EP0171298B1 - Verfahren zur Entschwefelung eines Schwefel enthaltenden brennbaren Gases - Google Patents

Verfahren zur Entschwefelung eines Schwefel enthaltenden brennbaren Gases Download PDF

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Publication number
EP0171298B1
EP0171298B1 EP85400298A EP85400298A EP0171298B1 EP 0171298 B1 EP0171298 B1 EP 0171298B1 EP 85400298 A EP85400298 A EP 85400298A EP 85400298 A EP85400298 A EP 85400298A EP 0171298 B1 EP0171298 B1 EP 0171298B1
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EP
European Patent Office
Prior art keywords
gas
manganese
zinc
iron
bath
Prior art date
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.)
Expired
Application number
EP85400298A
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English (en)
French (fr)
Other versions
EP0171298A1 (de
Inventor
Jean Cordier
André Rist
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.)
USINOR SA
Original Assignee
Union Siderurgique du Nord et de lEst de France SA USINOR
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Union Siderurgique du Nord et de lEst de France SA USINOR filed Critical Union Siderurgique du Nord et de lEst de France SA USINOR
Priority to AT85400298T priority Critical patent/ATE40149T1/de
Publication of EP0171298A1 publication Critical patent/EP0171298A1/de
Application granted granted Critical
Publication of EP0171298B1 publication Critical patent/EP0171298B1/de
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Classifications

    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10J—PRODUCTION OF PRODUCER GAS, WATER-GAS, SYNTHESIS GAS FROM SOLID CARBONACEOUS MATERIAL, OR MIXTURES CONTAINING THESE GASES; CARBURETTING AIR OR OTHER GASES
    • C10J3/00—Production of combustible gases containing carbon monoxide from solid carbonaceous fuels
    • C10J3/57—Gasification using molten salts or metals
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10J—PRODUCTION OF PRODUCER GAS, WATER-GAS, SYNTHESIS GAS FROM SOLID CARBONACEOUS MATERIAL, OR MIXTURES CONTAINING THESE GASES; CARBURETTING AIR OR OTHER GASES
    • C10J3/00—Production of combustible gases containing carbon monoxide from solid carbonaceous fuels
    • C10J3/72—Other features
    • C10J3/82—Gas withdrawal means
    • C10J3/84—Gas withdrawal means with means for removing dust or tar from the gas
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10K—PURIFYING OR MODIFYING THE CHEMICAL COMPOSITION OF COMBUSTIBLE GASES CONTAINING CARBON MONOXIDE
    • C10K1/00—Purifying combustible gases containing carbon monoxide
    • C10K1/002—Removal of contaminants
    • C10K1/003—Removal of contaminants of acid contaminants, e.g. acid gas removal
    • C10K1/004—Sulfur containing contaminants, e.g. hydrogen sulfide
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10K—PURIFYING OR MODIFYING THE CHEMICAL COMPOSITION OF COMBUSTIBLE GASES CONTAINING CARBON MONOXIDE
    • C10K1/00—Purifying combustible gases containing carbon monoxide
    • C10K1/04—Purifying combustible gases containing carbon monoxide by cooling to condense non-gaseous materials
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10K—PURIFYING OR MODIFYING THE CHEMICAL COMPOSITION OF COMBUSTIBLE GASES CONTAINING CARBON MONOXIDE
    • C10K1/00—Purifying combustible gases containing carbon monoxide
    • C10K1/20—Purifying combustible gases containing carbon monoxide by treating with solids; Regenerating spent purifying masses
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10J—PRODUCTION OF PRODUCER GAS, WATER-GAS, SYNTHESIS GAS FROM SOLID CARBONACEOUS MATERIAL, OR MIXTURES CONTAINING THESE GASES; CARBURETTING AIR OR OTHER GASES
    • C10J2300/00—Details of gasification processes
    • C10J2300/09—Details of the feed, e.g. feeding of spent catalyst, inert gas or halogens
    • C10J2300/0913—Carbonaceous raw material
    • C10J2300/093—Coal
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10J—PRODUCTION OF PRODUCER GAS, WATER-GAS, SYNTHESIS GAS FROM SOLID CARBONACEOUS MATERIAL, OR MIXTURES CONTAINING THESE GASES; CARBURETTING AIR OR OTHER GASES
    • C10J2300/00—Details of gasification processes
    • C10J2300/09—Details of the feed, e.g. feeding of spent catalyst, inert gas or halogens
    • C10J2300/0913—Carbonaceous raw material
    • C10J2300/0943—Coke
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10J—PRODUCTION OF PRODUCER GAS, WATER-GAS, SYNTHESIS GAS FROM SOLID CARBONACEOUS MATERIAL, OR MIXTURES CONTAINING THESE GASES; CARBURETTING AIR OR OTHER GASES
    • C10J2300/00—Details of gasification processes
    • C10J2300/09—Details of the feed, e.g. feeding of spent catalyst, inert gas or halogens
    • C10J2300/0953—Gasifying agents
    • C10J2300/0959—Oxygen
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10J—PRODUCTION OF PRODUCER GAS, WATER-GAS, SYNTHESIS GAS FROM SOLID CARBONACEOUS MATERIAL, OR MIXTURES CONTAINING THESE GASES; CARBURETTING AIR OR OTHER GASES
    • C10J2300/00—Details of gasification processes
    • C10J2300/09—Details of the feed, e.g. feeding of spent catalyst, inert gas or halogens
    • C10J2300/0953—Gasifying agents
    • C10J2300/0973—Water
    • C10J2300/0976—Water as steam
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10J—PRODUCTION OF PRODUCER GAS, WATER-GAS, SYNTHESIS GAS FROM SOLID CARBONACEOUS MATERIAL, OR MIXTURES CONTAINING THESE GASES; CARBURETTING AIR OR OTHER GASES
    • C10J2300/00—Details of gasification processes
    • C10J2300/09—Details of the feed, e.g. feeding of spent catalyst, inert gas or halogens
    • C10J2300/0983—Additives

