WO1998017374A1 - Method and agent for desulphurisation - Google Patents

Method and agent for desulphurisation Download PDF

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Publication number
WO1998017374A1
WO1998017374A1 PCT/GB1997/002735 GB9702735W WO9817374A1 WO 1998017374 A1 WO1998017374 A1 WO 1998017374A1 GB 9702735 W GB9702735 W GB 9702735W WO 9817374 A1 WO9817374 A1 WO 9817374A1
Authority
WO
WIPO (PCT)
Prior art keywords
agent
compound
desulphurisation
manganese
iron
Prior art date
Application number
PCT/GB1997/002735
Other languages
French (fr)
Inventor
Rodney Martin Sambrook
Original Assignee
Dytech Corporation Ltd.
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 Dytech Corporation Ltd. filed Critical Dytech Corporation Ltd.
Priority to BR9712408-7A priority Critical patent/BR9712408A/en
Priority to AU45664/97A priority patent/AU4566497A/en
Priority to EP97944019A priority patent/EP0946259A1/en
Priority to CA002266458A priority patent/CA2266458A1/en
Priority to JP10519058A priority patent/JP2001502236A/en
Publication of WO1998017374A1 publication Critical patent/WO1998017374A1/en

Links

Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/76Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/84Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/889Manganese, technetium or rhenium
    • B01J23/8892Manganese
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34Chemical or biological purification of waste gases
    • B01D53/74General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/86Catalytic processes
    • B01D53/8603Removing sulfur compounds

Definitions

  • the invention relates to desulphurisation and in particular to the purification of streams (liquid or gas or both) by the partial or complete removal of sulphur compounds, e.g. hydrogen sulphide, low molecular weight mercaptans, or the like therefrom.
  • sulphur compounds e.g. hydrogen sulphide, low molecular weight mercaptans, or the like therefrom.
  • the invention may also be applied to the purification of air or other gas containing sulphur compounds.
  • the invention relates to a method and a desulphurisation agent.
  • the invention provides a method of reducing the content of a sulphur compound in stream of gas and/or liquid, the method comprising contacting the stream with a desulphurisation agent comprising at least one compound of manganese and at least one compound of iron.
  • the desulphurisation may be performed, for example, at a temperature from about ambient up to about 450°C, preferably from about 20°C to about 450°C, most preferably from about 40°C to about 150°C.
  • the compounds are the oxides, hydroxides, carbonates, e.g. hydroxycarbonate or basic carbonate or the like of both manganese and iron.
  • These active ingredients may be incorporated within a carrier of the invention by simple impregnation or impregnation/deposition, co forming, precipitation from aqueous solution or other techniques well known to those skilled in the art of catalyst preparation.
  • the carrier may be alumina, sihca, alumino silicates or the like.
  • the content of the carrier material will be in the range 1 to 40% by weight.
  • the compounds are in the relative molar proportions of 8:1 to 1 :8, most preferably about 1 :1.
  • the desulphurisation agent comprises shaped particles.
  • the particles may be presented in a variety of shapes and sizes preferably as spheres; extrudates, granules, tablets or the like.
  • a binding agent such as cement, alumina, clay, sihca, orgamc resins or the like may be present to enhance the physical properties of the shaped material.
  • the shaped material may require exposure to elevated temperatures to achieve the optimum bond strength.
  • the agent includes a promoter which is one or more of potassium hydroxide, nickel hydroxide and sodium hydroxide, optionally with a derivative of zinc.
  • the concentration of the promoter is preferably in the range of from about 1% to about 10%.
