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US20040244282A1 - Process for removal of organic sulphur from high sulphur coal and a device therefor - Google Patents

Process for removal of organic sulphur from high sulphur coal and a device therefor Download PDF

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Publication number
US20040244282A1
US20040244282A1 US10/814,864 US81486404A US2004244282A1 US 20040244282 A1 US20040244282 A1 US 20040244282A1 US 81486404 A US81486404 A US 81486404A US 2004244282 A1 US2004244282 A1 US 2004244282A1
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United States
Prior art keywords
temperature
reactor
sulphur
coal
furnace
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Abandoned
Application number
US10/814,864
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English (en)
Inventor
Abdul Ali
Atulya Bhattacharya
Sukumar Banerjee
Dina Tiwari
Sushanta Hazra
Rama Yadav
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Council of Scientific and Industrial Research CSIR
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Council of Scientific and Industrial Research CSIR
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Priority to US10/814,864 priority Critical patent/US20040244282A1/en
Assigned to COUNCIL OF SCIENTIFIC AND INDUSTRIAL RESEARCH reassignment COUNCIL OF SCIENTIFIC AND INDUSTRIAL RESEARCH ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: ALI, ABDUL, BANERJEE, SUKUMAR, BHATTACHARYA, ATULYA, HAZRA, SUSHANTA KUMAR, TIWARI, DINA NATH, YADAV, RAMA SHANKAR
Publication of US20040244282A1 publication Critical patent/US20040244282A1/en
Abandoned legal-status Critical Current

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/24Stationary reactors without moving elements inside
    • B01J19/2415Tubular reactors
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/24Stationary reactors without moving elements inside
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10LFUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G OR C10K; LIQUIFIED PETROLEUM GAS; USE OF ADDITIVES TO FUELS OR FIRES; FIRE-LIGHTERS
    • C10L9/00Treating solid fuels to improve their combustion
    • C10L9/08Treating solid fuels to improve their combustion by heat treatments, e.g. calcining
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00051Controlling the temperature
    • B01J2219/00121Controlling the temperature by direct heating or cooling
    • B01J2219/00123Controlling the temperature by direct heating or cooling adding a temperature modifying medium to the reactants
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00051Controlling the temperature
    • B01J2219/00157Controlling the temperature by means of a burner

