EP 0000665 A1 19790207 - Rhodium recovery from hydroformylation still heel with triaryl phosphate ligand.
Title (en)
Rhodium recovery from hydroformylation still heel with triaryl phosphate ligand.
Title (de)
Rückgewinnung von Rhodium aus Hydroformylierungs-destillationsrückständen mit einem Triarylphosphit-ligand.
Title (fr)
Récupération du rhodium à partir des résidus de distillation d'hydroformylation avec un ligand triaryle phosphite.
Publication
Application
Priority
US 82004677 A 19770728
Abstract (en)
A process for recovering rhodium present in a still heel from the hydroformylation of an unsaturated hydrocarbon wherein rhodium and a triaryl phosphite ligand were used by a process comprising a) pretreating the still heel with a compatible organic solvent, at least 5 ml of water per 100 g of still heel, oxygen gas or a precursor thereof and sufficient base to produce a pH of 2 to 7 in the reaction mixture after rhodium precipitation; b) heating to a temperature of from 0 DEG to 80 DEG C to oxidize the triaryl phosphite ligand to the corresponding phosphate compound; c) heating the mixture from b) for from about 15 minutes to about 120 minutes at about 115 DEG C to about 175 DEG C to precipitate the rhodium and optionally purifying the rhodium from c) by d) separating the rhodium precipitate; e) washing the rhodium precipitate with a solvent-acid solution at a pH of 3 to 4; f) treating the rhodium precipitate with an alkaline reducing solution to reduce the trivalent rhodium impurity to zero valent rhodium; g) quenching the rhodium with glacial acetic acid; h) separating the rhodium; i) washing the rhodium with an acid solution at a pH of 3 to 4; j) drying the rhodium in an inert atmosphere at from 250 DEG to 400 DEG C; and k) oxidizing the rhodium at a temperature of from 300 DEG to 900 DEG C to convert the rhodium to Rn2O3.
IPC 1-7
IPC 8 full level
B01J 31/40 (2006.01); C01G 55/00 (2006.01); C07C 45/50 (2006.01); C22B 11/00 (2006.01); C22B 3/32 (2006.01); C22B 3/38 (2006.01); C22B 7/00 (2006.01)
CPC (source: EP US)
B01J 31/185 (2013.01 - EP US); B01J 31/20 (2013.01 - EP US); B01J 31/4046 (2013.01 - EP US); C01G 55/001 (2013.01 - EP US); C22B 3/32 (2021.05 - EP US); C22B 3/383 (2021.05 - EP US); C22B 3/3846 (2021.05 - EP US); C22B 11/04 (2013.01 - EP US); B01J 23/464 (2013.01 - EP US); B01J 31/0201 (2013.01 - EP US); B01J 2231/321 (2013.01 - EP US); B01J 2531/822 (2013.01 - EP US); Y02P 10/20 (2015.11 - EP US); Y02P 20/584 (2015.11 - EP US)
Citation (search report)
- [D] US 3998622 A 19761221 - BALMAT JEAN LOUIS
- US 3547964 A 19701215 - OLIVIER KENNETH L
Designated contracting state (EPC)
BE DE FR GB NL
DOCDB simple family (publication)
EP 0000665 A1 19790207; CA 1109274 A 19810922; IT 1097450 B 19850831; IT 7826186 A0 19780727; JP S5426218 A 19790227; US 4135911 A 19790123
DOCDB simple family (application)
EP 78300204 A 19780726; CA 308179 A 19780726; IT 2618678 A 19780727; JP 9167078 A 19780728; US 90520078 A 19780512