Process for the preparation of a nickel/phosphorous ligand catalyst for olefin hydrocyanation

A cyanation reaction and catalyst technology, which is applied in the field of preparation of hydrocyanation reaction catalysts, can solve the problems of ligand degradation and increase in the amount of by-products formed, etc.

Active Publication Date: 2006-02-15
INVISTA TECHNOLOG IES S A R L
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The application describes that as the temperature increases, the rate of catalyst producti

Method used

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  • Process for the preparation of a nickel/phosphorous ligand catalyst for olefin hydrocyanation
  • Process for the preparation of a nickel/phosphorous ligand catalyst for olefin hydrocyanation
  • Process for the preparation of a nickel/phosphorous ligand catalyst for olefin hydrocyanation

Examples

Experimental program
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Embodiment 1

[0048] Example 1 illustrates the aqueous NiCl 2 Azeotropic drying of , followed by reduction using zero-valent iron, to produce active catalysts. Example 2 illustrates the aqueous NiCl 2 Simultaneous drying and reduction using zero-valent iron to produce active catalysts.

[0049] Example 1

[0050] A 250 mL round bottom flask was fitted with a condenser for liquid removal, ligand addition funnel, stirrer, septum port, thermocouple, pressure sensor, and vacuum throttle to control pressure. An electric heating mantle provides heat to the round bottom flask. All accessories are joined by vacuum-tight ground glass joints. Under nitrogen, 120 ml of fresh 3-pentenenitrile was added to the addition funnel. 1.4 g of 30 wt% NiCl 2 The aqueous solution is filled into a gas-tight syringe with a valve between the needle and the syringe. 120 grams of 3-pentenenitrile plus 16.24 grams of ligands with the above structure IX (wherein R 17 is isopropyl, R 18 is H and R 19 is methyl)...

Embodiment 2

[0053] A 250 mL round bottom flask was fitted with a condenser for liquid removal, a liquid addition funnel, a stirrer, a septum port, a thermocouple, a pressure transducer, and a vacuum throttle to control pressure. An electric heating mantle provides heat to the round bottom flask. All accessories are joined by vacuum-tight ground glass joints. Under nitrogen, 120 ml of fresh 3-pentenenitrile was added to the addition funnel. 1.44 g of 30 wt% NiCl 2 The aqueous solution is filled into a gas-tight syringe with a valve between the needle and the syringe. 120 grams of 3-pentenenitrile plus 16.49 grams of ligands with the above structure IX (wherein R 17 is isopropyl, R 18 is H and R 19 is methyl) plus 6.59 g of iron was added to the round bottom flask. The system was degassed by pumping and purging three times with nitrogen. The flask was heated with stirring. The pressure was adjusted to -0.1 psia (0.7 kPa). Insert the needle on the gas-tight syringe through the septu...

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Abstract

A process for preparing a hydrocyanation catalyst comprising contacting a bidentate phosphorous-containing ligand with nickel chloride in the presence of a nitrile solvent and a reducing metal which is more electropositive than nickel the nickel chloride being introduced as an aqueous solution and the water being removed concurrently with the reduction reaction by azeotropic distillation.

Description

technical field [0001] The present invention relates to a process for the preparation of a hydrocyanation catalyst which is a complex of nickel and a bidentate phosphorus compound. Background technique [0002] It is well known in the prior art that nickel complexes with phosphorus-containing ligands can be used as catalysts in hydrocyanation reactions. Such nickel complexes using monodentate phosphites are known to catalyze the hydrocyanation of butadiene to produce a mixture of pentenenitriles. These catalysts are also used in the subsequent hydrocyanation of pentenenitriles to produce adiponitrile, an important intermediate in the production of nylon. It is also known that bidentate phosphite and phosphinite ligands can be used to form nickel-based catalysts for carrying out such hydrocyanation reactions. [0003] U.S. Patent 3,903,120 discloses a method for the preparation of zero-valent nickel complexes comprising combining elemental nickel with the general formula PZ...

Claims

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Application Information

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IPC IPC(8): B01J37/16B01J31/18B01J31/30C07F15/04C07C253/10B01JB01J31/00C07C253/02C07C255/00
CPCB01J2531/847B01J31/30C07C253/10B01J31/1875B01J31/185B01J37/16B01J2231/32C07C255/09
Inventor S·C·杰克逊R·J·麦金尼
Owner INVISTA TECHNOLOG IES S A R L
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