
to corresponding minerals depends on the degree of chemical
treatment. The major element (like Si, Al) of raw coal reduces
after caustic leaching. However, Fe, Na, K, Ca contents in the
leached coal were increased by alkali treatment. These ele-
ments are not easily dissolute during alkali leaching while
these are reduced by the sulfuric acid treatment. On the
other hand the Si, Al, Mg contents are increases in acid
treated coal.
Conclusion
The effect of chemical reagents (aqueous solution of NaOH,
Na2CO3, HCl,and H2SO4) at different concentration on the
LGCs for removal of mineral matters and characterization of
pre and post treated coal was studied. From the detailed
experimental investigation, it has been found that, alone caus-
tic leaching resulted in maximum reduction of the mineral
matters from LGCs as compared to acidic treatment.
Significantly elimination of the silica, alumina and the pyritic
sulphur was observed during the alkali leaching, as well as
substantial reduction in the ash from the coal. The degree of
ash reduction was obtained as 42% (leached coal ash content
22%) by the caustic treatment from the raw coal of 38% ash
content. The removal of mineral constituents (like sulphur,
quartz, clay minerals) from LGCs would reduce the fouling,
corrosion and erosion in the process units. The leaching
agents removed the mineral rich constituents without affect-
ing the original carbon content of the coal. SEM-EDX
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