  • the inclusion of copper or copper compounds has proved to be beneficial because it will scavenge lower concentrations of sulphur compounds and also remove arsine.
  • the shaped desulphurisation agent is porous.
  • the pore volume will be in the range of 0.1 to 0.6 ml/g, preferably 0.25-0.45 ml/g. It is recognised that the shaped porous materials should exhibit a significant level of macro porosity.
  • the desulphurisation agent may be used in a fixed bed, a fluid bed or a moving bed.
  • the choice of the reactor system will depend on generated requirements and the nature of the gas stream, e.g. sour feed. Particle sizes of about 3 to about 6mm are particularly useful in a fixed bed. In a fluid bed, the particle size is preferably in the range about 20 to about 120 microns, most preferably about 30 to about 100 microns.
  • the particle size is preferably in the range about 120 to 600
  • microns most preferably about 200 to about 500 microns.
  • the method of the invention may be enhanced by the incorporation of materials with
  • Such materials may be added according to the physical form of the desulphurisation agent. They may be added on to the surface or within the pores of a porous desulphurisation agent or in the bulk phase. Such materials may be catalytically
  • the materials may be incorporated within the material of the invention by impregnation, deposition, coforming, precipitation techniques well known to those skilled in the art of catalyst
  • the content of the sorption materials may range from about 0.5 to 40%
  • One such reagent is an alkaline reagent
  • alkah metal hydroxide or silicate such as alkah metal hydroxide or silicate
  • the alkah metal is preferably sodium.
  • Such an alkaline reagent will react with halides or strongly acidic gases present in the sour
  • reagents may be impregnated into the desulphurisation agent or incorporated into the bulk phase by other means well known to those skilled in the art of catalyst preparation.
  • the spent desulphurisation agent of the invention may be regenerated by exposure to an oxidising atmosphere e.g. air at elevated temperature.
  • an oxidising atmosphere e.g. air at elevated temperature.
  • the presence of steam when regenerating may be beneficial.
  • the method of the present invention includes the further step of exposing the spent agent to oxidation at elevated temperature to remove the sulphur compounds and regenerate the agent for re-use.
  • the sulphur compound to be removed may be hydrogen sulphide gas or a low molecular weight mercaptan such as propyl mercaptan.
  • the hydrocarbon stream may be liquid or gas or both, examples being natural gas, town gas, industrial waste gas, coke oven gas, coal gas, liquid or gas from petroleum plant oil refinery. Effluent streams from biomass digesters, general industrial process may also be treated.
  • the method may be performed at pressures ranging from about atmospheric to about
  • the invention provides a desulphurisation agent comprising at least one compound of manganese and at least one compound of iron in the relative molar proportions of from about 8:1 to 1 :8 (Mn:Fe).
  • a desulphurisation agent comprising at least one compound of manganese and at least one compound of iron in the relative molar proportions of from about 8:1 to 1 :8 (Mn:Fe).
  • the invention provides such an agent incorporating a promoter and in yet a further aspect the invention provides such an agent incorporating a sorption material.
  • Pellets of varying composition were prepared by standard forming techniques, calcined at 450OC and allowed to cool.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Environmental & Geological Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Biomedical Technology (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Gas Separation By Absorption (AREA)
  • Industrial Gases (AREA)