Definitions

  • the present invention relates to a process for desulfurization of a combustible synthesis gas containing sulfur, such as in particular a combustible gas obtained by gasification of coals or petroleum residues.
  • the invention relates in particular to a combustible gas obtained by gasifying coal on a bath of ferrous metal maintained in the liquid state, the coal being injected in a sprayed form into the metal bath by an injection lance, simultaneously with gaseous oxygen and vapor.
  • the gas thus produced contains a residual content of sulfur compounds in particular in the form of H 2 S and COS which is of the order of 100 to 600 ppmv in H 2 S + COS. It may be noted that, with respect to the sulfur content of the gas initially produced, a first significant desulfurization by iron has already taken place to transform the sulfur compounds into iron sulfide, but this desulfurization is insufficient for certain uses of the gas.
  • the present invention aims to solve this problem of advanced desulfurization of a combustible gas resulting from the gasification of sulfurous fuels.
  • Manganese desulphurization is preferably carried out by bringing the combustible gas into contact with the vapors of Mn and / or its oxides in the form of aerosols while it is at a temperature ranging from 1600 ° C. to 600 ° C.
  • Desulfurization with zinc is also preferably carried out by bringing the combustible gas into contact with zinc vapors and / or its oxides in the form of aerosols while it is at a temperature ranging from 1000 ° C. to 350 °. vs.
  • the sulfur content of the gas cooled in the presence of iron aerosols and of iron oxide is reduced to values of between 100 and 600 ppmv of sulfur, in the form of H 2 S, of COS, etc.
  • the sulfur is eliminated, by purification and thorough dedusting of the gas, in the form of iron sulfides and oxysulfides.
  • the subject of the invention is a process for the advanced desulfurization of a combustible gas containing sulfur resulting from the gasification of sulfurous fuel on a bath of ferrous metal maintained in the liquid state in which said combustible gas is subjected to desulfurization by iron vapors, then to a desulfurization by manganese vapors, while it is at a temperature ranging from 1600 ° C to 350 ° C, characterized in that the desulfurization is completed by bringing this gas into contact with vapors of zinc and / or its oxides in the form of aerosols, downstream of the points of contact with iron and manganese, said combustible gas being at a temperature ranging from 1000 ° C. to 350 ° C.
  • the reaction can continue up to 600 ° C and even 400 ° C, the residual sulfur content is extremely low; on the order of a few ppmv.
  • Zinc is an even more effective desulfurizer than manganese at less than 950 ° C. It completes the action of the manganese vapors introduced into the gas. From 850 ° C, zinc sulphide is more stable than manganese sulphide and zinc vapors, in aerosols quickly fix the sulfur of the gas in the form of sulphide and oxysulphides. zinc, so that at 800 ° C the gas contains less than 10 ppmv sulfur. At 600 ° C, the residual sulfur content in the gas is less than a few ppmv.
  • the sulfur is removed from the gas, purified and dusted, in the form of fine sulphide dust and oxysulphides of zinc, manganese and iron.
  • FIG. 1 is a graph illustrating the separate action of the vapors of Fe, Mn and Zn on the desulphurization of a gas resulting from the steel gasification of coal in which the initial sulfur content is 4000 ppmv and the initial content in each of metals (M) is 0.5 to 1 g / N m3.
  • the iron bath be maintained at a temperature between 1500 ° C and 1550 ° C.
  • manganese is added to the gasification zone while the gas is maintained at a temperature ranging from 1600 ° C. to 600 °. vs.
  • the Mn can be added in the form of an oxide such as, for example, a concentrate or a manganese ore, directly mixed with the pulverized coal injected by the lance.
  • Mn can also be added to the bath in the form of ferro-manganese or apt or any other alloy containing Mn.
  • the Mn content of the bath is preferably maintained between 0.5 and 1.5% and for example around 0.8%.
  • the manganese introduced is rapidly vaporized and ensures desulfurization of the bath at the same time as gas (which can only be ensured by desulfurization with iron vapors which only intervenes lower temperature as indicated above).
  • the action of desulphurization of manganese is completed by the addition of Zn vapors which react when the gas is at a temperature below 1000 ° C and up to 350 ° C.
  • This bringing the gas into contact with the Zn vapors can be carried out according to two variants.
  • Zinc introduced into a high temperature zone, is completely volatilized. However, its consumption is not negligible because it occurs, as explained above, at a temperature below about 950 ° C in competition with the manganese aerosol, while the sulfur content of the gas is still around from 20 to 40 ppmv of sulfur compounds.
  • a plasma torch which injects the vapor of Zn into the gas when the latter is at a temperature below 600 ° C., when the manganese has already reduced the sulfur content of the gas below 10 ppmv.
  • Fig. 2 is a graph illustrating the simultaneous action of the vapors of Mn and Zn on the desulphurization of a gas resulting from the steel gasification of coal in which the initial sulfur content is 4000 ppmv (COS + H 2 S + ... ), the Mn content being greater than 0.3 g / m 3 N and in particular from 0.5 to 1 g / m 3 N, the Zn content being greater than 0.01 g / m 3 N, in particular from 0.05 to 0.1 g / m 3 N.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Combustion & Propulsion (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Industrial Gases (AREA)
  • Treating Waste Gases (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Gas Separation By Absorption (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)

