Process for separating zero-valent nickel species from divalent nickel species

• US 4,387,056 A
• Filed: 04/16/1981
• Issued: 06/07/1983
• Est. Priority Date: 04/16/1981
• Status: Expired due to Fees

• Current Assignee: E. I. du Pont de Nemours and Company (Corteva, Inc.)
• Original Assignee: E. I. du Pont de Nemours and Company (Corteva, Inc.)
• Inventors: Stowe, Gerald T.
• Primary Examiner(s): SNEED, HELEN
• Application Number:
  US06/254,780
• Time in Patent Office: 782 Days
• Field of Search: 260/439 R, 252/414
• US Class Current: 556/13
• CPC Class Codes: B01J 2231/322 Hydrocyanation
• CPC Class Codes: B01J 2531/847 Nickel
• CPC Class Codes: B01J 31/2404 Cyclic ligands, including e.g. non-condensed polycyclic ligands, the phosphine-P atom being a ring member or a substituent on the ring
• CPC Class Codes: B01J 31/403 containing iron group metals or copper
• CPC Class Codes: B01J 31/4053 with recovery of phosphorous catalyst system constituents
• CPC Class Codes: C07C 253/34 Separation; Purification
• CPC Class Codes: C07C 255/07 Mononitriles
• CPC Class Codes: C07F 15/045 without a metal-carbon linkage
• CPC Class Codes: Y02P 20/584 Recycling of catalysts

Abstract

Separating active nickel hydrocyanation catalyst from deactivated catalyst by contact with selected solvents.

Claims

1. A process for separating zero-valent nickel species from divalent nickel species each in a solution of predominantly an organic phosphorus compound along with minor amounts of mononitriles and less than 10% by weight of dinitriles based upon the weight of said solution which comprises contacting said solution with a solvent selected from the class consisting of hydrocarbons having 5-9 carbon atoms, halohydrocarbons having 1-3 carbon atoms, nitriles having 2-5 carbon atoms and mixtures of the foregoing in an amount sufficient to form a precipitate and a single liquid phase and thereafter separating the precipitate from the liquid.

3. The process of claims 1 or 2 wherein the solvent is selected from the class of aliphatic and cycloaliphatic hydrocarbons having 5-9 carbon atoms and mixtures thereof.

4. The process of claim 1 wherein 0.1-5 parts by weight of solvent are contacted with one part by weight of said solution.

6. The process of claims 4 or 5 wherein the solvent is selected from the class consisting of aliphatic and aromatic hydrocarbons having 5-9 carbon atoms and mixtures thereof.

2. A method for recovery of active catalyst in a process for the production of pentenenitriles wherein a zero-valent nickel complexed with an organic phosphorus compound is used as a catalyst and wherein the reaction products are treated to remove a major portion of the pentenenitriles produced resulting in a liquid composition comprising predominantly zero-valent nickel, divalent nickel species and organic phosphorus compound along with minor amounts of pentenenitriles and dinitriles, the improvement which comprises maintaining the amount of dinitrile in said liquid composition less than about 10% by weight based upon the weight of said composition and contacting said composition with a solvent selected from the class consisting of hydrocarbons having 5-9 carbon atoms, halohydrocarbons having 1-3 carbon atoms, nitriles having 2-5 carbon atoms and mixtures of the foregoing in an amount sufficient to cause at least a portion of the divalent nickel species to precipitate while maintaining a single liquid phase and thereafter separating said solid from said liquid.

5. The process of claim 2 wherein 0.1-5 parts by weight of solvent are contacted with one part by weight of said solution.

7. The process of claim 5 wherein the solvent is cyclohexane.