Production of hydrogen sulphide in a reaction vessel
View Patent ↗The invention relates to a reaction vessel in which hydrogen sulphide is produced from sulphur and hydrogen, wherein the reaction vessel is partially or completely made up of a material which is resistant to the reaction mixture and its compounds and/or elements and which remains resistant even at high temperatures.
1. A method for preparing hydrogen sulphide in a reaction vessel, comprising:
reacting a mixture of sulphur and hydrogen in the reaction vessel to form a reaction mixture,
wherein the reaction vessel and, optionally, connection lines and fittings and measurement and control units consist(s) partly or fully of a material which is resistant towards the reaction mixture and comprises aluminum, and
wherein the reaction mixture consists of sulphur, hydrogen and hydrogen sulfide.
2. The method according to claim 1 , wherein the material has a content of more than 1% by weight of aluminum.
3. The method according to claim 1 , wherein the material has a content of 1 to 10% by weight of aluminum and a content of 0 to 5% by weight of at least one of Cu, Co and Y.
4. The method according to claim 1 , wherein the material contains 0 to 0.3% C, 0 to 2.5% Si, 0 to 2.5% Mn, 0 to 0.1% P, 0 to 0.3% S, 15.0 to 28.0% Cr, 0 to 1.0% Cu, 0 to remainder % Fe, 1.0 to 5.0% Al, 0 to 2.5% Co, 0 to 1.5% Ti, 0 to 0.4% Y and up to 70% Ni (% in % by weight).
5. The method according to claim 1 , wherein the material contains 0.1 to 0.25% C, 0 to 0.5% Si, 0 to 0.5% Mn, 0 to 0.05% P, 0 to 0.02% 5, 19.0 to 27.0% Cr, 0 to 0.2% Cu, 2 remainder % Fe, 1.5 to 4.0% Al, 0 to 0.3% Co, 0.1 to 0.3% Ti, 0.05 to 0.15% Y and 30 to 70% Ni.
6. The method according to claim 1 , wherein the material is coated with an aluminum oxide coating where the material is in contact with the reaction mixture.
7. The method according to claim 6 , wherein the aluminum oxide coating is in the form of a layer having a thickness of 0.05 to 1.0 mm.
8. The method according to claim 6 , wherein the material consists of a DIN No. 1.4571 material and is coated.
9. The method according to claim 1 , wherein an outer zone close to the surface of the material is enriched with aluminum oxide or aluminum in comparison to an inner zone.
10. The method according to claim 9 , wherein the outer zone is enriched by solid-state diffusion at high temperatures.
11. The method according to claim 9 , wherein the thickness of the outer zone enriched with aluminum is 0.05 to 1.0 mm.
12. The method according to claim 9 , wherein the vessel comprises a DIN No. 1.4571 material which is enriched with aluminum at a zone close to the surface.
13. The method according to claim 1 , wherein the material is pretreated by pickling or pre-oxidation.
14. The method for preparing hydrogen sulphide according to claim 1 , wherein the pressure in the reaction vessel during the reacting is >0 to 50 bar.
15. The method according to claim 14 , wherein the pressure in the reactor for the hydrogen sulphide synthesis ranges from less than 9 to 20 bar.
16. The method according to claim 14 , wherein the reacting is effected at a temperature between 300 and 600° C.
17. The method according to claim 14 , wherein the reacting is effected in the presence of a heterogeneous catalyst.
18. The method according to claim 14 , wherein the reacting is effected in the presence of a heterogeneous supported catalyst which comprises one or more of the active elements selected from the group consisting of molybdenum, nickel, tungsten, vanadium, cobalt, sulphur, selenium, phosphorus, arsenic, antimony, bismuth, silicon, aluminium, titanium and zirconium.
19. The method according to claim 14 , wherein the hydrogen sulphide is prepared in two or more reaction vessels connected or joined in series.
20. The method according to claim 1 , wherein the inner surface of the vessel is coated with a layer of aluminum oxide comprising aluminum metal in an amount of 5% by weight or more based on the total weight of the coating.
21. The method according to claim 1 , wherein the reaction vessel is made of a material which comprises 0 to 0.1% C, 0 to 0.5% Si, 0 to 1.0% Mn, 0 to 0.2% P, 0 to 0.15% 5, 0 to 25.5% Cr, 0 to 0.5% Cu, 0 to 18.0% Fe, 1.0 to 1.7% Al, 0 to 1.0% Co, 0 to 0.5% Ti, and 0.05 to 0.12% Y.
22. The method according to claim 1 , wherein the reaction vessel is made of a material comprising 0.15 to 0.25% C, 0 to 0.5% Si, 0 to 0.50% Mn, 0 to 0.02% P, 0 to 0.10% S, 24.0 to 26.0% Cr, 0 to 0.1% Cu, 8.0 to 11.0% Fe, 1.8 to 2.4% Al, 0 to 0.3% Co, 0.1 to 0.2% Ti, 0.05 to 0.12% Y and 41.0 to 66.0% Ni.
23. The method according to claim 1 , wherein the material is coated with a layer having a thickness of at least 100 μm.
24. The method according to claim 1 , wherein the reaction vessel is made of a material comprising 0 to 0.4% Si, 0 to 0.50% Mn, 0 to 0.3% Cr, 0 to 0.1% Cu, 0 to 4% Fe, 96.0 to 97.5% Al, 0 to 0.15% Ti, 0 to 0.2% Gn, 0 to 0.3% Cr, and 2.6 to 3.6% Mg.
25. The method according to claim 1 , comprising:
a first vessel and a second vessel connected in series,
wherein the first vessel contains a reaction mixture consisting of hydrogen, sulphur and hydrogen sulphide, and
wherein the second vessel contains a reaction mixture consisting of hydrogen, sulphur and hydrogen sulphide, wherein the hydrogen sulphide is present in a greater amount relative to the hydrogen and sulphur than the relative amount of hydrogen sulphide present in the reaction mixture of the first vessel.
26. The method according to claim 1 , wherein the reaction vessel is in the form of one or more tubes having an inner diameter of 30-130 mm and a length of from 1,000 to 4,000 mm.
27. A method for preparing hydrogen sulphide in a reaction vessel, comprising:
reacting sulphur and hydrogen in the reaction vessel to form a reaction mixture consisting of hydrogen sulphide, sulphur and hydrogen;
wherein the reaction vessel consists of a material which is resistant towards the reaction mixture and comprises an aluminum-containing material, or the reaction vessel has an inner surface in contact with the reaction mixture wherein the inner surface consists of the aluminum-containing material; and
wherein the aluminum-containing material consists of 0 to 0.3% C, 0 to 2.5% Si, 0 to 2.5% Mn, 0 to 0.1% P, 0 to 0.3% 5, 15.0 to 28.0% Cr, 0 to 1.0% Cu, 0 to remainder % Fe, 1.0 to 5.0% Al, 0 to 2.5% Co, 0 to 1.5% Ti, 0 to 0.4% Y and up to 70% Ni wherein % is % by weight based on the total weight of the aluminum-containing material.