Catalyst for the synthesis of alkyl mercaptans and process for producing it
View Patent ↗The present invention relates to a catalyst which comprises a support material and an oxidic composition containing at least one alkali metal and tungsten, a process for producing such catalysts and also a process for preparing alkyl mercaptans by reaction of alkanols with hydrogen sulphide in the presence of such a catalyst.
1. A process for producing a catalyst comprising a support material, wherein the support material has a particle size from 1-25 μm, and an oxidic composition comprising oxygen together with at least one alkali metal and tungsten, wherein the oxidic composition has a formula A x WO y , wherein A is at least one alkali metal, x is from 0.8 to 2 and represents the mole fraction of the alkali metal to tungsten in the composition, and y is from 3.4 to 4 and represents the mole fraction of oxygen in the composition, the process comprising:
1) mixing of the support material with an oxidic tungsten compound and at least one separate alkali metal compound to obtain a catalyst composition; and
2) shaping of the catalyst composition.
2. The process of claim 1 , wherein the oxidic tungsten compound is selected from the group consisting of tungsten trioxide (WO 3 ), tungstic acid (WO 3 .H 2 O), metatungstic acid, paratungstic acid, isopolytungstic acids, heteropolytungstic acids, ammonium salts thereof, hydrates thereof and mixtures thereof, ammonium orthotungstate, ammonium metatungstate and ammonium paratungstate.
3. The process of claim 1 , wherein at least one alkali metal compound is a basic alkali metal compound.
4. The process of claim 1 , wherein the support material is an oxidic inorganic support material.
5. The process of claim 1 , wherein the oxidic tungsten compound and the separate alkali metal compound are added in succession to the support material.
6. The process of claim 1 , wherein at least one organic and/or inorganic binder is added in one or both of 1) and 2).
7. The process of claim 1 , wherein the shaping of the catalyst is carried out by extrusion or pressing.
8. The process of claim 3 , wherein the basic alkali metal compound is selected from the group consisting of a hydroxide of an alkali metal and a carbonate of an alkali metal.
9. The process of claim 4 , wherein the support material is selected from the group consisting of aluminium oxide, silicon dioxide, titanium dioxide, zirconium oxide, and amorphous aluminosilicates and mixtures thereof.
10. The process of claim 5 , wherein the oxidic tungsten compound is added as a solid to the support material or to the mixture of support material and a least one alkali metal compound.
11. The process of claim 7 , further comprising:
(i) drying of the catalyst composition and/or of the shaped catalyst; and
(ii) calcination of the catalyst composition and/or of the shaped catalyst.
12. A catalyst, comprising:
a support material having a particle size from 1-25 μm; and
an oxidic composition comprising oxygen together with at least one alkali metal and tungsten, wherein the oxidic composition has a formula A x WO y , wherein A is at least one alkali metal, x is from 0.8 to 2 and represents the mole fraction of the alkali metal to tungsten in the composition, and y is from 3.4 to 4 and represents the mole fraction of oxygen in the composition.
13. The catalyst of claim 12 , wherein the catalyst is produced by a process comprising:
mixing a solid tungsten compound with the support material.
14. The catalyst of claim 12 , wherein the proportion of the oxidic composition composed of alkali metal and tungsten in the catalyst is greater than 15% by weight, based on the total weight of the catalyst.
15. The catalyst of claim 12 , wherein the support material comprises at least one oxidic inorganic compound.
16. The catalyst of claim 12 , which further comprises at least one organic and/or inorganic binder.
17. The catalyst of claim 12 , wherein a standard deviation, stadev, of the normalized tungsten concentration, c norm (W), over the cross section of the catalyst is less than 20, determined by quantitative EDX analysis in accordance with ISO 22309 (2006) in square measurement spots, which have a side length of 100 μm in each case and whose midpoints lie on a straight line and are in each case 100 μm from the midpoint of the adjoining square, with the first and last midpoint of a square being in each case 100 μm from the edge of the catalyst cross section.
18. A catalyst comprising, based on a total weight of the catalyst:
from 25% to 50% by weight of a support material having a particle size from 1-25 μm; and
greater than 40% by weight of an oxidic composition comprising oxygen together with at least one alkali metal and tungsten.