Definitions

  • the present invention relates to a process for removal of organic sulphur from high sulphur coal and a device therefor.
  • the invention finds its usage in utilizing for power generation in thermal coal plants, briquette making, active carbon and reduction of pollution.
  • Sulphur included within the coals make them undesirable for use without expensive and efficient reducing equipment to recover the products of sulphur by combustion.
  • One of the products of combustion is sulphur dioxide, which is considered to be a highly undesirable pollutant of the atmosphere.
  • sulphur in coal is present in various forms. There are three basic forms, namely; pyritic sulphur, sulphate sulphur and organic sulphur.
  • the pyritic sulphur is sulphur combined with iron.
  • the sulphate sulphur is generally of a minute quantity, that is, it usually constitutes 1% or 2% of all the sulphur in a given coal specimen.
  • Organic sulphur is sulphur, which is combined, in an organic compound with the carbon of the coal.
  • Organic sulphur is generally found to be difficult to remove from coal.
  • U.S. Pat. No. 4,233,034 the problem which confronts most investigators is how to remove organic sulphur from coal.
  • the patent discloses a process for removing sulphur from coal. But process does not distinguish between the removal of organic sulphur from the removal of pyritic sulphur, but the teaching is simply directed to a process of removing sulphur without distinction of what type of sulphur is removed. It is known to remove pyritic sulphur efficiently from coal. The problem revolves around removing the organic sulphur efficiently.
  • the mixture of coal and ethyl alcohol is placed in a reaction vessel, and temperature and pressure in the vessel are raised above the critical temperature and pressure of ethyl alcohol.
  • the mixture is maintained at a temperature and pressure above the critical temperature and pressure for a period of time. Any gas generated is collected and the coal solids of the mixture are separated from the liquid.
  • Prior art search for removal of organic sulphur from coal and a device therefor was made based on literature survey and patent databases, which did not yield any relevant references
  • the main object of the invention is to provide a device for removal of organic sulphur from high sulphur coal which obviates the drawbacks as detailed above.
  • Another object of the invention is a process for removal of organic sulphur from high sulphur coal.
  • the present invention relates to a device for reduction of organic Sulphur from high Sulphur coal which comprises a reactor essentially consisting of three heating zones such as steam heating zone capable of maintaining a temperature in the range of 450-500 degree centigrade, a promoter zone capable of maintaining a temperature of the order of 950-1100 degree centigrade and reaction zone capable of maintaining a temperature in the range of 900-950 degree centigrade, the said reactor being placed inside a tabular furnace capable of providing the above said temperature zones in the said reactor, the said furnace with reactor inside being enclosed in a movable cabinet, the said reactor and furnace being provided with energy regulator and indicators.
  • a reactor essentially consisting of three heating zones such as steam heating zone capable of maintaining a temperature in the range of 450-500 degree centigrade, a promoter zone capable of maintaining a temperature of the order of 950-1100 degree centigrade and reaction zone capable of maintaining a temperature in the range of 900-950 degree centigrade, the said reactor being placed inside a tabular furnace capable of providing the
  • the tabular furnace is made up of Silliminite and insulated by quartz wool.
  • an another embodiment of the present invention relates to a process for removal of organic sulphur from high sulphur coal using the device as claimed in claim 1 which comprises of heating the promoter zone (containing the promoter) at a temperature in the range of 1100 ⁇ 50 degree Celsius and steam zone at a temperature in the range of 450 to 500 degree Celsius, crushing the input coal to ⁇ 72 mesh BS and feeding into the reaction zone, producing steam in a flask, preferably made of glass and passing through the reactor, maintaining the temperature at 900 degree Celsius for about 1 hour, after it attains a temperature of 900 degree Celsius, passing the gas evolved from the reactor through a series of bubblers, preferably made of glass, containing ammoniacal cadmium chloride solution, cooling the furnace to room temperature and discharging the product coke/char.
  • the promoter zone is heated initially at a temperature in the range of 950 to 1000 degree Celsius at the rate of 5 degree Celsius rise in temperature and steam zone at a temperature in the range of 450 to 500 degree Celsius at the rate of 5 degree Celsius rise in temperature.
  • the input coal is crushed ⁇ 72 mesh BS and fed into the reaction zone.
  • Steam is produced in a round bottom flask and passed through the reactor. When temperature attains 900 degree Celsius, it is maintained at that temperature for a time period in the range of 0.5 to 2 hours.
  • the gas evolved is passed through a series of glass bubblers containing ammoniacal cadmium chloride solution resulting in formation of yellow precipitate of cadmium sulphide inside the bubblers.
  • the furnace is cooled to room temperature and the product coke/char is discharged.
  • the present invention provides a process for a device for removal of organic sulphur from high sulphur coal which comprises of a tubular furnace ( 6 ), made of silliminite and insulated by quartz wool ( 5 & 7 ), having outer diameter of 250 mm, internal diameter of 40 mm, length 650 mm with tube bore of 37.5 mm; a reactor, preferably made of silica ( 1 ), having three heating zones viz.
  • steam heating zone ( 2 ) of 17 mm long for maintaining a temperature in the range of 450 to 500 degree Celsius
  • Promoter heating zone ( 3 ) of 250 mm length for maintaining temperature in the range of 950 to 1200 degree Celsius
  • reaction zone ( 4 ) of 200 mm length for temperature in the range of 300 to 1100 degree Celsius
  • the said furnace is fitted with two chrome-aluminium thermocouples, digital temperature indicators with multi point switch and three energy regulators ( 9 ) to control the temperatures of the three zones