Claims (5)

1. Verfahren zur ausgedehnten Entschwefelung eines schwefelhaltigen brennbaren Gases, welches aus der Vergasung von schwefelhaltigem Brennstoff über einem Bad aus in flüssigem Zustand gehaltenem eisenhaltigem Metall hervorgegangen ist, bei welchem man das brennbare Gas einer Entschwefelung durch Eisendämpfe, außerdem einer Entschwefelung durch Mangandämpfe unterwirft, während es auf einer von 1600°C bis 350°C gehenden Temperatur gehalten wird, dadurch gekennzeichnet, daß die Entschwefelung vervollständigt wird, indem dieses Gas mit Dämpfen von Zink und/ oder seinen Oxiden in Form von Aerosolen strömungsunterhalb der Stellen des Inberührungbringens mit dem Eisen und dem Mangan in Berührung gebracht wird, wobei das brennbare Gas auf einer von 1000°C bis 350°C gehenden Temperatur ist.
2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß das Gas ein Gas ist, welches aus der Vergasung von Kohle und/oder Mineralölrückständen üben einem Bad aus schwefelhaltigem Metall stammt, das in flüssigem Zustand und auf einer Temperatur von 1300°C bis 1600°C, vorzugsweise 1450° bis 1500°C, je nach Schwefelgehalt des Gases, gehalten wird.
3. Verfahren nach den Ansprüchen 1 und 2, dadurch gekennzeichnet, daß das Mangan der zu vergasenden Kohle in Form feiner Manganerze zugesetzt wird.
4. Verfahren nach den Ansprüchen 1 und 2, dadurch gekennzeichnet, daß das Mangan über dem Bad aus in flüssigem Zustand gehaltenem schwefelhaltigem Metall in Form von Ferromangan oder einer Mn-Legierung zugesetzt wird.
5. Verfahren nach irgendeinem der Ansprüche 1 bis 4, dadurch gekennzeichnet, daß das Zink mit dem zuvor entschwefelten Gas in Form von durch einen Plasmabrenner erzeugten Zinkdämpfen in Berührung gebracht wird, wobei das Gas auf einer Temperatur unter 600°C ist.
EP85400298A 1984-02-23 1985-02-19 Verfahren zur Entschwefelung eines Schwefel enthaltenden brennbaren Gases Expired EP0171298B1 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT85400298T ATE40149T1 (de) 1984-02-23 1985-02-19 Verfahren zur entschwefelung eines schwefel enthaltenden brennbaren gases.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR8402769A FR2560209B1 (fr) 1984-02-23 1984-02-23 Procede de desulfuration d'un gaz combustible contenant du soufre
FR8402769 1984-02-23

