Energy Conversion and Management 43 (2002) 885–895

www.elsevier.com/locate/enconman

Demineralization and desulfurization of coals via column

froth flotation and different methods
Ayhan Demirbasß *
Department of Chemical Education, Karadeniz Technical University, P.K. 216, TR-61035 Trabzon, Turkey
Received 3 January 2001; accepted 25 April 2001

Abstract
Coals are heterogeneous, complex and noncrystalline macromolecules containing both organic and in-
organic materials. Inorganic materials of coal contain a number of inorganic constituents, especially sulfur,
which plays an important role in almost all coal utilization systems. Some techniques have been applied to
coal to remove its inorganic materials from the organic part. One of the most suitable methods is froth
flotation for removal of pyritic sulfur from coal. By this method, high sulfur removal from lignite was
possible. Alkali desulfurization and oxidesulfurization also are effective applicable methods for high sulfur
coals.
2002 Elsevier Science Ltd. All rights reserved.

Keywords: Coal; Desulfurization; Froth flotation; Pyritic sulfur

1. Introduction

Lignite is the most important source of energy in Turkey, and the average sulfur content of
Turkish lignites is relatively high. Turkish lignite, or brown coal, contains about 3–12% sulfur in
the form of inorganic and organic compounds. Pyrite is the major inorganic sulfur compound in
coal.
Existence of sulfur compounds in coal limits its industrial application due to environmental
as well as technical problems. However, high sulfur coals can be upgraded by desulfurization
through physical, chemical and biotechnological processes. One of the most suitable methods is

*
Tel.: +90-462-248-7429; fax: +90-462-248-7344.
E-mail address: ayhandemirabas@hotmail.com (A. Demirbasß).

0196-8904/02/$ - see front matter
2002 Elsevier Science Ltd. All rights reserved.
PII: S 0 1 9 6 - 8 9 0 4 ( 0 1 ) 0 0 0 8 8 - 7
886 A. Demirbasß / Energy Conversion and Management 43 (2002) 885–895

froth flotation for removal of pyritic sulfur from coal [1]. In Turkey, combustion of high sulfur
lignite is one of the fundamental reasons for the problem with sulfur dioxide emissions.
Mineral matter is an undesirable component of coal, and it affects mining, benefaction,
transformation and combustion of coal. Problems related to the commercial use of a coal are
usually due to its mineral matter content. The problems are often associated with the deposits in
boilers, as slagging, fouling, clinker and ash, decreasing thermal efficiency. Mineral matter also
affects the conversion products of coal into gaseous or liquid fuels [2–6]. The process described by
Gorin [7] relates to a method for removing ash, i.e. mineral contaminants and the like, from ash
containing coal extract prior to catalytic hydrogenation. In this process, ash containing extract,
obtained via solvent extraction of coal, is deashed in the admixture with a hydrogen transferred
hydrocarbonaceous liquid at a temperature that is at least as high as the temperature at which
hydrogen is transferred from the liquid. Normally, hydrogen is not transferred below 525 K. The
temperature at which hydrogen is transferred is referred to as the hydrogen transferring tem-
perature. The resulting demineralized extract is subsequently catalytically hydrogenated to yield
the desired hydrogen enriched hydrocarbonaceous product. When ash containing extract is
deashed without first substantially cooling the extract, at a temperature above 525 K, degradation
of the extract occurs, such that the resulting deashed extract is more difficult to hydrogenate
catalytically and gives poorer hydrogenation yields than extract which has not been deashed [8].
Mineral matter is a complex mixture of the inorganic minerals and elements, and coal contains
mineral matter in different quantities. The metallic contaminants found in coal extract are metals,
which usually appear in the form of compounds, for example, silicates, complex aluminum sili-
cates, sulfates, sulfides, chlorides and oxides. The metals include Na, B, K, Fe, Ca, Mg, Al, Ti and
Cr. Clay minerals are the most abundant mineral species found in coal, constituting 60–70% of the
average low temperature ash [4]. Quartz is usually the second most abundant mineral phase in
coal, contributing, on average, 20–30% to the mineral matter content [4]. Other mineral matter
forms are minor minerals and trace elements. The minor minerals are carbonates, disulfides,
sulfides, sulfates and feldspars. When coal is burned, the mineral species undergo significant
changes, forming ash. Oxides of Si, Ca, Mg, Na, K and Ti form in almost all of the high tem-
perature ashes of coals. Therefore, the chemical composition of high temperature ash and that of
the mineral matter is extremely different from each other. Approximation of the mineral species
from ash composition does not give reliable results.
The effect of demineralization on some of the processes, such as pyrolysis, combustion, liq-
uefaction and gasification, has also been studied [9]. A decrease in char reactivity [10,11] and an
increase in the pyrolytic yields of tar and gaseous hydrocarbons [12] were observed as a conse-
quence of demineralization. Dilatometric properties were affected adversely by the removal of
mineral matter [13]. It has also been observed that low rank coals have higher extractability in
pyridine than bituminous coals after demineralization [14]. Again, after demineralization, solvent
extraction through such chemical reactions as depolymerization, reduction, amidomethylation,
succinoylation, reductive acylation and alkylation revealed a decrease in the yield of benzene/
methanol extract [15].
In general, demineralization or deashing of coal aims at a desulfurization process. There are
nearly fifteen different processes that can be applied to remove sulfur dioxide from the flue gases
produced by coal combustion. These processes can, in general, be classified into two main groups:
wet processes [16–22] and dry processes [23–29]. The wet processes are:
 A. Demirbasß / Energy Conversion and Management 43 (2002) 885–895 887