  • the said furnace ( 6 ) is fitted with rollers to move freely on rail tracks fitted in a rectangular control cabinet, inside which energy regulators and indicators are fitted
  • a reactor ( 1 ) preferably made of silica, of length 940 mm, internal diameter of 21 mm and outer diameter of 23 mm is inserted into the said furnace
  • a frame ( 8 ) preferably made of mild stainless steel having length of 750 mm, width of 325 mm and depth of 325 mm, for accommodating the
  • the present invention provides a process for removal of organic sulphur from high sulphur coal which comprises of heating the promoter zone at a temperature in the range of 300 to 1100 degree Celsius and steam zone at a temperature in the range of 450 to 500 degree Celsius; crushing the input coal to ⁇ 72 mesh BS and feeding into the reaction zone; producing steam in a flask, preferably made of glass and passing through the reactor; maintaining the at the temperature 900 Celsius for a time period in the range of 0.5 to 2 hours, passing steam after it attains a temperature of 900 degree Celsius; passing the gas evolved from the reactor through a series of bubblers, preferably made of glass, containing ammoniacal cadmium chloride solution; cooling the furnace to room temperature and discharging the product coke/char.
  • the promoter used is mixture of copper-iron turnings in the ratio of 1:9.
  • the rate of rise in temperature in promoter zone and reaction zone is 5 degree Celsius per minute.
  • Novelty of this invention lies in removing of organic sulphur from high sulphur coal, which is otherwise unutilised worldwide
  • Organic sulphur is sulphur, which is combined, in an organic compound with the carbon of the coal.
  • Organic sulphur is generally found to be difficult to remove from coal.
  • Sulphur dioxide which is considered to be a highly undesirable pollutant of the atmosphere.
  • Present invention removes 79.77% of organic sulphur from coal, which is a break through.
  • the Promoter zone and steam zone was heated initially up to 1100 degree Celsius & 450 degree Celsius respectively with increase in temperature being 5 degree Celsius per minute.
  • 10 grams of coal was crushed to ⁇ 72 mesh BS and fed into the reaction zone.
  • 9 g of iron and 1 g of copper turnings were taken in the promoter chamber.
  • Steam was produced in a round bottom flask and passed through the reactor. When the furnace temperature attained 900 degree Celsius, it was maintained at that temperature for one hour.
  • the gas evolved was passed through a series of glass bubblers containing ammoniacal cadmium chloride solution, which resulted in formation of yellow precipitate of cadmium sulphide inside the bubblers.
  • the furnace was cooled to room temperature and the product coke/char was discharged. While the original coal contained 5.39% of organic Sulphur, after the above process it was reduced to 1.17%, resulting overall reduction in organic Sulphur as 78.29%.
  • the promoter zone and steam zone was heated initially up to 1000 degree Celsius & 400 degree Celsius respectively with increase in temperature being 5 degree Celsius.
  • 10 g of coal was crushed to ⁇ 72 mesh BS and fed into the reaction zone.
  • 9 g of iron and 1 g of copper turnings were taken in the promoter chamber.
  • Steam was produced in a round bottom flask and passed through the reactor. When the furnace temperature attained 900 degree Celsius, it was maintained at that temperature for one hour.
  • the gas evolved was passed through a series of glass bubblers containing ammoniacal cadmium chloride solution, which resulted in formation of yellow precipitate of cadmium sulphide inside the bubblers.
  • the furnace was cooled to room temperature and the product coke/char was discharged. While the original coal contained 5.39% of organic Sulphur, after the above process it was reduced to 0.88% resulting overall reduction in organic Sulphur as 79.77%.
  • the promoter zone and steam zone was heated initially up to 900 degree Celsius & 550 degree Celsius respectively with increase in temperature being 5 degree Celsius.
  • 10 g of coal was crushed to ⁇ 72 mesh BS and fed into the reaction zone.
  • 9 g of iron and 1 g of copper turnings were taken in the catalyst chamber.
  • Steam was produced in a round bottom flask and passed through the reactor. When the furnace temperature attained 900 degree Celsius, it was maintained at that temperature for one hour.
  • the gas evolved was passed through a series of glass bubblers containing ammoniacal cadmium chloride solution, which resulted in formation of yellow precipitate of cadmium sulphide inside the bubblers.
  • the furnace was cooled to room temperature and the product coke/char was discharged. While the original coal contained 5.39% of organic Sulphur, after the above process it was reduced to 1.51% resulting overall reduction in organic Sulphur as 71.98%.
  • the promoter zone and steam zone was heated initially up to 600 degree Celsius & 400 degree Celsius respectively with increase in temperature being 5 degree Celsius.
  • 10 grams of coal was crushed to ⁇ 72 mesh BS and fed into the reaction zone.
  • 9 g of iron and 1 g of copper turnings were taken in the catalyst chamber.
  • Steam was produced in a round bottom flask and passed through the reactor. When the furnace temperature attained 900 degree Celsius, it was maintained at that temperature for one hour.
  • the gas evolved was passed through a series of glass bubblers containing ammoniacal cadmium chloride solution, which resulted in formation of yellow precipitate of cadmium sulphide inside the bubblers.
  • the furnace was cooled to room temperature and the product coke/char was discharged. While the original coal contained 3.24% of organic Sulphur, after the above process it was reduced to 2.32%, resulting overall reduction in organic Sulphur as 28.39%.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Combustion & Propulsion (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Solid Fuels And Fuel-Associated Substances (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
US10/814,864 2003-03-31 2004-03-31 Process for removal of organic sulphur from high sulphur coal and a device therefor Abandoned US20040244282A1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
US10/814,864 US20040244282A1 (en) 2003-03-31 2004-03-31 Process for removal of organic sulphur from high sulphur coal and a device therefor

