Reactor and process for preparing hydrogen sulphide

Patent metadata

Field	Value
Publication number	US-9630843-B2
Application number	US-201314410378-A
Country	US
Kind code	B2
Filing date	May 31, 2013
Priority date	Jun 22, 2012
Publication date	Apr 25, 2017
Grant date	Apr 25, 2017

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 for continuous preparation of hydrogen sulphide by exothermic reaction of sulphur and hydrogen to form a final product gas mixture P final comprising hydrogen sulphide and sulphur at elevated temperature and elevated pressure relative to standard conditions, said reactor, comprising:
a lower reactor region including a sulphur melt, and
a gas collecting region configured for accommodating a product gas mixture P final at elevated temperature and elevated pressure relative to standard conditions,
wherein the reactor comprises at least two non-pressure-bearing first caverns and a supply device providing a controlled supply of pressurized gaseous hydrogen to the lower reactor region per first caverns, the caverns being configured for at least temporary accommodation of a product gas mixture P 1 which forms in exothermic reaction and comprises hydrogen sulphide, sulphur and hydrogen, and
the reactor additionally comprises a non-pressure-bearing second cavern which is arranged above the first cavern and is configured for at least temporary accommodation of the product gas mixture P 1 formed in the first cavern and for formation of further hydrogen sulphide by exothermic reaction of sulphur and hydrogen to form a product gas mixture P 2 .

2. The reactor according to claim 1 , wherein at least one of the second caverns comprises at least one supply device suitable for controlled supply of pressurized gaseous hydrogen.

3. The reactor according to claim 1 , wherein the reactor additionally comprises a non-pressure-bearing third cavern, and optionally further, correspondingly suitable caverns arranged above the second cavern.

4. The reactor according to claim 3 , wherein at least one of the pressure-bearing third or further suitable caverns has a greater volume than each of the first caverns, and/or in that at least one of the pressure-bearing third or further suitable caverns has lower heat removal for construction reasons than each of the first caverns.

5. The reactor according to claim 1 , wherein the reactor additionally comprises a non-pressure-bearing installed device configured for continuous transfer of the total amount of product gas mixture P u formed in the lower reactor region to the gas collecting region and, in the case that a catalyst is present in the installed device, the device is configured for reaction of sulphur and hydrogen still present in the product gas mixture P u to hydrogen sulphide.

6. The reactor according to claim 5 , wherein one, more than one or all of the installed devices for transfer of the product gas mixture Pu from the lower reactor region to the gas collecting region are arranged in terms of construction such that, after sufficient filling of the lower reactor region with a sulphur melt, they are in thermal contact with the sulphur melt such that, when the installed device contains a catalyst, the catalyst is cooled by transfer of heat to the sulphur melt.

7. The reactor according to claim 1 , wherein the reactor comprises an inner wall which, in the course of operation of the reactor with involvement of the space between outer reactor wall and the inner wall, obtains continuous circulation of the sulphur melt according to the airlift pump principle.

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

9. A process for preparing hydrogen sulphide by exothermic reaction of sulphur with hydrogen at elevated temperature and elevated pressure relative to standard conditions to form a product gas mixture P final comprising hydrogen sulphide and sulphur, the process comprising:
supplying pressurized hydrogen into a sulphur melt located in a lower reactor region of a pressurized reactor, the hydrogen supplied being accommodated at least partly, together with sulphur converted from the sulphur melt to the gaseous state, by at least two non-pressure-bearing first caverns, wherein the pressurized gaseous hydrogen is supplied by supply devices per first caverns;
at least temporarily leaving the hydrogen and the sulphur in the first caverns, so as to form, in exothermic reaction, a product gas mixture P 1 comprising hydrogen sulphide, sulphur and hydrogen;
at least temporarily leaving the product gas mixture P 1 formed in the first caverns in a second cavern, so as to react the 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 and
collecting the product gas mixture P final in a gas collecting region.

10. The process according to claim 9 , wherein at least a portion of the hydrogen supplied into the sulphur melt is accommodated directly by the second cavern.

11. The process according to claim 9 , wherein the product gas mixture is accommodated and left at least temporarily in a third or higher cavern, so as to react the sulphur and hydrogen present in the product gas mixture P 2 with formation of further hydrogen sulphide.

12. The process according to claim 9 , wherein the total amount of the product gas mixture P u formed in the lower reactor region is continuously transferred to the gas collecting region by a non-pressure-bearing installed device, wherein by use of a catalyst in the installed device the sulphur and hydrogen present in the product gas mixture P u are reacted with formation of further hydrogen sulphide.

13. The process according to claim 12 , 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.

14. The process according to claim 12 , wherein the proportion of hydrogen sulphide in the product gas mixture P u prior to introduction into the installed device containing the catalyst is at least 60% of the gas volume.

15. The process according to claim 9 , further comprising condensing and recycling directly into the reaction, sulphur present in the product gas mixture P final .

16. The process according to claim 9 , wherein the preparation of hydrogen sulphide is performed at a pressure of 5 to 15 bar.

17. The process according to claim 9 , wherein the temperature of the sulphur melt is 400 to 450° C.

18. The process according to claim 9 , wherein the sulphur melt is circulated continuously according to the airlift pump principle.

19. The process according to claim 9 , wherein the hydrogen sulphide has a sulphane content not exceeding 600 ppm.

Assignees

• Evonik Degussa Gmbh

Inventors

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

Classifications

• B01J19/006

  Baffles · CPC title

• B01J19/24

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

• 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

• B01J4/002

  Nozzle-type elements (nozzle-type reactors B01J19/26) · CPC title