Title of Invention

AN IMPROVED PROCESS TO PRODUCE LOW ASH COAL FROM HIGH ASH COAL AND SYSTEM THEREOF

Abstract The present invention relates to an improved process to produce low ash coal from high ash coal, comprising the steps of forming a slurry of coal fines in a N-Methyl-2-pyrrolidone (NMP) including Ethylenediamine (EDA), NMP and EDA being between 6:1 to 24:1 solution, said slurry containing about 6 to 25 ml of solution per g of coal; maintaining said slurry in refluxed condition at a temperature of about 170 °C for a period of about 15 minutes to 2 hours; separating the refluxed solution in two parts by coarse filtration at 0.025 mm filter cloth a cut size of the separation being variable depending on the particle size filtrate, extract and residue to be treated; cooling the filtered coal-solvent mixture; precipitating the coal by adding acetone in the extract; separating the coal by filtration, said coal having a reduced ash content; and recovering the rest of the solvent by distillation of the acetone-solvent solution.
Full Text FIELD OF THE INVENTION
The present invention relates to an improved process to produce low ash clean
coal from high ash coal. The invention further relates to a system for producing
low ash clean coal from high ash coal including high recovery of solvents
BACKGROUND OF THE INVENTION
Concept and implementation of chemical beneficiation comes from the limitation
of physical beneficiation processes. Broadly, a chemical beneficiation is possible
by chemical leaching of mineral matter present in coal or, dissolving organic
matter of coal in various organic solvents. As coal is a heterogeneous mixture of
organic and inorganic constituents, the degree of solvolysis of coal varies with its
constituents, maturity, and structural characteristics. Main advantages of the
chemical beneficiation process are i) ease of recovery of solvent in the main
process stream, ii) solvolytic efficiency of recovered solvents as that of fresh
solvent, iii) 98-% recovery of the solvent, iv) improved coking properties of clean
coal, and v) availability of industrial organic solvents. However, the operating
cost of this process is high because of high cost of solvents and energy
requirement in the process. There is an attempt to make this process techno-
economic through improving the yield to 70-80%. However, further research
may be required to make the process economically viable through reducing the
cost of solvent recovery.

Recovery of clean coal and its ash content depend on various operating
parameters of the process and feed characteristics like faster and convenient
filtration of refluxed solution at different size, solvent and co-solvent of choice,
coal source (feed characteristics), particles size, coal-solvent ratio, extraction
time, extraction temperature, etc. Thus, the process offers a balance between
the yield and the ash contents desired in the clean coal.
Since the mineral matter (non-combustible) in Indian coals (Gondwana coals) is
very finely disseminated in the organic mass, it is quite difficult to remove the
mineral matter by conventional physical coal washing techniques. High
percentage of near gravity material in this coal, makes the scope of gravity
process substantially limited. This indicate that chemical treatment may be the
right approach to overcome the limitation of physical beneficiation methods. A lot
of literature is available on chemical beneficiation techniques (US patent
5955375, 21/09/1999) that employ high corrosive chemicals (mostly acids and
alkalis). Recovery or regeneration of these chemicals is very important to make
this technology viable. A parallel approach towards lowering ash, is the process
of recovering the premium organic matter from coal by solvent refining.
Literature (India 1088/KOL/2007) reveals that most of the research work on this
subject was carried out with an objective to produce ultra clean coal or super
clean coal with ash content less than 0.2% for various high tech end uses. This
known solvent refining process does not serve the objective of low ash coal
requirement of steel industries because of mainly low recovery which makes the
process uneconomic especially when such an ultra coal is not absolutely desired
at the cost of restricting to low yields.

Patent literatures described solvent extraction (India 1292/KOL/2006, India
1336/KOL/2008 techniques that employ expensive solvents. According to the
existing process, coal, solvent and co-solvents are mixed thoroughly to produce
coal slurry. The coal slurry is extracted in a known manner which includes coal-
solvent mixture. The mixture is separated in a separation unit to produce a
coarser fraction and a finer fraction. The finer fraction is fed to an evaporator
unit to allow 70 to 80% of solvent recovery. The hot concentrated coal-solvent
mixture is then flushed in a precipitation tank to precipitate the coal. Water as an
anti-solvent is being used. Coal is precipitated and water-solvent mixture as
obtained separated in a distillation column. Recovery or regeneration of these
solvents and anti solvent are very important to make this technology viable.
Conventionally solvent is recovered by hot precipitation of coal extracts in anti
solvent, but there is no prior art available on cold precipitation. Therefore there
is a need to propose a noble process to recover the solvent and anti solvent
which is convenient and adapts cold precipitation.
OF THE INVENTION
It is therefore an object of the invention to propose an improved process to
produce low ash clean coal from high ash coal.
Another object of the invention is to produce an improved process to produce
low ash clean coal from high ash coal, which adapts an economic and
environment-friendly Anti-solvent suitable for industrial extraction of coal.