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US45914103P 2003-03-31 2003-03-31
US10/814,864 US20040244282A1 (en) 2003-03-31 2004-03-31 Process for removal of organic sulphur from high sulphur coal and a device therefor

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US10/814,864 Abandoned US20040244282A1 (en) 2003-03-31 2004-03-31 Process for removal of organic sulphur from high sulphur coal and a device therefor

Country Status (7)

Country Link
US (1) US20040244282A1 (fr)
EP (1) EP1622995A1 (fr)
JP (1) JP2006522201A (fr)
KR (1) KR20060006902A (fr)
CN (1) CN1768126A (fr)
AU (1) AU2004225664A1 (fr)
WO (1) WO2004087844A1 (fr)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP4927020B2 (ja) * 2008-04-16 2012-05-09 新日本製鐵株式会社 石炭中硫黄の形態別定量方法
KR100947556B1 (ko) 2008-05-16 2010-03-12 장익병 싸이클 헬스카의 증속장치
CN114517116B (zh) * 2022-02-14 2024-10-22 三门峡市精捷自动化设备有限公司 一种低挥发分煤体热蒸冷淬工艺

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3350845A (en) * 1965-11-18 1967-11-07 Union Carbide Corp Metal alloy for hydrogen separation and purification
US4118201A (en) * 1976-07-14 1978-10-03 Mobil Oil Corporation Production of low sulfur fuels from coal
US4233034A (en) * 1979-05-03 1980-11-11 Union Oil Company Of California Desulfurization of coal
US4409094A (en) * 1980-08-08 1983-10-11 Massachusetts Institute Of Technology Process for detoxifying coal tars
US4441886A (en) * 1982-11-22 1984-04-10 Southern Illinois University Foundation Process for removing organic sulphur from coal and material resulting from the process
US4704134A (en) * 1981-03-24 1987-11-03 Carbon Fuels Corporation Coal derived/aqueous fuel system and method of manufacture
US5178785A (en) * 1990-07-11 1993-01-12 Norton Company Heat sink formulation
US5296007A (en) * 1986-11-17 1994-03-22 Ensci Inc. Process for removing sulfur from coal

Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1136979B (de) * 1955-10-24 1962-09-27 Braunschweigische Kohlen Bergw Verfahren zum Entschwefeln von Koks
GB838605A (en) * 1957-04-04 1960-06-22 Collier Carbon & Chemical Co Apparatus and method for calcining petroleum coke, coal and similar substances containing volatile combustible material
US3361538A (en) * 1964-11-13 1968-01-02 Selas Corp Of America Tube heater
GB1492600A (en) * 1974-01-02 1977-11-23 Occidental Petroleum Corp Process for treating coal to produce a carbon char of low sulphur content
DE2659752C3 (de) * 1976-12-31 1981-04-23 L. & C. Steinmüller GmbH, 5270 Gummersbach Verfahren zum Entschwefeln von auf unter 0,1 mm zerkleinerter Kohle
US4359451A (en) * 1978-09-05 1982-11-16 Occidental Research Corporation Desulfurization of carbonaceous materials
US4270928A (en) * 1978-09-05 1981-06-02 Occidental Research Corporation Desulfurization of carbonaceous materials
JPH11226447A (ja) * 1998-02-12 1999-08-24 Mitsubishi Heavy Ind Ltd 石炭の脱硫方法および装置

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3350845A (en) * 1965-11-18 1967-11-07 Union Carbide Corp Metal alloy for hydrogen separation and purification
US4118201A (en) * 1976-07-14 1978-10-03 Mobil Oil Corporation Production of low sulfur fuels from coal
US4233034A (en) * 1979-05-03 1980-11-11 Union Oil Company Of California Desulfurization of coal
US4409094A (en) * 1980-08-08 1983-10-11 Massachusetts Institute Of Technology Process for detoxifying coal tars
US4704134A (en) * 1981-03-24 1987-11-03 Carbon Fuels Corporation Coal derived/aqueous fuel system and method of manufacture
US4441886A (en) * 1982-11-22 1984-04-10 Southern Illinois University Foundation Process for removing organic sulphur from coal and material resulting from the process
US5296007A (en) * 1986-11-17 1994-03-22 Ensci Inc. Process for removing sulfur from coal
US5178785A (en) * 1990-07-11 1993-01-12 Norton Company Heat sink formulation

Also Published As

Publication number Publication date
CN1768126A (zh) 2006-05-03
KR20060006902A (ko) 2006-01-20
EP1622995A1 (fr) 2006-02-08
JP2006522201A (ja) 2006-09-28
WO2004087844A1 (fr) 2004-10-14
AU2004225664A1 (en) 2004-10-14

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