• lime or limestone/sludge processes [19],

• magnesium oxide–magnesium carbonate/sludge process [22,30],
• dual alkali process [31,32],
• ammonia based scrubber process [33],
• sodium (Na2 SO3 ) based scrubber process,
• organic based scrubber process [34,35],
• seawater process [36].

Dry processes are:

• spray dry processes [37],

• alkali injection processes,
• calcium based alkali injection process [27],
• humidified duct injection process [38,39],
• active carbon adsorption process [28],
• catalytic oxidation [35,40],
• electron beam treatment.

2. Demineralization and desulfurization methods

2.1. Column froth flotation method

Lignite, before utilization, is subjected to some physical, chemical and biological desulfuriza-
tion methods. In mineral processing, a flotation method is used to separate and concentrate ores
by altering their surfaces to a hydrophobic or hydrophilic condition, i.e., the surfaces either repell
or attract water. Most kinds of minerals require coating with a water repellent to make them float.
By coating the minerals with small amounts of chemicals or oils, finely ground particles of the
minerals remain unwetted and will, thus, adhere to air bubbles. The mineral particles are coated
by agitating a pulp of ore, water and suitable chemicals. The latter bind to the surface of the
mineral particles and make them hydrophobic. The unwetted particles adhere to air bubbles and
are carried to the upper surface of the pulp, where they enter the froth and the froth containing
these particles can then be removed. Froth flotation is separation of minerals that differ little in
density but greatly in wettability by surface active agents that stabilize a froth formed on the
surface of an agitated suspension of the mineral in water.
Froth flotation is a mineral processing method for separation of the valuable minerals from the
gangue minerals, which can be achieved by utilizing differences in physico-chemical surface
properties between valuable and gangue minerals. The establishment of contact among three
phases, which are mineral particles to be floated, an aqueous electrolyte solution and a gas,
characterize flotation. In froth flotation, ground ore is agitated in water, and various chemical
reagents are added to cause the selected (valuable or sometimes gangue) minerals to adhere to the
air bubbles. These air bubbles, carrying the hydrophobic mineral particles, rise to the surface of
the pulp, where they are removed in the froth, while hydrophilic mineral particles remain sus-
pended in the pulp. The froth, or float fraction, is usually named concentrate.
888 A. Demirbasß / Energy Conversion and Management 43 (2002) 885–895

