Reactor and process for preparing hydrogen sulphide

Patent metadata

Field	Value
Publication number	US-9649615-B2
Application number	US-201314408687-A
Country	US
Kind code	B2
Filing date	May 31, 2013
Priority date	Jun 22, 2012
Publication date	May 16, 2017
Grant date	May 16, 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 an elevated temperature and an elevated pressure relative to standard conditions, said reactor comprising:
a lower reactor region including a sulphur melt,
a non-pressure-bearing first cavern and a supply device providing a controlled supply of pressurized gaseous hydrogen per first cavern, said cavern 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,
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 , and
a gas collecting region configured for accommodating the product gas mixture P final at an elevated temperature and an elevated pressure relative to standard conditions,
wherein the second cavern comprises a supply device providing a controlled supply of pressurized gaseous hydrogen.

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

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

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

5. The reactor according to claim 1 , wherein the reactor further 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, wherein a catalyst is present in the installed device, the catalyst being suitable 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 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 in terms of construction 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, when the installed device comprises 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, allows continuous circulation of the sulphur melt according to the airlift pump principle.

8. The reactor according to claim 1 , wherein the reactor further comprises:
a reflux condenser suitable for condensation of the 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 the condensed sulphur to the reactor.

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

10. A process for preparing hydrogen sulphide by 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, 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 and at least one non-pressure-bearing second cavern,
at least temporarily leaving the hydrogen and the sulphur in the first cavern, so as to form, in exothermic reaction, a product gas mixture P 1 comprising hydrogen sulphide, sulphur and hydrogen,
accommodating the product gas mixture P 1 in the second cavern and at least temporarily leaving the product gas mixture P 1 therein, such that the sulphur and hydrogen present in the product gas mixture P 1 is reacted with formation of further hydrogen sulphide to a product gas mixture P 2 ,
supplying pressurized hydrogen into the sulphur melt, wherein the hydrogen is at least partly directly supplied by a supply device to the at least one non-pressure-bearing second cavern, together with sulphur converted to the gaseous state from the sulphur melt, and
collecting the product gas mixture P final in a gas collecting region.

11. The process according to claim 10 , wherein the product gas mixture is accommodated and left at least temporarily in one or more third or higher caverns, 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 10 , 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 one or more non-pressure-bearing installed device(s), wherein in the presence a catalyst in the installed device(s) the sulphur and hydrogen present in the product gas mixture P u are reacted to form 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 one or more installed devices comprising the catalyst is at least 60% of the gas volume.

15. 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.

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

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

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

Assignees

• Evonik Degussa Gmbh

Inventors

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

Classifications

• B01J19/006

  Baffles · CPC title

• B01J2219/00768

  vertical · CPC title

• B01J19/24 Primary

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

• B01J19/2415

  Tubular reactors · CPC title

• B01J2219/24

  Stationary reactors without moving elements inside · CPC title