Abstract

Sulphur compounds are removed from a gas and/or liquid stream by an agent comprising at least one compound of manganese and at least one compound of iron. Desulphurization agent comprising at least one compound of manganese and at least one of iron, present in relative molar proportions of about 8:1 to 1:8.

Description

METHOD AND AGENT FOR DESULPHURISATION
The invention relates to desulphurisation and in particular to the purification of streams (liquid or gas or both) by the partial or complete removal of sulphur compounds, e.g. hydrogen sulphide, low molecular weight mercaptans, or the like therefrom. The invention may also be applied to the purification of air or other gas containing sulphur compounds. The invention relates to a method and a desulphurisation agent.
In one aspect the invention provides a method of reducing the content of a sulphur compound in stream of gas and/or liquid, the method comprising contacting the stream with a desulphurisation agent comprising at least one compound of manganese and at least one compound of iron.
The desulphurisation may be performed, for example, at a temperature from about ambient up to about 450°C, preferably from about 20°C to about 450°C, most preferably from about 40°C to about 150°C. Preferably the compounds are the oxides, hydroxides, carbonates, e.g. hydroxycarbonate or basic carbonate or the like of both manganese and iron. These active ingredients may be incorporated within a carrier of the invention by simple impregnation or impregnation/deposition, co forming, precipitation from aqueous solution or other techniques well known to those skilled in the art of catalyst preparation. The carrier may be alumina, sihca, alumino silicates or the like. The content of the carrier material will be in the range 1 to 40% by weight. Preferably the compounds are in the relative molar proportions of 8:1 to 1 :8, most preferably about 1 :1.
In a preferred feature the desulphurisation agent comprises shaped particles. The particles may be presented in a variety of shapes and sizes preferably as spheres; extrudates, granules, tablets or the like. A binding agent such as cement, alumina, clay, sihca, orgamc resins or the like may be present to enhance the physical properties of the shaped material. The shaped material may require exposure to elevated temperatures to achieve the optimum bond strength. Preferably the agent includes a promoter which is one or more of potassium hydroxide, nickel hydroxide and sodium hydroxide, optionally with a derivative of zinc. The concentration of the promoter is preferably in the range of from about 1% to about 10%. The inclusion of copper or copper compounds has proved to be beneficial because it will scavenge lower concentrations of sulphur compounds and also remove arsine.
In a further preferred feature the shaped desulphurisation agent is porous. The pore volume will be in the range of 0.1 to 0.6 ml/g, preferably 0.25-0.45 ml/g. It is recognised that the shaped porous materials should exhibit a significant level of macro porosity.
The desulphurisation agent may be used in a fixed bed, a fluid bed or a moving bed. The choice of the reactor system will depend on generated requirements and the nature of the gas stream, e.g. sour feed. Particle sizes of about 3 to about 6mm are particularly useful in a fixed bed. In a fluid bed, the particle size is preferably in the range about 20 to about 120 microns, most preferably about 30 to about 100 microns.
For the moving bed, the particle size is preferably in the range about 120 to 600
microns, most preferably about 200 to about 500 microns.
The method of the invention may be enhanced by the incorporation of materials with
sorption properties. Such materials may be added according to the physical form of the desulphurisation agent. They may be added on to the surface or within the pores of a porous desulphurisation agent or in the bulk phase. Such materials may be catalytically
active. The materials (which may be included either singly or in combination) are
preferably oxides, carbonates, sihcates, phosphates of alkah metals, alkaline earths, rare
earths, Zn, Co, Ni, Mo, Cr, Cu, Ti, Zr, Si, Al, precious metals. The materials may be incorporated within the material of the invention by impregnation, deposition, coforming, precipitation techniques well known to those skilled in the art of catalyst
preparation. The content of the sorption materials may range from about 0.5 to 40%
by weight, preferably in the range 2 to 20% by weight.
In a preferred feature of the invention, other reagents are associated with the
desulphurisation agent to react with other substances present in the stream to be
treated at from about ambient to about 250°C. One such reagent is an alkaline reagent
such as alkah metal hydroxide or silicate, the alkah metal is preferably sodium. Such an alkaline reagent will react with halides or strongly acidic gases present in the sour
feed such as SOx to form halide or sulphite respectively (which may be recovered later). The reagents may be impregnated into the desulphurisation agent or incorporated into the bulk phase by other means well known to those skilled in the art of catalyst preparation.
The spent desulphurisation agent of the invention may be regenerated by exposure to an oxidising atmosphere e.g. air at elevated temperature. The presence of steam when regenerating may be beneficial.
In another aspect the method of the present invention includes the further step of exposing the spent agent to oxidation at elevated temperature to remove the sulphur compounds and regenerate the agent for re-use.
The sulphur compound to be removed may be hydrogen sulphide gas or a low molecular weight mercaptan such as propyl mercaptan. The hydrocarbon stream may be liquid or gas or both, examples being natural gas, town gas, industrial waste gas, coke oven gas, coal gas, liquid or gas from petroleum plant oil refinery. Effluent streams from biomass digesters, general industrial process may also be treated.
The method may be performed at pressures ranging from about atmospheric to about
100 atmospheres without adverse effect.
In another aspect the invention provides a desulphurisation agent comprising at least one compound of manganese and at least one compound of iron in the relative molar proportions of from about 8:1 to 1 :8 (Mn:Fe). In a further aspect the invention provides such an agent incorporating a promoter and in yet a further aspect the invention provides such an agent incorporating a sorption material.
In order that the invention may be well understood it will now be described by way of illustration with reference to the following example.
Example I
Pellets of varying composition, as detailed below, were prepared by standard forming techniques, calcined at 450OC and allowed to cool.
Component, Wt. % A B C D manganese dioxide 5 38 iron oxide 80 70 70 10 sodium hydroxide 10 5 2 binder 20 20 20 20
30 ml. of each sample were placed in a tubular reactor subjected to a flow (3 litres/hour) of nitrogen containing 20% hydrogen sulphide at ambient temperature and pressure and the time noted for 10 ppm hydrogen sulphide to be detected at the outlet of the reactor. The following results were obtained.
Sample time mins
A 62
B 74
C 92
D 330 It will be observed that when both Mn and Fe were present the time increased and that this increase was greatly improved when more manganese was present.