A still another object of the invention is to propose an improved process to
produce low ash clean coal from high ash coal, which is economic and
environment-friendly.
A further object of the invention is to propose an improved process to produce
low ash clean coal from high ash coal, which provides better separation and
ensures high recovery of solvents.
A still further object of the invention is to propose an improved process to
produce low ash clean coal from high ash coal, which provides better separation
of extracted coal and solvent mixture.
Yet another object of the invention is to propose a system for producing low ash
clean coal from high ash coal including high recovery of solvents.
SUMMARY OF INVENTION
Accordingly, in a first aspect of the invention, there is provided An improved
process to produce low ash coal from high ash coal, comprising the steps of
forming a slurry of coal fines in a N-Methyl-2-pyrrolidone (NMP) including
Ethylenediamine (EDA), NMP and EDA being between 6:1 to 24:1 solution, said
slurry containing about 6 to 25 ml of solution per g of coal; maintaining said
slurry in refluxed condition at a temperature of about 170 °C for a period of
about 15 minutes to 2 hours;

separating the refluxed solution in two parts by coarse filtration at 0.025 mm
filter cloth a cut size of the separation being variable depending on the particle
size filtrate, extract and residue to be treated; cooling the filtered coal-solvent
mixture; precipitating the coal by adding acetone in the extract;; separating the
coal by filtration, said coal having a reduced ash content; and recovering the rest
of the solvent by distillation of the acetone-solvent solution.
According to the invention, coal solvent and co-solvent are mixed thoroughly to
produce a coal slurry. The coal slurry is extracted in a known manner which
includes coal-solvent mixture. The mixture is separated in a separation unit to
produce a coarser fraction and a finer fraction. The finer fraction is cooled in a
jacketed vessel and not being fed to evaporation unit, thus this energy can be
used for heating purpose in the process. The cooled extracted clean coal-solvent
mixture is then flushed in a precipitation tank to precipitate the coal, where,
Acetone as an anti-solvent is being used. Acetone separates the solvent from
coal very effectively, and we get acetone-solvent mixture, which is easily
separable at lower temperature in distillation unit, thus energy is being saved in
distillation column too. And precipitated coal is separated in a rotary drum filter.
The process is an economic and environment-friendly coal extraction process
which is less energy intensive and economically viable. The invention process is
enabled to produce low ash clean coal which provides better separation of
extracted coal and solvent mixture.

According to a second aspect of the invention, there is provided A system for
producing low ash coal from high ash coal, comprising an extractor (1) enabled
to received a coal-slurry produced by thoroughly mixing coal, solvent, and anti-
solvent in a coal-solvent feed plant, temperature in the extractor (1) being
gradually generated to about 200 °C, the residue time of the coal-solvent feed
depending on the process parameters varies between 15 - minutes to 2-hours a
first filter (2) for separating the extracted coal - solvent mixture into a coarser
fraction called as a residue containing high ash , and a finer fraction known as
the filtered extract; a cooler unit (3) for directly receiving the finer fraction; a
precipitation tank (4) for receiving the cooled coal-solvent mixture in which the
acetone acting as an anti-solvent gets the extracted coal separated from the
coal-slurry solution for further precipitation; a second filter (5) for separating the
precipitated coal to produce a clean coal; and a distillation unit (6) for receiving
the filtrate containing solvent and anti-solvent solution to recover the solvent and
the anti-solvent.
BRIEF DESCRIPTION OF THE ACCOMPANYING DRAWING
Figure - 1 - shows a system for producing low ash clean coal from high ash coal
according to the invention.
DETAILED DESCRIPTION OF THE INVENTION
As shown in figure - 1, the inventive system comprises an Extractor (1); a first

