Institute of Energy and Environmental Engineering

Clean Coal Technology

Open-Ended Lab
Submitted By:
Amna Tariq Roll No.05
Laiba Ashiq Roll No.17
Ayesha Nasir Roll No.18
Bisma Tahir Roll No.25
Introduction:
Coal:
Coal is a sedimentary deposit composed predominantly of carbon that is readily combustible.
Coal is black or brownish-black, and has a composition that (including inherent moisture)
consists of more than 50 percent by weight and more than 70 percent by volume of carbonaceous
material.
Coals which are low in specific energy because of high moisture content and / or high ash/ sulfur
contents, and produce emissions of concern are termed as low grade coal. Coal generally
incorporates various amounts of mineral matter as impurity. The presence of mineral matter
adversely affects most aspects of coal utilization and processing. Therefore, removal of mineral
matter prior to coal utilization is desirable. Sulfur both in inorganic and organic forms is
deleterious in coal which releases SO2 during burning. Therefore, it is necessary to demineralise
and desulfurize such coals prior to utilization for its economical and environmental benefits.
Our Coal sample is from Kaka Khel , a town and union council of Lakki Marwat
District in Khyber Pakhtunkhwa province of Pakistan. It is located at 32°32'59N 70°47'44E and
has an altitude of 307 metres. The coal here is composed primarily of carbon but also contains
other elements like hydrogen, oxygen, nitrogen, and sulfur.
Coal Beneficiation:
Coal beneficiation, or coal preparation as it is also termed, refers to the processes through which
inorganic impurities are separated from raw mined coal, thereby providing improved combustion
characteristics to the fuel produced. It can be done by physical or chemical processes.
Chosen Technique:
 Chemical Leaching:
Leaching is a process of extracting a substance from a solid material that is dissolved in a
liquid. This process is commonly referred to as extraction, particularly in the chemical
industry. Three basic steps are involved in the leaching process: contact, separation, and
extraction.
Chosen Acid:
 H 2 SO4

The most common reagent used in leaching of metals is sulphuric acid (H2SO4). Whereas other
heavy metals are able to dissolve in H2SO4, copper (Cu) dissolves quicker in this acid than
metals such as zinc, cobalt and iron because it is higher up in the electrochemical series.
Literature Review:
The effect of hydrogen peroxide alone and in presence of dilute sulfuric acid on desulfurization
and demineralization of coal of north-eastern region, India was investigated by Mukherjee et al.,
2001. H202 (15%) alone removed over 76% pyritic sulfur,70% sulfate sulfur, 5% organic sulfur
and over 14% ash at 25°C which improved to almost complete removal of pyritic and sulfate
sulfur, over 26% organic sulphur and 43% ash in the presence of 0.1 N H2SO4. Sulfuric acid
acts as catalyst for bringing oxygen and pyrite molecules close to each other which helps in
desulfurization. The kinetic and energetic studies on the acidic (0.1 N H2SO4) hydrogen
peroxide desulfurization of Indian coal were reported by Mukherjee and Srivastava, 2004.
Vasilakos et aL, 1984 investigated chemical beneficiation of high volatile bituminous coal with
H202/H2SO4 at ambient temperature. Almost complete removal of inorganic sulfur and
substantial reduction in ash were observed. However, organic sulfur was hardly affected.
Ahnonldtpanit and Prasassarakich, 1989 followed the similar treatment for subbituminous high
volatile coals from Thailand and observed removal Of a small amount of organic sulfur (7.1%)
along with most of the ash and inorganic sulfur. Karaca and Ceylan, 1997 also found H202 as an
effective agent for removal of ash and pyritic sulfur, but less effective for organic sulfur. A. 15%
H202 was suitable for appreciable reduction in ash and pyritic sulfur from lignites within 60 min
at 30°C.

