Method for preparing alkali metal sulphide

Patent metadata

Field	Value
Publication number	US-9458015-B2
Application number	US-201314439925-A
Country	US
Kind code	B2
Filing date	Nov 13, 2013
Priority date	Nov 15, 2012
Publication date	Oct 4, 2016
Grant date	Oct 4, 2016

Abstract

The present invention concerns a method for preparing an alkali metal sulfide, from at least one oxygenated alkali metal compound comprising at least one step a) involving reacting said oxygenated alkali compound(s) with at least one sulfur compound of formula (I):

in which: R represents a linear or branched alkyl or alkenyl radical, containing 1 to 6 carbon atoms, preferably 1 to 4 carbon atoms; n is equal to 0, 1 or 2; x is equal to 0 or to a whole number having a value of between 1 and 10, preferably x is a whole number equal to 1, 2, 3 or 4; R′ represents a linear or branched alkyl or alkenyl radical, containing 1 to 6 carbon atoms, preferably 1 to 4 carbon atoms or, only if n=x=0, a hydrogen atom; or indeed R and R′ can form, together and with the sulfur atom(s) bearing them, a sulfur heterocycle containing 2 to 12 carbon atoms, preferably 2 to 8 carbon atoms, and optionally one or a plurality of heteroatoms chosen from oxygen, nitrogen and sulfur.

First claim

The invention claimed is:

1. A process for the preparation of an alkali metal sulfide from at least one oxygen-comprising alkali metal compound, comprising at least one stage a) involving reacting said oxygen-comprising alkali metal compound(s) with at least one sulfur-comprising compound of formula (I):

in which:
R represents a linear or branched alkyl or linear or branched alkenyl radical comprising from 1 to 6 carbon atoms, limits included;
n is equal to 0, 1 or 2;
x is equal to 0 or to an integer taking the values from 1 to 10, limits included;
R′ represents a linear or branched alkyl or linear or branched alkenyl radical comprising from 1 to 6 carbon atoms, limits included, or, only if n=x=0, a hydrogen atom;
or else R and R′ can together form, and with the sulfur atom(s) which carry(ies) them, a sulfur-comprising heterocycle comprising from 2 to 12 carbon atoms, limits included, and optionally, in addition to the sulfur atom(s) indicated in the formula (I), one or more heteroatoms chosen from oxygen, nitrogen and sulfur.

2. The process as claimed in claim 1 , wherein said oxygen-comprising alkali metal compound is selected from the group consisting of the oxides, hydroxides, hydrogencarbonates, carbonates, sulfates, sulfites, nitrates, nitrites and carboxylates of said alkali metal and also the mixtures of two or more of them, in all proportions.

3. The process as claimed in claim 1 , wherein the alkali metal is selected from the group consisting of lithium, sodium, potassium, rubidium, cesium and their mixtures.

4. The process as claimed in claim 1 , wherein said sulfur-comprising compound of formula (I) is such that n=0.

5. The process as claimed in claim 1 , wherein said sulfur-comprising compound of formula (I) is such that x=1, 2 or 3 or is a mixture of sulfur-comprising compounds with, on average, x between 2 and 10 (limits included).

6. The process as claimed in claim 1 , wherein the sulfur-comprising compound is selected from the group consisting of dimethyl trisulfide, diethyl trisulfide, dimethyl tetrasulfide, diethyl tetrasulfide, dimethyl disulfide, diethyl disulfide, di(n-propyl) disulfide, diisopropyl disulfide and their mixtures, preferably dimethyl disulfide, diethyl trisulfide and dimethyl tetrasulfide, and their mixtures.

7. The process as claimed in claim 1 , wherein stage a) is carried out at a temperature of between 150° C. and 1500° C.

8. The process as claimed in claim 1 , wherein stage a) is carried out in the presence of at least one catalyst selected from the group consisting of cobalt oxides, nickel oxides, molybdenum oxides and their mixtures, which are or are not supported, at a temperature of between 150 and 400° C.

9. The process as claimed in claim 1 , wherein stage a) is carried out in the absence of catalyst at a temperature of between 300 and 600° C.

10. The process as claimed in claim 1 , wherein lithium sulfide (Li 2 S) is prepared from dimethyl disulfide (DMDS) and lithium hydroxide or lithium carbonate or lithium oxide.

11. The process as claimed in claim 1 , wherein the alkali metal sulfide has formula M 2 S, where M represents an alkali metal selected from the group consisting of lithium, potassium, sodium, rubidium and cesium.

12. The process as claimed in claim 1 , wherein the compound of formula (I) is dimethyl disulfide and the alkali metal sulfide is lithium sulfide.

13. The process as claimed in claim 1 , wherein the sulfur-comprising compound(s) and oxygen-comprising alkali metal compounds are present in amounts to provide a sulfur/alkali metal molar ratio of between 0.5 and 10.

14. The process as claimed in claim 1 , wherein stage a) is carried out at a temperature of between 300° C. and 800° C.

15. The process as claimed in claim 1 , wherein stage a) is carried out at a temperature of between 300° C. and 600° C.

16. The process as claimed in claim 1 , wherein x is an integer equal to 1, 2, 3 or 4.

17. The process as claimed in claim 1 , wherein R represents a linear or branched alkyl or linear or branched alkenyl radical comprising from 1 to 4 carbon atoms, limits included.

18. The process as claimed in claim 1 , wherein R′ represents a linear or branched alkyl or linear or branched alkenyl radical comprising from 1 to 4 carbon atoms, limits included, or, only if n=x=0, a hydrogen atom.

19. The process as claimed in claim 1 , wherein stage a) is carried out in the presence of at least one of hydrogen or water.

20. The process as claimed in claim 1 , wherein stage a) is carried out in the presence of sulfur.

Assignees

• Arkema France

Inventors

• Schmitt Paul Guillaume
• Fremy Georges

Classifications

• C01B17/22 Primary

  Alkali metal sulfides or polysulfides · CPC title