Patent EP0055487A1 successfully refreshed from Google Patents.
EP0055487A1
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Preparation of rhodium complex compounds
Assignee: Union Carbide Corp
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Filing: 1981-12-29
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Granted: —
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Expires: 2001-12-29
Abstract
Abstract Process for preparing halocarbonylbis(triorganophosphorus) rhodium compounds and hydridocarbonyltris(triorganophosphorus) rhodium compounds.
Inventors
- 👤 Ernst Billig
- 👤 David Robert Bryant
- 👤 Jackie Dean Jamerson
Bibliographic Details
Application Number
—
Jurisdiction
EP
Data Source
google_patents
Last Synchronized
2026-11-08 21:11
CPC Classifications
C; C07; C07F; C07F15/00; B; B01; B01J; B01J31/00; B01J31/16; B01J31/24; B01J31/2404; B01J31/20; B01J31/40; B01J31/4015; B01J31/4023; B01J31/4038; B01J31/4046; B01J31/4053; C07F15/0006; C07F15/0073; C07F15/008; B01J2231/00; B01J2231/30; B01J2231/32; B01J2231/321; B01J2531/00; B01J2531/80; B01J2531/82; B01J2531/822; Y; Y02; Y02P; Y02P20/00; Y02P20/50; Y02P20/584
Claims Analysis
Total Claims: 15
Claim 1
Independent Claim
201 words
An organic one-phase process for preparing a halocarbonylbis(triorganophosphorus) rhodium compound which comprises reacting, at a temperature from about 20°C. to about 200°C., an essentially non-aqueous, homogeneous organic reaction solution consisting essentially of (a) a rhodium complex concentrate, (b) a halide ion source, (c) carbon monoxide gas or a carbon monoxide source and (d) free triorganophosphorus ligand, for at least a sufficient period of time to form said halo- carbonylbis(triorganophosphorus) rhodium compound; said rhodium complex concentrate consisting essentially of from about 0.1 to about 30 percent by weight of a spent hydroformylation reaction medium and having been produced by concentrating a spent hydroformylation reaction medium that contains a partially deactivated soluble rhodium complex hydroformylation catalyst, aldehyde products, higher boiling aldehyde condensation by-products, and free triorganophosphorus ligand, so as to remove from said medium, while retaining a major amount of the rhodium values of said catalyst present in said medium, at least essentially all of said aldehyde products, at least 50 percent by weight of said higher boiling aldehyde condensation by-products that have a boiling point below that of said free triorganophosphorus ligand present in said medium and at least 50 percent by weight of said free triorganophosphorus ligand present in said medium.
Claim 2
Dependent Claim
201 words
An organic one-phase process for preparing a halocarbonylbis(triorganophosphorus) rhodium compound which comprises reacting, at a temperature from about 20°C. to about 200°C., an essentially non-aqueous, homogeneous organic reaction solution consisting essentially of (a) a rhodium complex concentrate, (b) a halide ion source, (c) carbon monoxide gas or a carbon monoxide source and (d) free triorganophosphorus ligand, for at least a sufficient period of time to form said halo- carbonylbis(triorganophosphorus) rhodium compound; said rhodium complex concentrate consisting essentially of from about 0.1 to about 30 percent by weight of a spent hydroformylation reaction medium and having been produced by concentrating a spent hydroformylation reaction medium that contains a partially deactivated soluble rhodium complex hydroformylation catalyst, aldehyde products, higher boiling aldehyde condensation by-products, and free triorganophosphorus ligand, so as to remove from said medium, while retaining a major amount of the rhodium values of said catalyst present in said medium, at least essentially all of said aldehyde products, at least 50 percent by weight of said higher boiling aldehyde condensation by-products that have a boiling point below that of said free triorganophosphorus ligand present in said medium and at least 50 percent by weight of said free triorganophosphorus ligand present in said medium.
Claim 3
Dependent Claim
29 words
A process as defined in claim 1, wherein the rhodium complex concentrate consists essentially of from about 1 to 10 percent by weight of said spent hydroformylation reaction medium.
Claim 4
Dependent Claim
36 words
A process as defined in claim 2, wherein said concentrate has been oxygenated, the oxidative treatment being at least sufficient to convert any remaining free triorganophosphorus ligand present in the concentrate to its corresponding triorganophosphorus oxide.
Claim 5
Dependent Claim
21 words
A process as defined in claim 3, wherein the oxidative treatment is conducted at a-temperature of about 90 to about 175°C.
Claim 6
Dependent Claim
13 words
A process as defined in claim 4, wherein the oxidative agent is air.
Claim 7
Dependent Claim
19 words
A process as defined in claim 4, wherein said halide ion source is a hydrohalic acid preferably hydrochloric acid.
Claim 8
Dependent Claim
13 words
A process as defined in claim 4, wherein carbon monoxide gas is employed.
Claim 9
Dependent Claim
14 words
A process as defined in claim 4, wherein a carbon monoxide source is employed.
Claim 10
Dependent Claim
30 words
A process as defined in claim 8, wherein the carbon monoxide source is an amide,preferably N,N-dimethylformamide and wherein the reaction temperature ranges from about 130 °C. to about 190 °C.
Claim 11
Dependent Claim
14 words
A process as defined in claim 4, wherein said free triorganophosphorus ligand is triphenylphosphine.
Claim 12
Dependent Claim
62 words
A process as defined in claim 4 and 5, wherein a suspension of precipitated chlorocarbonylbis(triorganophosphine) rhodium is prepared by refluxing the essentially non-aqueous, homogeneous reaction solution, at a temperature of from about 130°C. to about l90°C., consisting essentially of (a) said oxygenated rhodium complex concentrate, (b) hydrochloric acid, (c) N,N-dimethylformamide and (d) free triphenylphosphine ligand and isolated and recovered from said suspension.
Claim 13
Dependent Claim
84 words
A process for preparing a hydridocarbonyl- tris(triorganophosphorus) rhodium compound which comprises reacting, at a temperature of from about 20°C. to about 100°C., the halocarbonylbis(triorganophosphorus) rhodium compound, preferably chlorocarbonylbis(triphenylphosphine) rhodium compound produced as defined in claim 11 produced as defined in claim 1 to 11 without isolating said halocarbonylbis(triorganophosphorus) rhodium compound from its product mixture, with a metal hydride preferably a borohydride reducing agent and free triorganophosphorus ligand, preferably triphenylphosphine for at least a sufficient period of time to form said hydridocarbonyl- tris(triorganophosphorus) rhodium compound.
Claim 14
Dependent Claim
27 words
A process as defined in claim 12, wherein the reduction process is conducted in the presence of an aliphatic alcohol containing from 2 to 5 carbon atoms.
Claim 15
Dependent Claim
38 words
A process as defined in claim 13, wherein the oxidant employed in oxygenating the rhodium complex concentrate is air, wherein the aliphatic alcohol is ethanol or isopropanol and wherein a solvent solution of said sodium borohydride is employed.
References Cited (Backward Citations)
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