Because Turkish lignite is usually low in heating value and burning characteristic, with high
sulfur and ash content, they are unable to conform to air protection regulation requirements if
burned as mined. The majority of the sulfur of the lignite is generally present as pyritic sulfur,
which has different sizes and forms. Conventional mineral processing techniques of coal cleaning,
such as gravity separation, can be applied to the coarse particles. Fine grinding is required to
liberate the finely distributed pyritic sulfur in the coal. The conventional froth flotation method is
applied to the lignite for three aims: (1) to obtain a product with low sulfur and ash content by
recovery of the coal in slime, (2) to diminish pollution of the environment by cleaning the process
water, which is called black water and is removed from the coal preparation plant and (3) to
produce cooking coal by separating macerals from the coal.
Coal is native floatability and, native floatability depends on the amount of mineral matter
or ash content of the coal, in other words, the rank of the coal. All the coal types oxidize when
exposed to the atmosphere. The effect is attributed to surface oxidation, which takes place readily
at normal atmospheric conditions, is characterized by the formation of acidic groups at the coal
surface and results in a reduction of the hydrophobicity of the coal. Low rank coals are readily
oxidized and lose much of their floatability. In these cases, flotation of the gangue minerals has
been preferred to flotation of the coal [41,42].
In the conventional flotation process, the pulp in a flotation cell is agitated to obtain particle
suspension, and the mechanism of agitation permits entrainment of air into the cell. This air is
dispersed as fine bubbles. During the flotation, the bubbles rise to the surface of the pulp, and a
froth zone is taking place. In a flotation froth, both water and solids are recovered into the
concentrate from the level of the equilibrium froth height. Most of the solids are hydrophobic
mineral particles, and these particles leave the cell-attached bubbles surfaces. Hydrophilic mineral
particles, called slime, are recovered by mechanical entrainment in the froth. Hydrophilic mineral
particles are transferred up and out of cell, suspended in the water between bubbles. Recovery of
the concentrate is increased by entrainment, while the grade of concentrate is decreased. En-
trainment is a problem in fine particle flotation. Using a column flotation method minimizes this
problem. Column flotation has an advantage over conventional flotation because it can provide
higher concentrate grade, higher recovery, lower maintenance costs and improved process control.
Flotation variables are the pH of pulp, types and dosages of reagents, percentage of solid in pulp,
temperature and agitation rate [1].

2.2. Other methods

Any deashing process, that is suitable for at least a portion of the ash contained in coal extract
at a temperature above 525 K is applicable. Specific deashing methods are washing the containing
extract with organic and inorganic acids. Aqueous solutions of strong inorganic acids, such as
hydrochloric acid and phosphoric acid, are particularly suitable. An organic acid, performic acid,
has the potential of oxidation of the organic matrix of coal at low temperatures, leaving con-
centrated mineral matter [43]. Researches on performic acid oxidation, using both mineral matter
of coal and some commercial minerals, showed that clay minerals and silicates are almost inert to
performic acid oxidation. However, carbonates and sulfur minerals are not resistant to performic
acid, even at low temperature [44].
 A. Demirbasß / Energy Conversion and Management 43 (2002) 885–895 889

Oxydesulfurization is a method by which considerable proportions of both pyritic and organic

sulfur can be eliminated from coal, using mainly water and oxygen [45–47]. Certain abundant and
cheap materials are potential reagents for desulfurization. Of these materials, biomass ash is
of interest. Since ash from biomass, especially tea waste, has abundant alkaline compounds
(K2 O þ CaO), it is possible to use the water extractable components of tea ash as a desulfurization
reagent [18]. However, the cost of extracting the alkali from the ash in a high pressure and
temperature stainless steel plant is likely to make these materials expensive reagents. Minerals
(potassium, calcium, sodium and magnesium), appearing in the unburned biomass in the form of
salts, are converted into their oxides during the burning process. These oxides combine with the
carbon dioxide, produced as a result of combustion, to form the carbonates. The oxydesulfuri-
zation kinetics of a hard lignite sample from a Turkish lignite (from the Gediz area) has been
investigated under the conditions of an oxygen partial pressure of 1 MPa, with a 0.10 M
equivalent Na2 CO3 solution of trona, at temperatures of 423–473 K [45]. Trona minerals were
seen as a suitable alkaline to use in oxydesulfurization of coal [46]. The oxydesulfurization kinetics
of a hard lignite sample from the Gediz area (in Turkey) has been investigated by the oxyde-
sulfurization method using an ammonia solution [47]. It was concluded that the use of an am-
monia solution as an extraction solution increased the efficiency of the oxydesulfurization process.
The sulfur removal potential of the water soluble fraction of fly ash in oxydesulfurization of coal
was studied using some high sulfur lignites [17].
Desulfurization of four samples of Central Anatolian lignites by treatment with aqueous NaOH
was examined [48]. NaOH concentration and temperature were significant parameters, but the
extraction time had only a slight effect. Organic sulfur was not removed from three of the samples,
but in the other lignite 12.5% of the organic sulfur was removed by treatment at 345 K for 8 h with
20 wt./v% NaOH solution [48]. Total sulfur contents were considerably reduced by aqueous
NaOH treatment, but one high sulfur lignite was found to be more resistant to sulfur removal
than the others. The desulfurization of a Turkish lignite with acidic ferric chloride solution and its
kinetics and mechanism were investigated, and it was found that the effects of leaching temper-
ature and particle size on the removal of pyritic sulfur are very significant [49]. Increase of the
FeCl3 concentration and decrease of the acidity increased the removal of pyritic sulfur. Another
study [50] reports desulfurization of the asphaltite using aqueous H2 O2 –H2 SO4 solutions. The
main reaction between H2 O2 and FeS2 in coal can be expressed as follows:
FeS2 þ 7H2 O2 ¼ FeSO4 þ H2 SO4 þ 6H2 O

