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Method for preparing adiponitrile

A technology of adiponitrile and pentenenitrile, which is applied in the field of preparation of adiponitrile, can solve problems that need to be improved, and achieve the effects of low cost, high purity, and simple and easy-to-operate process

Active Publication Date: 2014-03-26
ANHUI ANQING SHUGUANG CHEM GRP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Yet the method for preparing adiponitrile at present stage still needs to be improved

Method used

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  • Method for preparing adiponitrile
  • Method for preparing adiponitrile
  • Method for preparing adiponitrile

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] a) Hydrocyanide I: A complex composed of monodentate phosphine (tri-m-cresyl phosphite) and bidentate phosphine (compound represented by formula I) and zero-valent nickel (in monodentate phosphine and bidentate phosphine with zero In the complex composed of valent nickel, the molar ratio of monodentate phosphine: bidentate phosphine: zero-valent nickel is 6:2:1), and the molar ratio of HCN (hydrogen cyanide) and BD (butadiene) is 6:115. : 165 was put into the tank reactor, the controlled reaction temperature was 100° C., the pressure was 1.0 MPa, and the reaction residence time was 4 hours, so as to obtain the mixture 1 containing 3-pentenenitrile.

[0055]

[0056] b) Separation I: The resulting mixture 1 is introduced into separation I (rectification column). The rectification tower adopts a rectification tower with 50 trays, wherein the top pressure of the rectification tower is 0.05 MPa, the bottom pressure is 0.06 MPa, the temperature at the top is 40 degrees Ce...

Embodiment 2

[0062]a) Hydrocyanide I: A complex composed of monodentate phosphine (tri-o-cresyl phosphite) and bidentate phosphine (compound shown in formula II) and zero-valent nickel (in monodentate phosphine and bidentate phosphine with zero In the complex composed of valent nickel, the molar ratio of monodentate phosphine: bidentate phosphine: zero-valent nickel is 5:5:1), HCN and BD are put into the tank reactor with a molar ratio of 6:115:165, and the control The reaction temperature was 70° C., the pressure was 1.8 MPa, and the reaction residence time was 4 hours, in order to obtain a mixture 1 containing 3-pentenenitrile.

[0063]

[0064] b) Separate I:

[0065] Same as Example 1.

[0066] c) Hydrocyanation II: The above heavy component mixture 2 is introduced into the tank reactor of hydrocyanation II to carry out further 3-pentenenitrile hydrocyanation reaction.

[0067] Then, in the tank reactor, the co-catalyst triphenylboron is added according to the molar ratio of co-ca...

Embodiment 3

[0072] a) Hydrocyanide I: A complex composed of monodentate phosphine (tri-p-cresyl phosphite) and bidentate phosphine (compound represented by formula III) and zero-valent nickel (in monodentate phosphine and bidentate phosphine with zero In the complex composed of valent nickel, the molar ratio of monodentate phosphine: bidentate phosphine: zero-valent nickel is 7:2:1), HCN and BD are put into the tank reactor with a molar ratio of 6:115:165, and the control The reaction temperature was 90° C., the pressure was 1.8 MPa, and the reaction residence time was 4 hours, in order to obtain a mixture 1 containing 3-pentenenitrile.

[0073]

[0074] b) Separate I:

[0075] Same as Example 1.

[0076] c) Hydrocyanation II: The above heavy component mixture 2 is introduced into the tank reactor of hydrocyanation II to carry out further 3-pentenenitrile hydrocyanation reaction.

[0077] Then, into the tank reactor, the cocatalyst ZnCl 2 According to the molar ratio of hydrocyanic ...

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Abstract

The invention discloses a method for preparing adiponitrile. The method comprises the following steps: performing a first hydrocyanation reaction on butadiene and first hydrocyanic acid under the action of a catalyst to obtain a first mixture; performing primary separation on each component in the first mixture to obtain a second mixture, residual butadiene and residual first hydrocyanic acid respectively; adding a co-catalyst into the second mixture, and introducing second hydrocyanic acid to obtain a third mixture containing the adiponitrile; performing secondary separation on the third mixture to obtain the adiponitrile, residual 3-pentenenitrile, residual second hydrocyanic acid, the reacted catalyst and the reacted co-catalyst, wherein the catalyst is a coordination compound consisting of a monodentate phosphine ligand, a bidentate phosphine ligand and zerovalent nickel, and the co-catalyst is Lewis acid. The method for preparing the adiponitrile has the advantages of small quantity of side products, no need of performing a 2M3BN isomerization reaction, simple process, low cost, high yield, good product quality, economical efficiency and environmental friendliness.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a preparation method of adiponitrile. Background technique [0002] The process of producing adiponitrile by hydrocyanation of butadiene was successfully developed by DuPont Company of the United States in the 1970s and applied to industrial production. At present, monodentate phosphine-zero-valent nickel complexes are mainly used as catalysts in the hydrocyanation of butadiene to produce adiponitrile, which mainly includes the following three reaction steps (Ma Yuan, Yu Baowei, Zhang Haiyan, comparison of adiponitrile production process , Henan Chemical Industry, Vol. 24 (8), 2007, 4-6, which is hereby incorporated by reference in its entirety): [0003] [0004] First, the hydrocyanation reaction of butadiene (BD) and hydrocyanic acid (HCN) under the catalysis of monodentate phosphine-zero-valent nickel complex produces linear product 3-pentenenitrile (3PN) and branched-cha...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/10C07C255/04
Inventor 韩明汉余永发朱润雨陈长斌刘昆陈韬王军吴琨余升琴
Owner ANHUI ANQING SHUGUANG CHEM GRP
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