Objective:
Coal Beneficiation by chemically treating it with 3% H 2 SO4 of Kaka khel coal sample.
Apparatus:
 Oven
 Hot Plate
 Beakers
 Stirrers
 Funnel
 Filter Paper
Chemical:
 H 2 SO4

Solution Preparation:
Prepare 3% diluted solution of H 2 SO4 with concentration 98% in 100ml water:
C 1 V 1=C 2 V 2

98 ×V 1=0.03 ×100

V 1=3.06 ml of H 2 SO4

Procedure:
 Mix 3.06 ml of H 2 SO4 in 96.94 ml of hot water.
  Add 15g of coal in the prepared solution.
 Stir the solution for about 15 minutes and keep it on rest for 1 or 1.5 hrs.
 Filter the solution using a filter paper.
 Do washing of the remaining coal left in beaker with hot water.
 Dry the filter paper in oven for about 1 hr.
 Do Proximate analysis, eschka of the treated coal to examine the effect.
Proximate:
MOISTURE:
• Weight the empty crucible.
• Take 1 gram of sample in weighed crucible.
• Place the crucible with coal sample in the hot air oven.
• Maintain the oven at temperature of 110C.
• Keep the crucible in oven for 1 hour.
• Remove the crucible with the help of tongs and place it in desiccators. • Again, weigh the
sample.
• Loss in weight is reported as the moisture content on percentage basis.
VOLATILE MATTER:
• Weight the empty crucible.
• Take 1 gram of sample in weighed crucible.
• Cover the crucible with lid and place the crucible in muffle furnace.
• Maintain the temperature of muffle furnace at 900 ± 50C.
• Keep the crucible for 7 minutes.
• Keep the crucible in desiccators for cooling.
• Weigh the crucible again.
• Loss in weight is reported as volatile matter on percentage basis.
ASH:
• Weight the empty crucible.
• Take 1 gram of sample in weighed crucible.
• Keep crucible in the muffle furnace without lid.
• Maintain the temperature of 700±50C in muffle furnace.
• Keep the crucible for 3 hours.
• Remove the crucible and keep it in desiccators for cooling.
• The weight left will be the weight of ash.
• Report the residue as ash (on % basis).
FIXED CARBON:
• Add all the percentages of Moisture, Volatile matter and Ash the subtract it from 100 to get the
percentage of fixed carbon.
Eschka:
• Preparation of Sample and Mixture—Thoroughly mix on glazed paper approximately 1 g of the
sample, weighed to nearest 0.1 mg and 3 g of Eschka mixture. The amount of sample to be taken
will depend on the amount of BaCl2 solution. Transfer to a porcelain capsule, or porcelain
crucible, or a platinum crucible and cover with about 1 g of Eschka mixture.
• Ignition—Heat the crucible over an alcohol, gasoline, or gas flame or in a gas or electrically
heated muffle. The use of artificial gas for heating the sample and the Eschka mixture is
permissible only when the crucibles are heated in a muffle.
• Open Flame—Heat the crucible, placed in a slanting position on a triangle, over a very low
flame to avoid rapid expulsion of the volatile matter that tends to prevent complete absorption of
the products of combustion of the sulfur. Heat the crucible slowly for 30 min, gradually increase
the temperature, and occasionally stir until all black particles have disappeared, which is an
indication of the completeness of the procedure.
• Muffle (Coal)—Place the crucible in a cold-vented muffle and gradually raise the temperature
to 800 ± 25°C in about 1 h. Maintain this maximum temperature until, on stirring, all black
particles have disappeared (about 1 - 1⁄2 h).
• Subsequent Treatment—Remove the crucible and empty the contents into a 200-mL beaker and
digest with 100 mL of hot water for 1⁄2 to 3⁄4 h, while stirring occasionally.
• Decant the solution through filter paper, retaining as much insoluble material in beaker as
possible.
• Thoroughly wash the insoluble matter in the beaker with hot water. After several washings in
this manner, transfer the insoluble matter to the filter and wash five times with hot water,
keeping the mixture well agitated.
• Make the filtrate, amounting to about 250 mL, just neutral to methyl orange with NaOH or
Na2CO3 solution; then add 1 mL of HCL (1 + 9).
• Boil and add slowly from a pipet, while stirring constantly, 10 mL or more of BaCl2 solution.
The BaCl2 solution must be in excess. If more than 10 mL of BaCl2 solution is required, reduce
the weight of sample to about 0.5 g and repeat the ignition and digestion.
• Continue boiling for 15 min and allow to stand for at least 2 h, or preferably overnight, at a
temperature just below boiling.
• Filter through a fine ashless paper, such as Whatman No. 42 or similar, and wash with hot
water until 1 drop of silver nitrate (AgNO3) solution produces no more than a slight opalescence
when added to 8 to 10 mL of filtrate.
• Place the wet filter containing the precipitate of barium sulfate (BaSO4) in a weighed platinum,
porcelain, silica, or alundum crucible, fold the paper loosely over the precipitate to allow a free
access of air but prevent spattering.
• Smoke the paper off gradually in a muffle furnace and at no time allow to burn with flame.
After the paper is practically consumed, raise the temperature to approximately 800 ± 50°C and
heat to constant weight. Weigh the barium sulfate to the nearest 0.1 mg.
Results and Calculation:
Recovery of Coal after leaching:
Filter Paper Weight: 0.92g
Initial Coal weight: 15g
Final weight: 14.95
Recovered Coal: 14.03g
Proximate Analysis:
Moisture:
Petri dish weight=43.73g
Final weight=44.73g
Sample=1g
%moisture= 0%
Volatile Matter:
Crucible weight= 35.17g
Final weight= 36.04g
Coal sample = 1g
%VM= 13%
Ash:
Crucible weight= 46.2g
Final weight=46.37g
 Coal sample =1g
%Ash= 15%
Fixed Carbon:
%FC=72%
Esckha:
Sample =1g
Initial filter paper = 0.92g
Final filter paper = 1.15g
%Sulfur= 3.16%