3. Experimental considerations

Lignite samples used in this work were supplied from different Turkish lignite and coal sources.
Proximate analyses of these samples were performed according to ASTM Standards (D 3173-74
and D 3175-77). Ash contents of the lignite and tea waste samples were determined according to
ASTM Standard (D 3174-75), and the mineral matter contents of the ashes were determined by
ASTM Standard (D 2795-69). Proximate and sulfur analyses of the lignite and coal samples are
presented in Tables 1 and 2, respectively. The six lignite samples had sulfur contents ranging from
3.1% to 11.8% dry basis and ash contents from 10.7% to 26.4% dry basis. The three coal samples
were of bituminous rank with uniform sulfur contents, 0.5% dry basis, and ash contents ranging
890 A. Demirbasß / Energy Conversion and Management 43 (2002) 885–895

Table 1
Proximate analyses of lignite and coal samples (wt.%, mean and standard deviation)
Sample Moisture Volatile matter Fixed carbon Ash
Lignite-1 15:3  1:05 41:0  2:12 30:0  1:30 10:7  0:62
Lignite-2 10:0  0:64 39:2  2:14 43:0  2:25 13:7  0:88
Lignite-3 25:4  1:36 35:3  1:88 13:9  0:63 26:4  1:29
Lignite-4 14:0  0:92 38:9  2:04 33:3  1:25 14:4  0:96
Lignite-5 14:6  0:94 43:6  2:18 33:7  1:28 8:1  0:38
Lignite-6 12:8  0:71 38:9  1:92 42:4  2:16 11:7  0:54
Coal-1 0:5  0:04 25:9  1:76 59:1  2:82 14:5  1:04
Coal-2 1:6  0:12 26:8  1:86 60:2  3:04 11:4  0:92
Coal-3 2:2  0:20 26:9  1:90 57:4  2:88 13:5  0:98

Table 2
Sulfur analyses of lignite and coal samples (wt.%, mean and standard deviation)
Sample Organic sulfur Pyritic sulfur Sulfate sulfur Total sulfur
Lignite-1 1:82  0:10 0:98  0:05 0:26  0:04 3:06  0:18
Lignite-2 4:21  0:23 2:75  0:14 0:38  0:05 7:34  0:42
Lignite-3 2:08  0:12 1:32  0:09 0:08  0:01 3:48  0:20
Lignite-4 1:94  0:11 1:87  0:13 0:52  0:06 4:33  0:30
Lignite-5 1:71  0:09 5:27  0:34 0:21  0:02 7:19  0:45
Lignite-6 4:79  0:18 6:41  0:38 0:64  0:07 11:84  0:63
Coal-1 0:34  0:03 0:15  0:02 0:07  0:00 0:51  0:04
Coal-2 0:28  0:03 0:16  0:02 0:05  0:01 0:49  0:04
Coal-3 0:32  0:03 0:14  0:02 0:06  0:01 0:52  0:04

from 11.4% to 14.5% dry basis. In each case, the organic sulfur constitutes 55–60% of the total
sulfur in the coal, while the pyritic sulfur is 30–40% of the total.