Claims

1. A method of reducing the content of a sulphur compound in stream of gas
and/or hquid, the method comprising contacting the stream with a
desulphurisation agent comprising at least one compound of manganese and at least one compound of iron.
2. A method according to Claim 1 , wherein the contact is made at a temperature
of from about ambient to about 450°C.
3. A method according to Claim 2, wherein the contact temperature is from about
20°C to about 450°C.
4. A method according to Claim 3, wherein the contact temperature is from about
40°C to 450°C.
5. A method according to Claim 4, wherein the contact temperature is from about
40°C to about 150°C.
6. A method according to any preceding Claim, wherein desulphurisation agent
comprises an oxide, hydroxide or carbonate of each of manganese and iron.
7. A method according to Claim 6, wherein the relative molar proportions of manganese compound to iron compound are from 8:1 to 1 :8 (Mn:Fe).
8. A method according to Claim 7, wherein the relative molar proportions are about 1 :1.
9. A method according to any preceding Claim, wherein the manganese compound and the iron compound are presented together in the form of bonded particles.
10. A method according to Claim 9, wherein the particles are bonded by a bonding agent which is a cement, alumina or a clay; sihca; organic resin; or the like.
11. A method according to any preceding Claim, wherein the desulphurisation agent includes a promoter which is a hydroxide of a potassium, nickel and sodium, optionally with a compound of zinc.
12. A method according to any preceding Claim, wherein the desulphurisation agent includes copper or a compound thereof as a scavenger.
13. A method according to any preceding Claim, wherein a sorption material is present in or on the desulphurisation agent.
14. A method according to Claim 13, wherein the content of sorption material is from 0.5% by weight to about 40% by weight of the agent.
15. A method according to any preceding Claim, wherein the desulphurisation
agent is present in the form of particles from about 3mm to about 6mm in a fixed bed.
16. A method according to any of Claims 1 to 14, wherein the desulphurisation
agent is present in the form of particles from about 20 to about 120 microns in a fluid bed.
17. A method according to any of Claims 1 to 14, wherein the desulphurisation agent is present in the form of particles from about 120 microns to about 600
microns, in a moving bed.
18. A method according to any preceding Claim, wherein the desulphurisation agent is associated with an alkaline reagent to react with a hahde or strongly
acidic gas in the stream.
19. A method according to Claim 18, wherein the alkaline reagent is an alkah metal
hydroxide or silicate.
20. A method according to Claim 18 or 19, wherein the alkaline reagent is
contacted with the stream at a temperature of from about ambient to about
250°C.
21. A method according to any preceding Claim, including the step of regenerating the spent desulphurisation agent.
22. A method according to Claim 20, wherein the spent agent is regenerated by contact with air or steam at elevated temperature.
23. A desulphurisation agent comprising at least one compound of manganese and at least one of iron, present in relative molar proportions of about 8:1 to 1 :8.
24. An agent according to Claim 23, wherein the molar proportions are about 1 :1.
25. An agent according to Claim 23 or 24, including a promoter.
26. An agent according to Claim 23, 24 or 25, including a sorption material.
27. An agent according to any of Claims 23 to 26, including an alkaline reagent.
PCT/GB1997/002735 1996-10-21 1997-10-06 Method and agent for desulphurisation WO1998017374A1 (en)

Priority Applications (5)

Application Number Priority Date Filing Date Title
BR9712408-7A BR9712408A (en) 1996-10-21 1997-10-06 Method and agent for desulfurization
AU45664/97A AU4566497A (en) 1996-10-21 1997-10-06 Method and agent for desulphurisation
EP97944019A EP0946259A1 (en) 1996-10-21 1997-10-06 Method and agent for desulphurisation
CA002266458A CA2266458A1 (en) 1996-10-21 1997-10-06 Method and agent for desulphurisation
JP10519058A JP2001502236A (en) 1996-10-21 1997-10-06 Sulfur removal method and chemicals

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
GB9621906.8 1996-10-21
GBGB9621906.8A GB9621906D0 (en) 1996-10-21 1996-10-21 Desulphurisation

Publications (1)

Publication Number Publication Date
WO1998017374A1 true WO1998017374A1 (en) 1998-04-30

