Reactor and process for preparing hydrogen sulphide

Patent metadata

Field	Value
Publication number	US-9440208-B2
Application number	US-201314410360-A
Country	US
Kind code	B2
Filing date	May 31, 2013
Priority date	Jun 22, 2012
Publication date	Sep 13, 2016
Grant date	Sep 13, 2016

Abstract

The present invention relates to a reactor and to a process for synthesis of hydrogen sulphide from elemental sulphur and hydrogen at elevated pressure and elevated temperature. The invention further relates to the use of the reactor for preparation of hydrogen sulphide in high yield and with a low H 2 S X content.

First claim

The invention claimed is:

1. A reactor suitable for continuous preparation of hydrogen sulphide by an exothermic reaction of sulphur and hydrogen to form a final product gas mixture P final comprising rising hydrogen sulphide and sulphur at an elevated temperature and an elevated pressure relative to standard conditions, said reactor comprising:
a lower reactor region suitable for accommodating a sulphur melt,
a non-pressure-bearing first cavern and a supply device which is accommodated directly into the first caverns suitable for controlled supply of pressurized gaseous hydrogen to the non-pressure-bearing first cavern, said cavern being suitable for at least temporary accommodation of a product gas mixture P 1 which forms in the exothermic reaction and comprises hydrogen sulphide, sulphur and hydrogen, and
a gas collecting region suitable for accommodating the product gas mixture P final at an elevated temperature and an elevated pressure relative to standard conditions,
wherein an installed non-pressure-bearing device is suitable for continuous transfer of the total amount of a product gas mixture P u formed in the lower reactor region to the gas collecting region, wherein said non-pressure-bearing installed device comprises a heterogeneous catalyst for further conversion of hydrogen and sulphur present in the product gas P u to hydrogen sulphide, wherein the reactor does not contain a frit for the supply of pressurized hydrogen.

2. The reactor according to claim 1 , wherein the reactor comprises at least two non-pressure-bearing first caverns and a supply device suitable for controlled supply of pressurized gaseous hydrogen to the non-pressure-bearing first caverns, said first caverns being suitable for at least temporary accommodation of the product gas mixture P 1 .

3. The reactor according to claim 1 , wherein the reactor further comprises at least one non-pressure bearing second cavern which is arranged above the non-pressure bearing first cavern and is suitable for at least temporary accommodation of the product gas mixture P 1 formed in the non-pressure bearing first cavern and for formation of further hydrogen sulphide by the exothermic reaction of sulphur and hydrogen to form a product gas mixture P 2 .

4. The reactor according to claim 3 , wherein at least one of the non-pressure bearing second caverns comprises a supply device suitable for controlled supply of pressurized gaseous hydrogen.

5. The reactor according to claim 3 , wherein the reactor further comprises a non-pressure-bearing third cavern, and, optionally, correspondingly suitable caverns arranged above the non-pressure bearing second cavern.

6. The reactor according to claim 5 , wherein at least one of the second or higher non-pressure bearing caverns has a greater volume than each of the non-pressure bearing first caverns, and/or wherein at least one of the non-pressure bearing second or third caverns has lower heat removal than each of the non-pressure bearing first caverns.

7. The reactor according to claim 3 , wherein at least one of the installed devices for transfer of the product gas mixture P u from the lower reactor region to the gas collecting region are arranged such that after sufficient filling of the lower reactor region with the sulphur melt the installed device is in thermal contact with the sulphur melt such that the catalyst is cooled by transfer of heat to the sulphur melt.

8. The reactor according to claim 1 , wherein the reactor comprises an inner wall, wherein the reactor has a space between an outer reactor wall and the inner wall that allows continuous circulation of the sulphur melt according to the airlift pump principle.

9. The reactor according to claim 1 , wherein the reactor further comprises:
a reflux condenser suitable for condensation of sulphur present in the product gas mixture P final ,
an input line suitable for transport of the product gas mixture P final from the gas collecting region to the reflux condenser, and
a return line suitable for return of condensed sulphur to the reactor.

10. A process for preparing hydrogen sulphide by an exothermic reaction of sulphur with hydrogen at an elevated temperature and an elevated pressure relative to standard conditions to form a product gas mixture P final comprising hydrogen sulphide and sulphur, said process comprising:
providing a sulphur melt in a lower reactor region of a pressurized reactor,
supplying pressurized hydrogen into the sulphur melt through a supply device which is accommodated directly into the first caverns, the hydrogen supplied being accommodated at least partly, together with sulphur converted from the sulphur melt to the gaseous state, by at least one non-pressure-bearing first cavern,
at least temporarily leaving the hydrogen and the sulphur in the non-pressure-bearing first cavern, so as to form, in the exothermic reaction, a product gas mixture P 1 comprising hydrogen sulphide, sulphur and hydrogen, and
continuously transferring the total amount of the product gas mixture P u formed in the lower reactor region to a gas collecting region by one or more installed non-pressure-bearing devices, wherein in the presence of a catalyst in the installed non-pressure-bearing devices sulphur and hydrogen present in the product gas mixture P u are reacted to form further hydrogen sulphide, wherein the reactor does not contain a frit for the supply of pressurized hydrogen.

11. The process according to claim 10 , wherein the product gas mixture P 1 is accommodated in one or more non-pressure-bearing second caverns and is left at least temporarily therein, so as to react sulphur and hydrogen present in the product gas mixture P 1 with formation of further hydrogen sulphide to give a product gas mixture P 2 .

12. The process according to claim 11 , wherein at least a portion of the hydrogen supplied into the sulphur melt is accommodated directly by one or more non-pressure-bearing second caverns.

13. The process according to claim 11 , wherein the product gas mixture is accommodated and left at least temporarily in one or more non-pressure-bearing third or higher caverns, so as to react sulphur and hydrogen present in the product gas mixture P 2 with formation of further hydrogen sulphide.

14. The process according to claim 10 , wherein the catalyst is cooled by heat transfer of the heat of reaction, released by the reaction of sulphur and hydrogen in the catalyst, to the sulphur melt.

15. The process according to claim 10 , wherein a proportion of hydrogen sulphide in the product gas mixture P u prior to introduction into the one or more installed devices comprising the catalyst is at least 60% of the gas volume.

16. The process according to claim 10 , further comprising condensing the sulphur present in the product gas mixture P final and recycling the condensed sulphur directly into the reactor.

17. The process according to claim 10 , wherein the hydrogen sulphide is prepared at a pressure of 5 to 15 bar.

18. The process according to claim 10 , wherein the sulphur melt has a temperature of 400 to 450° C.

19. The process according to claim 10 , wherein the sulphur melt is circulated continuously according to the airlift pump principle.

20. The reactor according to claim 1 , wherein the hydrogen sulphide produced by the reactor comprises a sulphane content not exceeding 600 ppm.

Assignees

• Finkeldei Caspar-Heinrich
• Cheung Chiu Kee
• Maassen Ralf
• Wenner Stefan
• Koerfer Martin
• Evonik Degussa Gmbh

Inventors

• Finkeldei Caspar-Heinrich
• Cheung Chiu Kee
• Maassen Ralf
• Wenner Stefan
• Koerfer Martin

Classifications

• B01J2219/00166

  controlling the residence time inside the reactor vessel · CPC title

• B01J10/005 Primary

  carried out at high temperatures in the presence of a molten material · CPC title

• C01B17/162 Primary

  from elemental sulfur and hydrogen · CPC title

• B01J2219/00777

  horizontal · CPC title

• B01J19/24

  Stationary reactors without moving elements inside (B01J19/08, B01J19/26 take precedence; with stationary particles B01J8/02) · CPC title