3.1. Column froth flotation method

A schematic representation of the flotation column, which is used in the experiments, is shown
in Fig. 1. A flotation column has a circular or square cross-section and has no impeller to agitate
the pulp mechanically and disperse air within it. The conditioned pulp is fed into the column at
the feed point. In order to generate air bubbles, the air is introduced at the base of the column via
an internal air sparger. All particles collide with rising bubbles in the collection zone, and hy-
drophobic particles adhere to the bubbles and are transported to the cleaning zone. Hydrophilic
particles exit from the base of column. In the cleaning zone, the froth is washed by a net
downward flow of water, called a positive bias. This bias water is provided by the wash water
added into the cleaning zone, either just below or just above the top of the column. The washing
eliminates entrainment of the hydrophobic particles. In order to produce a high quality product,
downward flow of the water through the froth must be maintained. Superficial or volumetric flow
rates of air, feed, wash water, bias water and heights of cleaning and collection zone are important
variables for a column flotation operation. Typical values of the column flotation variables are
summarized in Table 3.
 A. Demirbasß / Energy Conversion and Management 43 (2002) 885–895 891

Fig. 1. Experimental set up for column froth flotation tests.

Table 3
Typical values of column flotation variables
Variable
Aira Washwatera Bias watera Froth height Gas holdup Diameter/o-
height ratio
Range 1.0–3.0 0.1–0.5 0.1–0.5 up to 1.5 m 20–25% 1:5–1:30
a
Superficial flow rates in cm/s.

A direct flotation or reverse flotation method can achieve removal of the sulfur from lignite.
The reverse flotation method can usually be used for oxidized or weathered lignite, which has
a hydrophilic property in the flotation process. In this case, using a suitable collector, such as
xanthate, floats the sulfur bearing minerals. As was seen in Table 2, the Lignite-6 sample has
11.8% S, and the pyritic sulfur content of the sample is 6.4%. At the beginning of the experimental
studies, because lignite has generally native hydrophobicity, direct flotation method tests are
conducted for removal of the sulfur from the lignite sample, but when the lignite sample is oxi-
dized; the results obtained from the tests are not satisfactory. Although pyritic sulfur can be
collected in the froth by using the reverse flotation method, in order to remove sulfur from the
lignite, reverse flotation tests are conducted.
At the beginning of the column flotation tests, the chemical variables are the same as for
conventional flotation tests. In order to determine the other variables, which belong to column
flotation, serial tests were conducted. Initial values of the variables are given as follows:

Superficial feed flow rate: 0.26 cm/s

Superficial wash water flow rate: 0.26 cm/s
Superficial air flow rate: 1.31 cm/s
Superficial tailing flow rate: 0.30 cm/s
Superficial feed flow rate: 0.24 cm/s
Positive bias rate: 1.14
892 A. Demirbasß / Energy Conversion and Management 43 (2002) 885–895

Table 4
Conventional reverse flotation (Run-1) and serial conventional flotation (Run-2) tests conditions
Variables Run-1 Run-2
PH (adjusted by H2 SO4 ) 7.0 6.0
Depressant (g/t) (condition time is 2 min) 50 50
Collector (g/t) (condition time is 4 min) 100 150
Flotanol (g/t) (condition time is 1 min) 50 50
Flotation time (min) 4 4
Solid percent of the pulp (%) 10 20
Stirring rate (rpm) 1500 1300

Diameter of column: 0.09 m

Mean residence time: 7 min
Gas holdup: 20%
Height of column: 1.85 m

Flotation test conditions for the column froth flotation are given in Table 4. The conventional
reverse flotation tests are conducted with the initial flotation conditions in Table 4 (Run-1). In
order to obtain optimum values of the pH, particle size, amount of collector, frother and de-
pressant, serial conventional flotation tests are conducted (Table 4, Run-2). Increasing the pH,
amount of the collector and depressant and solid percent of the pulp cause a decrease in the
efficiency of desulfurization [1].
The column flotation method is more effective than the conventional flotation method for re-
moval of pyritic sulfur from lignite coal. The flotation process can be more effective in desulfu-
rization of the coal when the majority of the sulfur content of the coal is pyritic sulfur. In addition,
it was believed that the higher percent of pyritic sulfur in the total sulfur content of the coal
prompted the production of lower sulfur content clean coal, and the column flotation method can
produce a cleaner coal product than the conventional flotation. By using the column flotation
method for desulfurization of low rank lignites, they will create lower environmental pollution.

