WO2004022482A2 - Procede de purificatin d'un gaz de synthese a base de sulfure dhydrogene - Google Patents
Procede de purificatin d'un gaz de synthese a base de sulfure dhydrogene Download PDFInfo
- Publication number
- WO2004022482A2 WO2004022482A2 PCT/FR2003/002638 FR0302638W WO2004022482A2 WO 2004022482 A2 WO2004022482 A2 WO 2004022482A2 FR 0302638 W FR0302638 W FR 0302638W WO 2004022482 A2 WO2004022482 A2 WO 2004022482A2
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- sulfur
- filter
- activated carbon
- gas
- hydrogen
- Prior art date
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/16—Hydrogen sulfides
- C01B17/168—Purification
Definitions
- the present invention relates to the industrial production of hydrogen sulfide.
- This industrial production generally consists in reacting hydrogen gas with sulfur in the liquid state at a temperature of about 400 to 450 ° C in a reactor surmounted by a sulfur reflux column. The gas leaving the column head is then cooled in one or more condensers where sulfur is recovered by solidification.
- the gas at 30 ° C. at the outlet of the condenser may still contain impurities leading, without the implementation of a post-reaction, to the deposition in the rest of installation of at least 100 mg of sulfur per kilogram of H 2 S produced.
- This deposit corresponds to a pseudo-saturated vapor pressure at least 10 times higher than the saturated vapor pressure of pure sulfur at this same temperature of 30 ° C.
- the object of the present invention is to find another technical solution, simple to implement, to avoid clogging of the pipes.
- This object is achieved by a process for the purification of a synthesis gas containing mainly hydrogen sulfide H 2 S and obtained by the reaction of hydrogen and liquid sulfur in an industrial apparatus, characterized in that the this gas is passed through a filter containing a solid chosen from porous grains of activated carbon, alumina, silica.
- the purified gas leaving the filter has, under these conditions, a reduced or even non-existent ability to deposit solid sulfur in said apparatus.
- porous grains lies in the fact that they are saturated with sulfur and / or sulfur compounds inside their pores, thus avoiding the clogging by sulfur of the empty spaces between the grains.
- the porous grains are activated carbon.
- such a carbon is capable of retaining by adsorption in its pores up to
- the used coal containing sulfur products can be completely incinerated and thus be transformed into CO 2 , SO 2 and H 2 O.
- the filter also contains a material which adsorb water selectively with respect to hydrogen sulphide, in particular a molecular sieve of type 3 A. This material, by drying the hydrogen sulphide then makes it possible to avoid corrosion problems in the rest of the installation.
- the operational temperature of the porous solid is from 0 to 200 ° C, preferably 0 ° to 100 ° C.
- the pressure inside the filter ranges from 1 to 100 bar absolute and preferably from 1 to 10 bar absolute.
- the contact time of the synthesis gas with the porous solid ranges from 0.1 second (s) to 5 minutes, preferably from ls to 30s.
- the linear speed of the synthesis gas in the filter ranges from 0.01 m / s to 2 m / s, preferably from 0.02 m / s to 0.1 m / s.
- the filter containing the activated carbon is subjected to a gas stream, either of synthesis, or having a purity by weight of 99.7% in H 2 S, for a determined period.
- the filter is then isolated from the gas stream, then with the usual precautions, purged with nitrogen at a temperature ranging from 20 to 100 ° C., to remove the H 2 S. Despite this purging, there may be subsequent releases of sulfur compounds.
- the sample is subjected to total combustion in the presence of oxygen; the sulfur compounds are transformed into SO 2 , then into H 2 SO by oxidation with hydrogen peroxide and finally dosed by coulometry according to E. Debal and R. Levy, Bull. Soc. Chim. Fr N ° 68 (1), pp. 426-434, 1967.
- This gas is passed through a cylindrical filter of revolution with an internal diameter of 23 cm and an internal length of 50 cm.
- This filter is filled with 8 kg of activated carbon ACTICARBONE ® AC 35 from the French company CECA.
- This activated carbon is in the form of small cylinders 4 mm in diameter. Its BET specific surface is at least 1000 m 2 / g.
- the filter After 8 h of filtration, the filter is isolated and subjected to the procedure described above to analyze the gradient of its sulfur content.
- the coal samples are taken from the different layers of the bed, spaced 10 cm apart depending on the length of the filter. The results are presented in the following table.