Comparison Table:
Sample Moisture Volatile Ash Fixed Eschka
Matter Carbon
Raw 4% 10% 19% 67% 3.72%
Treated 0% 13% 15% 72% 3.16

Analysis of results:
 After chemicaly treating coal with H₂SO₄ moisture decreases from 4% to 0% because
H₂SO₄ has a high affinity for water, meaning it can absorb water molecules from the
coal, effectively drying it out. The acid binds to the water and forms a more stable
compound, thus removing free water from the coal. The reaction between H₂SO₄ and
water is exothermic, meaning it releases heat. This heat can evaporate moisture from the
coal sample.
 Volatile matter increases from by 3% it may be due to Sulfuric acid may chemically react
with certain constituents in the coal, leading to the formation of new volatile compounds
or the release of previously bound volatiles. For example, sulfuric acid can decompose
certain mineral matter or organic compounds in coal, increasing the overall volatile
content.
 The reduction in ash content from 19% to 15% after treating your coal sample with
sulfuric acid (H₂SO₄) can be because Sulfuric acid can dissolve certain mineral
components in the coal, such as carbonates, sulfates, and some metal oxides. This
dissolution reduces the overall ash content, as these minerals contribute to the ash when
the coal is combusted.
 The treatment with sulfuric acid reduces the moisture content from 4% to 0% and the ash
content from 19% to 15%. Since fixed carbon is calculated on a dry, ash-free basis, the
removal of these components increases the relative proportion of fixed carbon.
  Sulfur content reduces by 0.56%. it can be due to Sulfuric acid can react with sulfur-
containing minerals in the coal, such as pyrite (FeS₂), to form soluble products like iron
sulfate (FeSO₄) and hydrogen sulfide (H₂S), which can then be removed from the coal.
Conclusion:
Treating coal with sulfuric acid (H₂SO₄) effectively alters its composition by reducing
undesirable components and concentrating valuable ones. The acid acts as a strong dehydrating
agent, removing moisture and promoting the dissolution and leaching of ash-forming minerals
and sulfur compounds. This treatment also affects the volatile matter and fixed carbon content
through chemical reactions and structural changes in the coal. Overall, sulfuric acid treatment
improves the coal's quality by enhancing its combustion properties and reducing its
environmental impact.
Safety Precautions:
 Chemical Handling: Handle all chemicals, especially acids and peroxide, with extreme
care to avoid accidents.
 Protective Gear: Always use appropriate protective gear, including gloves, goggles, and
lab coats, to ensure personal safety during the experiments.