3.2. Other methods

Performic acid (HCO3 H) is an effective oxidation agent for the organic matrix of coal at low
temperatures, leaving concentrated mineral matter. A coal sample was treated with performic
acid, and the mineral matter that remained after the applied stage can be isolated. During oxi-
dation, carbon dioxide bubbles were rising in the acidic suspension, and the color of the coal–
formic acid–hydrogen peroxide mixture turned from black to light brown. When oxidation was
completed, the mineral matter is filtered through a Whatman no. 1 filter paper and washed several
times with hot distilled water, to remove excess acid, and dried at 383 K for 24 h under a nitrogen
atmosphere.
The performic acid oxidation method is a rapid, practical and suitable method for isolation of
mineral matter from the organic part of coal. However, some organic constituents of coal cannot
be eliminated completely. C–H and C@O stretching vibrations of organic material were the ev-
 A. Demirbasß / Energy Conversion and Management 43 (2002) 885–895 893

idence of this fact. By removal of some mineral species from coal, it is appropriate to determine
other minerals, such as pyrite, that is almost impossible to detect it in the presence of them.
Extraction of biomass ash is performed by placing 15–60 g of ash in 500 ml of water in a conical
flask held at a constant temperature by a thermostat. The ash water mixture is stirred for 10–70
min at 300–650 rpm. At the end of the stirring period, the mixture was immediately filtered
through a Whatman no. 1 filter paper, washed with 100 ml of distilled water, and the residue is
dried and weighed.
Desulfurization of lignite samples was performed using a magnetically stirred 1-l Parr autoclave
[18]. The filtrate solution with the water extractable components of the tea waste ash was added to
a 10 g lignite sample of <0.250 mm particle size in the autoclave. Afterwards, the autoclave was
sealed and heating was started while stirring the suspension. The optimal heating time was 30 min.
The mixture was allowed to stand at a given temperature for the desired period. At the end of this
period, the autoclave was rapidly cooled using tap water, its contents were filtered through a
Whatman no. 1 filter paper, and the treated lignite was washed with hot distilled water until the
water extractables were eliminated, and the pH of the washings became neutral. The treated
lignite was dried at 360 K for 20 h in a vacuum oven under nitrogen flow [18].
The effects of temperature on sulfur removal were investigated using the water soluble fraction
of 20 g of biomass ash under different vapor pressures of water for 30 min at 500 rpm stirring

Fig. 2. Influence of temperature on total sulfur removal of coals by biomass ash method sample: 15 g, stirring speed:
500 rpm, extraction time: 30 min.
894 A. Demirbasß / Energy Conversion and Management 43 (2002) 885–895

speed [18]. The relations between temperature and total sulfur removal from the lignite samples
are shown in Fig. 2. Removal of total sulfur content in the different samples increased continu-
ously with increasing temperature. For example, it increased from 12.3% to 14.0% at 350 K and
51.5% to 56.0% at 525 K. Desulfurization of the samples of coals with distilled water under 1.7
MPa partial pressure of water vapor at 475 K for 30 min at 500 rev min1 stirring speed resulted in
the removal of about 34.5% of the total sulfur content.

4. Conclusion

The emission of sulfur oxides resulting from coal combustion is one of the great problems that
leads to undesirable changes in the environment. This type of pollution can cause serious damage,
not only on public health but also on soil, water and other natural resources. Sulfur corrosion is a
problem specific to Turkey and other countries burning high sulfur lignite. Various methods exist
for reducing these hazardous effects. One of the most suitable methods is froth flotation for re-
moval of pyritic sulfur from coal. Alkali desulfurization and oxidesulfurization also are effective
applicable methods for high sulfur coals.

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