filter (2) enabled to separate solid-liquid upto size 500 mesh a cooler (3); a
Precipitation tank (4); a second filter (5) enabled to completely separate solid-
liquid; and a Distillation column (6).
According to the invention, acetone has been identified as the anti-solvent for
convenient, environmental friendly and economical industrial coal-solvent
separation operation. The coal sample is refluxed with NMP and a small amount
of co-solvent (EDA) for 1 h at atmospheric pressure. Then the refluxed mixture
using 500 stainless steel BSS mesh (0.25 mm) cloth is filtered. This arrangement
allowed a coarser and faster filtration at 0.25 mm size in comparison to that
observed by using the known Whatman filter paper. Therefore, increase in yield
of clean and simultaneously increase in ash content of clean coal, have been
clearly established. Thus, the identified anti-solvent is found to be advantageous
to produce high yield clean coal with low ash content (5-8%) through a faster
filtration process.
According to the invention, an improved process to produce low ash clean coal
from high ash cola in the inventive system comprises a step of thoroughly mixing
coal, solvent and co-solvent in a coal - solvent feed tank (not shown). The coal
slurry is then pumped from the tank into the extractor (1). A temperature around
170 - 200 °C is gradually generated in the extractor (1). Residence time in the
extractor (1) may vary form 15 mins to 2 h and i.e. dictated by the techno
economics of the process and its specific requirement. The extracted coal-solvent

mixture is then separated through the first filter (2) which cut the mixture in two
fractions for example, a coarser fraction (+0.25 mm), and a finer fraction (-0.025
mm). The coarser fraction contains high ash and is called as residue. The finer
fraction or filtered extract is then fed to the cooler unit (3) directly, bypassing the
evaporator unit (3). The cooled coal-solvent mixture is flushed in thee
precipitation tank (4), where the acetone acts as an anti-solvent. As the solvents
are strongly soluble in Acetone, the extracted coal gets separated from the
solution phase and gets precipitated. This precipitated coal is separated through
the second filter (5). Thus, a clean coal is obtained which contains less than 4%
ash. The filtrated coal slurry consists of solvent-anti solvent (Acetone) solution
which is sent to a distillation unit (6) where the solvent and the anti-solvent are
recovered after distillation.
EXAMPLE
A sample of 10 gm coal, having - 30 mesh sizes and 27% ash content, is
extracted, using NMP and EDA as a solvent and co-solvent respectively for one
hour. Filtration is done through a 500 stainless steel BSS mesh (0.025 mm).
Precipitation is thereafter separately done in water and acetone. An analysis is
done for clean coal and residue both the clean obtained through extraction and
filtration.
As interesting phenomenon is observed when the acetone is used as the anti-
solvent. For example, if the hot filtered coal-solvent mixture is poured in the

precipitation tank, then the coal is not agglomerated, and further the separation
of coal-solvent is poor. In contrast, if a filtered coal-solvent is properly mixed
acetone. Comparative study of precipitation in water and precipitation in acetone
is shown in table 1.

Table 1 shows that precipitation in water gives less yield, i.e. 35% while
precipitation in acetone gives higher yield, i.e., 43.45% of clean coal. Ash
content of such an experimentation establishes that acetone is better anti-
solvent than water, in terms of yield and in terms of saving of energy mainly
because of low boiling point of the acetone,

WE CLAIM
1. An improved process to produce low ash coal from high ash coal,
comprising the steps of:
(i) forming a slurry of coal fines in a N-Methyl-2-pyrrolidone (NMP)
including Ethylenediamine (EDA), NMP and EDA being between 6:1 to
24:1 solution, said slurry containing about 6 to 25 ml of solution per g
of coal;
(ii) maintaining said slurry in refluxed condition at a temperature of about
170 °C for a period of about 15 minutes to 2 hours;
(iii) separating the refluxed solution in two parts by coarse filtration at
0.025 mm filter cloth a cut size of the separation being variable
depending on the particle size filtrate, extract and residue to be
treated;
(iv) cooling the filtered coal-solvent mixture;
(v) precipitating the coal by adding acetone in the extract;;
(vi) separating the coal by filtration, said coal having a reduced ash
content; and
(vii) recovering the rest of the solvent by distillation of the acetone-solvent
solution.