Publications (2)

Publication Number Publication Date
EP0171298A1 EP0171298A1 (de) 1986-02-12
EP0171298B1 true EP0171298B1 (de) 1989-01-18

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ID=9301324

Family Applications (1)

Application Number Title Priority Date Filing Date
EP85400298A Expired EP0171298B1 (de) 1984-02-23 1985-02-19 Verfahren zur Entschwefelung eines Schwefel enthaltenden brennbaren Gases

Country Status (11)

Country Link
US (1) US4852995A (de)
EP (1) EP0171298B1 (de)
JP (1) JPS617390A (de)
AT (1) ATE40149T1 (de)
AU (1) AU581423B2 (de)
BR (1) BR8500791A (de)
CA (1) CA1287479C (de)
DE (1) DE3567673D1 (de)
FR (1) FR2560209B1 (de)
IN (1) IN164158B (de)
ZA (1) ZA851355B (de)

Families Citing this family (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS61221292A (ja) * 1985-03-27 1986-10-01 Sumitomo Metal Ind Ltd 低硫黄含有石炭ガス化ガスの製造方法
US5538703A (en) * 1993-10-29 1996-07-23 Massachusetts Institute Of Technology Hot gas desulfurization by injection of regenerable sorbents in gasifier-exit ducts
US5581085A (en) * 1995-03-06 1996-12-03 Spectra-Tech, Inc. Infrared microspectrometer accessory
GB9602037D0 (en) * 1996-02-01 1996-04-03 Univ Birmingham Desulphurisation
US5980606A (en) * 1996-03-22 1999-11-09 Steel Technology Corporation Method for reducing sulfuric content in the offgas of an iron smelting process
US6693280B2 (en) 2001-08-03 2004-02-17 Sensir Technologies, L.L.C. Mid-infrared spectrometer attachment to light microscopes
US8597934B2 (en) * 2009-10-30 2013-12-03 Coskata, Inc. Process for controlling sulfur in a fermentation syngas feed stream
US9847543B2 (en) 2013-03-06 2017-12-19 Fuelcell Energy, Inc. Fuel cell system having biogas desulfurizer assembly with manganese oxide desulfurizer material

Family Cites Families (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2612444A (en) * 1948-12-28 1952-09-30 Rummel Roman Production of metals from their ores
US2858255A (en) * 1953-03-23 1958-10-28 Segui Esteban Domingo Process and device for the regeneration of monomers starting from polymethacrylate and, more especially, methyl polymethacrylate
US3983218A (en) * 1970-11-18 1976-09-28 Heins Sidney M Method for dry removal of sulfur dioxide from furnace flue, coal and other gases
GB1568703A (en) * 1976-03-29 1980-06-04 British Gas Corp Sulphur purification process
DE2620454A1 (de) * 1976-05-08 1977-11-24 Kloeckner Humboldt Deutz Ag Verfahren zum vergasen von kohlenstoffhaltigen brennstoffen zur herstellung eines reduktionsgases
US4180549A (en) * 1976-08-27 1979-12-25 United States Steel Corporation Desulfurization of hot reducing gas
US4141694A (en) * 1977-08-26 1979-02-27 Technology Application Services Corporation Apparatus for the gasification of carbonaceous matter by plasma arc pyrolysis
DE2843997A1 (de) * 1978-10-09 1980-04-10 Kloeckner Humboldt Deutz Ag Verfahren zur herstellung von spaltgas in einem metallbad
DE3032043A1 (de) * 1980-08-26 1982-03-04 Klöckner-Werke AG, 4100 Duisburg Verfahren zur entschwefelung bei der gaserzeugung im eisenbadreaktor
JPS5794092A (en) * 1980-12-01 1982-06-11 Sumitomo Metal Ind Ltd Method for operating coal gasification furnace
SE426074B (sv) * 1981-04-21 1982-12-06 Boliden Ab Forfarande for att avlegsna svavel vid forgasning i metallsmeltor av kolhaltiga material innehallande svavel

Also Published As

Publication number Publication date
JPS617390A (ja) 1986-01-14
CA1287479C (en) 1991-08-13
FR2560209A1 (fr) 1985-08-30
BR8500791A (pt) 1985-10-08
FR2560209B1 (fr) 1986-11-14
AU581423B2 (en) 1989-02-23
IN164158B (de) 1989-01-21
ZA851355B (en) 1985-10-30
US4852995A (en) 1989-08-01
AU3902685A (en) 1985-09-05
EP0171298A1 (de) 1986-02-12
ATE40149T1 (de) 1989-02-15
DE3567673D1 (en) 1989-02-23

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