- Example 1 is repeated identically with new activated carbon but tripling the duration of : filtration. (24 h). The / results appear in the following table II: * . . .. x L - '
- Example 1 The conditions of Example 1 are identical except the filtration time which is 56 h. The results are shown in Table III below:
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Separation Of Gases By Adsorption (AREA)
- Treating Waste Gases (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
- Biological Treatment Of Waste Water (AREA)
- Catalysts (AREA)
Abstract
Description
Claims
Priority Applications (5)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE60303453T DE60303453T2 (de) | 2002-09-06 | 2003-09-03 | Reinigung von H2S durch poröse Medien |
CA2499916A CA2499916C (fr) | 2002-09-06 | 2003-09-03 | Purification du h2s par supports poreux |
SI200330240T SI1542924T1 (sl) | 2002-09-06 | 2003-09-03 | Postopek za ciscenje sinteznega plina na osnovi vodikovega sulfida |
AU2003278253A AU2003278253A1 (en) | 2002-09-06 | 2003-09-03 | Method for purifying hydrogen sulphide on porous supports |
EP03769563A EP1542924B1 (fr) | 2002-09-06 | 2003-09-03 | Procede de purificatin d un gaz de synthese a base de sulfur e dhydrogene |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR0211156A FR2844208B1 (fr) | 2002-09-06 | 2002-09-06 | Purification du h2s par supports poreux |
FR02/11156 | 2002-09-06 |
Publications (2)
Publication Number | Publication Date |
---|---|
WO2004022482A2 true WO2004022482A2 (fr) | 2004-03-18 |
WO2004022482A3 WO2004022482A3 (fr) | 2004-06-10 |
Family
ID=31725950
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/FR2003/002638 WO2004022482A2 (fr) | 2002-09-06 | 2003-09-03 | Procede de purificatin d'un gaz de synthese a base de sulfure dhydrogene |
Country Status (11)
Country | Link |
---|---|
EP (1) | EP1542924B1 (fr) |
AT (1) | ATE316940T1 (fr) |
AU (1) | AU2003278253A1 (fr) |
CA (1) | CA2499916C (fr) |
DE (1) | DE60303453T2 (fr) |
DK (1) | DK1542924T3 (fr) |
ES (1) | ES2257696T3 (fr) |
FR (1) | FR2844208B1 (fr) |
PT (1) | PT1542924E (fr) |
RU (1) | RU2294893C2 (fr) |
WO (1) | WO2004022482A2 (fr) |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2008087106A1 (fr) * | 2007-01-16 | 2008-07-24 | Basf Se | Procédé et dispositif de préparation continue d'acide sulfhydrique |
WO2010072756A1 (fr) | 2008-12-23 | 2010-07-01 | Basf Se | Procédé de compression de gaz contenant du sulfure d'hydrogène |
WO2015142980A1 (fr) * | 2014-03-21 | 2015-09-24 | Chevron Phillips Chemical Company Lp | Procédés d'élimination de polysulfanes et de soufre élémentaire à partir de sulfure d'hydrogène |
WO2016001553A1 (fr) | 2014-07-04 | 2016-01-07 | Arkema France | Procédé de préparation de méthylmercaptan |
WO2016001554A1 (fr) | 2014-07-04 | 2016-01-07 | Arkema France | Procédé de préparation de disulfure de diméthyle |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE10245164B4 (de) * | 2002-09-26 | 2014-11-13 | Evonik Degussa Gmbh | Verfahren zur Umwandlung von Polysulfanen |
CA2674554C (fr) | 2007-01-16 | 2016-09-20 | Basf Se | Procede et dispositif de preparation de sulfure d'hydrogene en continu |
CN110124651B (zh) * | 2018-02-09 | 2022-03-04 | 中国石油化工股份有限公司 | 含有碳纳米笼的分解硫化氢的催化剂及其制备方法和应用 |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
BE352419A (fr) * | ||||
US2474066A (en) * | 1946-01-04 | 1949-06-21 | Barium Reduction Corp | Method of making hydrogen sulfide |