2. The process as claimed in claim 1 wherein said coal comprises run of mine
coal.
3. The process as claimed in claim 2 wherein said particles size is preferably
between - 2mm and - 0.5 mm, more preferably between 0-25 mm.
4. The process as claimed in claim 1 wherein a moderate ash clean having
ash content 5. The process as claimed in claim 4 wherein said moderate ash clean coal
having ash content furnace injection in iron and steel industries and power generation.
6. The process as claimed in claim 1 wherein acetone is used as the anti-
solvent which is an economic and environment-friendly anti-solvent
suitable for industrial extraction of coal.
7. A system for producing low ash coal from high ash coal, comprising:
- an extractor (1) enabled to received a coal-slurry produced by thoroughly
mixing coal, solvent, and anti-solvent in a coal-solvent feed plant,
temperature in the extractor (1) being gradually generated to about 200
°C, the residue time of the coal-solvent feed depending on the process
parameters varies between 15 - minutes to 2-hours;

- a first filter (2) for separating the extracted coal - solvent mixture into a
coarser fraction called as a residue containing high ash , and a finer
fraction known as the filtered extract;
- a cooler unit (3) for directly receiving the finer fraction;
- a precipitation tank (4) for receiving the cooled coal-solvent mixture in
which the acetone acts as an anti-solvent to get the extracted coal
separated from the coal-slurry solution for further precipitation;
- a second filter (5) for separating the precipitated coal to produce a clean
coal; and
- a distillation unit (6) for receiving the filtrate containing solvent and anti-
solvent solution to recover the solvent and the anti-solvent.
8. An improved process to produce low ash coal from high ash coal as
substantially described and illustrated herein with reference to the
accompanying drawings.
9. A system for producing low ash coal from high ash coal as substantially
described and illustrated herein with reference to the accompanying
drawings.

The present invention relates to an improved process to produce low ash coal from high ash coal, comprising the steps of forming a slurry of coal fines in a N-Methyl-2-pyrrolidone (NMP) including Ethylenediamine (EDA), NMP and EDA
being between 6:1 to 24:1 solution, said slurry containing about 6 to 25 ml of solution per g of coal; maintaining said slurry in refluxed condition at a temperature of about 170 °C for a period of about 15 minutes to 2 hours;
separating the refluxed solution in two parts by coarse filtration at 0.025 mm filter cloth a cut size of the separation being variable depending on the particle size filtrate, extract and residue to be treated; cooling the filtered coal-solvent mixture; precipitating the coal by adding acetone in the extract; separating the
coal by filtration, said coal having a reduced ash content; and recovering the rest of the solvent by distillation of the acetone-solvent solution.

Documents:

950-KOL-2009-(23-01-2013)-ABSTRACT.pdf

950-KOL-2009-(23-01-2013)-CLAIMS.pdf

950-KOL-2009-(23-01-2013)-CORRESPONDENCE.pdf

950-KOL-2009-(23-01-2013)-FORM-1.pdf

950-KOL-2009-(23-01-2013)-FORM-2.pdf

950-kol-2009-abstract.pdf

950-kol-2009-claims.pdf

950-KOL-2009-CORRESPONDENCE 1.1.pdf

950-kol-2009-correspondence.pdf

950-kol-2009-description (complete).pdf

950-kol-2009-drawings.pdf

950-KOL-2009-FORM 1 1.1.pdf

950-kol-2009-form 1.pdf

950-kol-2009-form 18.pdf

950-kol-2009-form 2.pdf

950-kol-2009-form 3.pdf

950-kol-2009-form 5.pdf

950-kol-2009-specification.pdf

abstract-950-kol-2009.jpg


Patent Number 260994
Indian Patent Application Number 950/KOL/2009
PG Journal Number 22/2014
Publication Date 30-May-2014
Grant Date 30-May-2014
Date of Filing 07-Jul-2009
Name of Patentee TATA STEEL LIMITED
Applicant Address RESEARCH AND DEVELOPMENT DIVISION, JAMSHEDPUR 831001
Inventors:
# Inventor's Name Inventor's Address
1 VIMAL KUMAR CHANDALIYA TATA STEEL LIMITED, RESEARCH AND DEVELOPMENT DIVISION, JAMSHEDPUR 831001
2 PRADIP KUMAR BANERJEE TATA STEEL LIMITED, RESEARCH AND DEVELOPMENT DIVISION, JAMSHEDPUR 831001
3 PINAKPANI BISWAS TATA STEEL LIMITED, RESEARCH AND DEVELOPMENT DIVISION, JAMSHEDPUR 831001
PCT International Classification Number C10L9/00
PCT International Application Number N/A
PCT International Filing date
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 NA