Claims
- 1. A process for the preparation of a hydrocyanation catalyst comprising an aqueous solution of at least one water-soluble phosphine and nickel values, which comprises (a) admixing an aqueous solution of said at least one water-soluble phosphine with a nickel hydroxide, (b) adding hydrogen cyanide or a compound which generates hydrogen cyanide to the mixture thus formed, (c) stirring the resulting mixture until the nickel values have at least partially dissolved, and (d) reducing at least a portion of said nickel values having an oxidation state of greater than zero to the zero oxidation state.
- 2. The process as defined by claim 1, comprising maintaining stirring at a temperature of less than 100° C.
- 3. The process as defined by claim 2, comprising maintaining stirring at a temperature ranging from 20° C. to 80° C.
- 4. The process as defined by claim 1, comprising adding nickel in the zero oxidation state to the mixture of reaction, prior to the reduction stage (d) thereof.
- 5. The process as defined by claim 1, comprising (b) adding hydrogen cyanide in an amount at least equal to the stoichiometric amount for converting nickel hydroxide into nickel cyanide.
- 6. The process as defined by claim 5, comprising (b) adding a 30% to 200% stoichiometric excess of hydrogen cyanide.
- 7. The process as defined by claim 1, the amount of said at least one water-soluble phosphine, expressed as number of moles per 1 mol of nickel, ranging from 0.5 and 2,000.
- 8. The process as defined by claim 7, said amount ranging from 2 to 300.
- 9. The process as defined by claim 1, comprising (d) reducing said nickel values with gaseous hydrogen.
- 10. The process as defined by claim 1, comprising (d) reducing said nickel values electrochemically.
- 11. The process as defined by claim 1, comprising (d) reducing said nickel values with an organic/inorganic reducing agent.
- 12. The process as defined by claim 1, said at least one water-soluble phosphine having the structural formula (I):
- 13. The process as defined by claim 12, said at least one water-soluble phosphine having the structural formula (I) comprising an alkali metal or alkaline earth metal salt, ammonium salt, or quaternary ammonium salt of (3-sulfo-4-methylphenyl)di (4-methylphenyl)phosphine, (3-sulfo-4-methoxyphenyl)di(4-methoxyphenyl)phosphine, (3-sulfo-4-chlorophenyl)di(4-chlorophenyl)phosphine, di(3-sulfophenyl)phenylphosphine, di(4-sulfophenyl)phenylphosphine, di(3-sulfo-4-methylphenyl) (4-methylphenyl)phosphine, di(3-sulfo-4-methoxyphenyl)(4-methoxyphenyl)phosphine, di(3-sulfo-4-chlorophenyl)(4-chlorophenyl)phosphine, tri(3-sulfophenyl)phosphine, tri(4-sulfophenyl)phosphine, tri(3-sulfo-4-methylphenyl)phosphine, tri(3-sulfo-4-methoxyphenyl)phosphine, tri(3-sulfo-4-chlorophenyl)phosphine, (2-sulfo-4-methylphenyl)(3-sulfo-4-methylphenyl)(3,5-disulfo-4-methylphenyl)phosphine or (3-sulfophenyl)(3-sulfo-4-chlorophenyl)(3,5-disulfo-4-chlorophenyl)phosphine.
- 14. The process as defined by claim 1, said at least one water-soluble phosphine having the structural formula (II):
- 15. The process as defined by claim 14, said at least one water-soluble phosphine having the structural formula (II) or (III) comprising tris(hydroxymethyl)phosphine, tris(2-hydroxyethyl)phosphine, tris(3-hydroxypropyl)phosphine, tris(2-carboxymethyl)phosphine, the sodium salt of tris(3-carboxyphenyl)phosphine, tris(3-carboxyethyl)phosphine, tris(4-trimethylammoniophenyl)phosphine iodide, the sodium salt of tris(2-phosphonoethyl)phosphine, bis(2-carboxyethyl)phenylphosphine, the sodium salt of 2,2′-bis[di(sulfophenyl)phosphino]-1, 1′-binaphthyl, the sodium salt of 1,2-bis[di(sulfophenyl) phosphinomethyl]cyclobutane (CBDTS), 1,2-bis(dihydroxymethylphosphino)ethane, 1,3-bis(dihydroxymethylphosphino)propane, or the sodium salt of 2,2′-bis[di(sulfophenyl)phosphinomethyl]-1,1 ′-binaphthyl.
- 16. The hydrocyanation catalyst comprising an aqueous solution of at least one water-soluble phosphine and nickel values, prepared by the process which comprises (a) admixing an aqueous solution of said at least one water-soluble phosphine with a nickel hydroxide, (b) adding hydrogen cyanide or a compound which generates hydrogen cyanide to the mixture thus formed, (c) stirring the resulting mixture until the nickel values have at least partially dissolved, and (d) reducing at least a portion of said nickel values having an oxidation state of greater than zero to the zero oxidation state.
Priority Claims (1)
Number |
Date |
Country |
Kind |
98/16469 |
Dec 1998 |
FR |
|
CROSS-REFERENCE TO COMPANION APPLICATION
[0001] Our copending application Ser. No._______[Attorney Docket No. 022701-933], filed concurrently herewith, assigned to the assignee hereof and also expressly incorporated by reference.
Continuations (1)
|
Number |
Date |
Country |
Parent |
PCT/FR99/03232 |
Dec 1999 |
US |
Child |
09886289 |
Jun 2001 |
US |