Family

ID=10801748

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/GB1997/002735 WO1998017374A1 (en) 1996-10-21 1997-10-06 Method and agent for desulphurisation

Country Status (7)

Country Link
EP (1) EP0946259A1 (en)
JP (1) JP2001502236A (en)
AU (1) AU4566497A (en)
BR (1) BR9712408A (en)
CA (1) CA2266458A1 (en)
GB (2) GB9621906D0 (en)
WO (1) WO1998017374A1 (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2008040966A1 (en) 2006-10-02 2008-04-10 M-I Drilling Fluids Uk Limited Method of forming an agent and its use in desulphurisation
WO2018156006A1 (en) * 2017-02-22 2018-08-30 Instituto Nacional De Investigación Forestales, Agrícolas Y Pecuarias Low-temperature removal of h2s using large-surface-area nano-ferrites obtained using a modified chemical coprecipitation method

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7105140B2 (en) * 2002-03-04 2006-09-12 Conocophillips Company Desulfurization compositions

Citations (2)

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GB1144071A (en) * 1965-02-10 1969-03-05 Grillo Werke Ag Process for the removal of sulphur-containing compounds from industrial gases
EP0078576A1 (en) * 1981-10-30 1983-05-11 Nederlandse Organisatie voor toegepast-natuurwetenschappelijk onderzoek TNO Process for removing hydrogen sulphide from process gases using solid acceptors, process for cyclic regenerating the used acceptors at high temperature, as well as process for preparing acceptors, which are suitable for this process

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JPS56100622A (en) * 1980-01-17 1981-08-12 Hitachi Zosen Corp Dry desulfurizing method in reducing atmosphere
DE3228481A1 (en) * 1982-07-30 1984-02-02 VEG-Gasinstituut N.V., 7300 Apeldoorn REACTION MEASURES, METHOD FOR THEIR PRODUCTION AND THEIR USE
GB2125779B (en) * 1982-08-19 1986-01-29 Nippon Shokubai Kagaku Gogyo C Desulfurization of h2s-containing gases
GB2152489B (en) * 1983-05-26 1986-10-08 Azerb I Nefti Khimii Im M Aziz Method for purifying gases from sulphurous compounds
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GB1144071A (en) * 1965-02-10 1969-03-05 Grillo Werke Ag Process for the removal of sulphur-containing compounds from industrial gases
US3492083A (en) * 1965-02-10 1970-01-27 Grillo Werke Ag Process for the removal of sulphur from industrial gases and to apparatus for use in such a process
EP0078576A1 (en) * 1981-10-30 1983-05-11 Nederlandse Organisatie voor toegepast-natuurwetenschappelijk onderzoek TNO Process for removing hydrogen sulphide from process gases using solid acceptors, process for cyclic regenerating the used acceptors at high temperature, as well as process for preparing acceptors, which are suitable for this process

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2008040966A1 (en) 2006-10-02 2008-04-10 M-I Drilling Fluids Uk Limited Method of forming an agent and its use in desulphurisation
EP2402069A1 (en) 2006-10-02 2012-01-04 M-I Drilling Fluids UK Limited Porous articles
AU2007304053B2 (en) * 2006-10-02 2012-07-12 M-I Drilling Fluids Uk Limited Method of forming an agent and its use in desulphurisation
US8871675B2 (en) 2006-10-02 2014-10-28 M I Drilling Fluids Uk Ltd. Method of forming an agent and its use in desulphurisation
US9987625B2 (en) 2006-10-02 2018-06-05 M-I Drilling Fluids Uk Limited Desulfurization agent
WO2018156006A1 (en) * 2017-02-22 2018-08-30 Instituto Nacional De Investigación Forestales, Agrícolas Y Pecuarias Low-temperature removal of h2s using large-surface-area nano-ferrites obtained using a modified chemical coprecipitation method

Also Published As

Publication number Publication date
CA2266458A1 (en) 1998-04-30
JP2001502236A (en) 2001-02-20
GB9621906D0 (en) 1996-12-11
EP0946259A1 (en) 1999-10-06
GB2318309B (en) 2001-05-16
GB2318309A (en) 1998-04-22
AU4566497A (en) 1998-05-15
BR9712408A (en) 1999-10-19
GB9721228D0 (en) 1997-12-03

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