Method for producing chlorotris(triphenylphosphine) rhodium (i)

• US 20060058543A1
• Filed: 07/08/2003
• Published: 03/16/2006
• Est. Priority Date: 07/08/2003
• Status: Active Grant

• Current Assignee: Heraeus Precious Metals GmbH & Co. KG (Einhorn Verwaltungsgesellschaft mbH)
• Original Assignee: WC Heraeus GmbH (Heraeus Holding GMBH)
• Inventors: Meyer, Horst, Walter, Richard
• Granted Patent: US 7,145,027 B2
• Time in Patent Office: Days
• US Class Current: 556/16
• CPC Class Codes: C07F 15/008 without a metal-carbon linkage

Abstract

A process is described for the manufacture of chlorotris(triphenylphosphine)-rhodium(1) by means of causing a reaction of RhCl₃ solution with triphenylphosphin in mixtures of C2-C5 alcohols with water subsequently cooling down and filtering the crystalline precipitate obtained characterized in that the mixture of the reactants is handled in such a way that B is warmed up to 75° C., and C is maintained at 80 to 110° C. The technique leads to improvements in the yield and quality of the crystals obtained.

Claims

1. Process for the manufacture of chlorotris(triphenylphosphine)-rhodium(I) by means of causing a reaction of RhCl₃ solution with triphenylphosphin, subsequently cooling down and filtering the crystalline precipitate obtained wherein the mixture of the reactants is treated in such a way that

A is heated up to about 30°

C. in an initial stage,

B is heated up from 30 to about 75°

C. in a second stage,

C is maintained at 80 to 110°

C.

5. Process pursuant to claim 1, wherein the stages last:

A, about ½

to 1 h;

B, 1 to 4 h and C, about ½

to 1 h.

2. Process for the manufacture of chlorotris(triphenylphosphine)-rhodium(I) by means of causing a reaction of RhCl₃ solution with triphenylphosphin, subsequently cooling down and filtering the crystalline precipitate obtained a 30 to 40°

C. warm mixture of reactants is treated in such a way that

B is heated up from about 30°

C. to 40°

C. to about 75°

C.,

C is maintained at 80 to 110°

C.

6. Process pursuant to claim 2, wherein the stages last:

A, about ½

to 1 h.

3. Process for the manufacture of chlorotris(triphenylphosphine)-rhodium(I) wherein

a solution of RhCl₃ is manufactured in water or an RhCl₃ solution is prepared from a recycling process,

a solution, if necessary under cooling with a C₂-C₅ alcohol, is combined with alcohol,

triphenylphosphin, if necessary under cooling, is added in excess.

A in an initial stage the suspension obtained is heated up from about 5 to 20 to about 30°

C.,

B further in a second stage heated up from about 30 to about 75°

C.,

C is maintained at 80 to 110°

C.;

the solution obtained is cooled down,

the crystals precipitated out are filtered, washed and subsequently dried.

7. Process pursuant to claim 3, wherein the stages last:

A, about ½

to 1 h.

4. Process for the manufacture of tris(triphenylphosphin)-rhodium(I) chlorotris(triphenylphosphine)-rhodium(I) wherein

a solution RhCl₃ is manufactured in water or an RhCl₃ ion is prepared from a recycling process,

isopropanol is produced under a protective inert gas,

the RhCl₃ solution is added

triphenylphosphin is added in excess as an alcoholic solution or suspension

A the mixture obtained is heated up from about 20 to about 30°

C. in an initial stage,

B further in a second stage is heated up from about 30 to about 75°

C.,

C is boiled under reflux at 80 to 110°

C.

the solution obtained is cooled down,

the crystals precipitated out are filtered, washed with alcohol and/or water and/or petroleum ether and subsequently dried.

8. Process pursuant to claim 4, wherein the stages last:

A, about ½

to 1 h;

B, 1 to 4h and C, about ½

to 1 h.