US5173285A (en) * | 1988-04-07 | 1992-12-22 | Jgc Corporation | Process for the manufacture of hydrogen sulfide |
-
2002
- 2002-09-06 FR FR0211156A patent/FR2844208B1/fr not_active Expired - Fee Related
-
2003
- 2003-09-03 DE DE60303453T patent/DE60303453T2/de not_active Expired - Lifetime
- 2003-09-03 AU AU2003278253A patent/AU2003278253A1/en not_active Abandoned
- 2003-09-03 CA CA2499916A patent/CA2499916C/fr not_active Expired - Fee Related
- 2003-09-03 PT PT03769563T patent/PT1542924E/pt unknown
- 2003-09-03 AT AT03769563T patent/ATE316940T1/de active
- 2003-09-03 DK DK03769563T patent/DK1542924T3/da active
- 2003-09-03 WO PCT/FR2003/002638 patent/WO2004022482A2/fr not_active Application Discontinuation
- 2003-09-03 ES ES03769563T patent/ES2257696T3/es not_active Expired - Lifetime
- 2003-09-03 RU RU2005109941/15A patent/RU2294893C2/ru not_active IP Right Cessation
- 2003-09-03 EP EP03769563A patent/EP1542924B1/fr not_active Revoked
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
BE352419A (fr) * | ||||
US2474066A (en) * | 1946-01-04 | 1949-06-21 | Barium Reduction Corp | Method of making hydrogen sulfide |
US5173285A (en) * | 1988-04-07 | 1992-12-22 | Jgc Corporation | Process for the manufacture of hydrogen sulfide |
Cited By (13)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US7833509B2 (en) | 2007-01-16 | 2010-11-16 | Basf Se | Method and device for the continuous production of hydrogen sulfide |
WO2008087106A1 (fr) * | 2007-01-16 | 2008-07-24 | Basf Se | Procédé et dispositif de préparation continue d'acide sulfhydrique |
WO2010072756A1 (fr) | 2008-12-23 | 2010-07-01 | Basf Se | Procédé de compression de gaz contenant du sulfure d'hydrogène |
US9067872B2 (en) | 2008-12-23 | 2015-06-30 | Basf Se | Method for compressing gases containing hydrogen sulfide |
US10773958B2 (en) | 2014-03-21 | 2020-09-15 | Chevron Phillips Chemical Company Lp | Processes for removing polysulfanes and elemental sulfur from hydrogen sulfide |
WO2015142980A1 (fr) * | 2014-03-21 | 2015-09-24 | Chevron Phillips Chemical Company Lp | Procédés d'élimination de polysulfanes et de soufre élémentaire à partir de sulfure d'hydrogène |
CN114044495A (zh) * | 2014-03-21 | 2022-02-15 | 切弗朗菲利浦化学公司 | 用于从硫化氢中去除聚硫烷和元素硫的方法 |
CN106163982A (zh) * | 2014-03-21 | 2016-11-23 | 切弗朗菲利浦化学公司 | 用于从硫化氢中去除聚硫烷和元素硫的方法 |
WO2016001554A1 (fr) | 2014-07-04 | 2016-01-07 | Arkema France | Procédé de préparation de disulfure de diméthyle |
US10689334B2 (en) | 2014-07-04 | 2020-06-23 | Arkema France | Method for preparing methyl mercaptan |
US10550077B2 (en) | 2014-07-04 | 2020-02-04 | Arkema France | Method for preparing dimethyl disulphide |
US11104642B2 (en) | 2014-07-04 | 2021-08-31 | Arkema France | Method for preparing methyl mercaptan |
WO2016001553A1 (fr) | 2014-07-04 | 2016-01-07 | Arkema France | Procédé de préparation de méthylmercaptan |
Also Published As
Publication number | Publication date |
---|---|
ATE316940T1 (de) | 2006-02-15 |
FR2844208A1 (fr) | 2004-03-12 |
PT1542924E (pt) | 2006-06-30 |
CA2499916A1 (fr) | 2005-03-22 |
DE60303453T2 (de) | 2006-11-16 |
AU2003278253A1 (en) | 2004-03-29 |
EP1542924A2 (fr) | 2005-06-22 |
WO2004022482A3 (fr) | 2004-06-10 |
RU2005109941A (ru) | 2005-10-27 |
RU2294893C2 (ru) | 2007-03-10 |
ES2257696T3 (es) | 2006-08-01 |
CA2499916C (fr) | 2012-02-28 |
FR2844208B1 (fr) | 2004-10-15 |
DK1542924T3 (da) | 2006-05-29 |
EP1542924B1 (fr) | 2006-02-01 |
DE60303453D1 (de) | 2006-04-13 |
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