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Separation of nickel(0) complexes and phosphorus-containing ligands from nitrile mixtures

A technology of phosphorus ligands and complexes, applied in the purification/separation/stabilization of organic compounds, purification/separation of carboxylic acid nitriles, organic compounds/hydrides/coordination complex catalysts, etc., can solve poor selection Sexuality related, short life of catalyst system, etc.

Inactive Publication Date: 2007-02-14
BASF AG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The problem with this minimal conversion of 3-pentenenitrile is that higher 3-pentenenitrile conversion is associated with poor selectivity of adiponitrile based on 3-pentenenitrile and hydrogen cyanide
Furthermore, the minimum 3-pentenenitrile conversion of 60% results in a shorter lifetime of the catalyst system

Method used

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  • Separation of nickel(0) complexes and phosphorus-containing ligands from nitrile mixtures
  • Separation of nickel(0) complexes and phosphorus-containing ligands from nitrile mixtures
  • Separation of nickel(0) complexes and phosphorus-containing ligands from nitrile mixtures

Examples

Experimental program
Comparison scheme
Effect test

Embodiment I

[0155] In a glass flask, a 5-gram mixture of ADN, 3PN and tricresyl phosphite (TTP) as a ligand was prepared in a protective gas atmosphere (argon) (refer to the attached table for the composition), and then 5 grams of cyclohexane was added . Stir at the indicated temperature to combine the ingredients. After switching off the stirring unit, the phase separation was observed visually during the continuous heating. The system was rated as not separating into separate phases when two separate phases could not be visually discerned after 5 minutes. The results are listed in Table 1.

[0156] ADN

Embodiment II

[0158] The steps are equivalent to those in Example 1, except that the chelating ligand of formula A is used instead of tricresyl phosphite. The results are listed in Table 2.

[0159] Formula A:

[0160]

[0161] ADN

Embodiment III

[0163] The steps are equivalent to those in Example I, except that the chelating ligand of formula B is used instead of tricresyl phosphite. The results are listed in Table 3.

[0164] ADN

Ligand

Formula B

3PN

phase separation

20°C

phase separation

40℃

phase separation

60℃

20％

10％

70％

no

no

no

30％

10％

60％

yes

yes

no

30％

20％

50％

yes

yes

no

60％

20％

20％

yes

yes

yes

[0165] Formula B:

[0166]

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PUM

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Abstract

The invention relates to a method for the extractive separation of nickel(0) complexes and phosphorus-containing ligands and / or free phosphorus-containin g ligands from a reaction discharge of a hydrocyanation of unsaturated mononitries to dinitriles, by means of a hydrocarbon, the hydrocarbon and the reaction discharge being separated into two phases at a temperature T (DEG C). The invention is characterised in that the content of nickel(0) complexes and phosphorus-containing ligands and / or free phosphorus-containing ligands in the reaction discharge of the hydrocyanation is at least y wt%, depending on the temperature T, and a maximum of 60 wt% independently of the temperature T. The numerical value of the minimum content y is indicated by the equation y = 0.5 T + 20, T being a dimensionless numerical value.

Description

technical field [0001] The invention relates to a process for the extraction of nickel(0) complexes with phosphorus ligands and / or free phosphorus ligands from reaction effluents of the hydrocyanation of unsaturated mononitriles to dinitriles by extraction with the aid of hydrocarbons, which The phase separation into two phases with the reaction effluent is carried out at a temperature T in °C, [0002] wherein the content of nickel(0) complexes with phosphorus ligands and / or free phosphorus ligands in the hydrocyanated reaction effluent is at least y% by weight as a function of temperature T, with a maximum value independent of temperature T, is 60% by weight, wherein the numerical value of the minimum content y is expressed by the following formula: [0003] y=0.5·T+20 [0004] And T is used in the formula as a dimensionless value. Background technique [0005] Nickel complexes of phosphorus ligands are suitable catalysts for the hydrocyanation of unsaturated mononitril...

Claims

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Application Information

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IPC IPC(8): C07F9/00B01J31/12C07B43/04C07B63/00C07C253/10C07C253/34C07C255/04
CPCB01J2531/847C07C253/34C07C253/10B01J31/185B01J2231/32
Inventor J·沙伊德尔T·容坎普M·巴尔奇G·哈德莱恩R·巴默H·鲁肯P·德克特P·朴法布W·塞格尔T·埃克特纳
Owner BASF AG
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