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Preparation method of 1,3,6-hexanetricarbonitrile

A technology of hexane trinitrile and dinitrile, which is applied in the field of compound preparation, can solve the problems of poor whiteness and low purity, and achieve the effects of high yield, high product purity and easy availability of raw materials

Active Publication Date: 2015-11-11
SHIJIAZHUANG SAN TAI CHEM CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the technical problems that the method for preparing 1,3,6-hexanetrinitrile in the prior art is difficult to industrialize, and the preparation of 1,3,6-hexanetrinitrile has low purity and poor whiteness, it provides a 1 , The preparation method of 3,6-hexanetrinitrile can practice the effects of high yield, easy access to raw materials, simple reaction control and high product purity

Method used

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  • Preparation method of 1,3,6-hexanetricarbonitrile

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Experimental program
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Effect test

Embodiment 1

[0020] The preparation method of 1,3,6-hexane trinitrile includes the following steps:

[0021] A. Preparation of 1,6-Dicyano-2-butene: Using 1,4-dioxane as the reaction solvent, place 1mol1,6-dichloro-2-butene, 0.5gCuCl and 2molNaCN in 1 In ,4-dioxane, the substitution reaction is carried out at 40°C for 2h to obtain 1,6-dianitrile-2-butene;

[0022] B. Preparation of 1,3,6-hexane trinitrile: The 1,6-dianitrile-2-butene prepared in step A was reacted with 90g HCl methanol solution at 40℃ for 4h, and then NaCN was added to it at 40℃. The substitution reaction was carried out at ℃ for 2h to obtain 1,3,6-hexanetrinitrile. The calculated yield was 52.1%. The purity of the tested product was 99.55%, the product color number APHA was 15, and the product moisture was 16PPM.

Embodiment 2

[0024] The preparation method of 1,3,6-hexane trinitrile includes the following steps:

[0025] A. Preparation of 1,6-dicyano-2-butene: using 1,4-dioxane as the reaction solvent, 1mol 1,6-dichloro-2-butene, 0.5gCu 2 O and 2.5mol NaCN were placed in 1,4-dioxane, and the substitution reaction was carried out at 80°C for 5h to obtain 1,6-dianitrile-2-butene;

[0026] B. Preparation of 1,3,6-hexane trinitrile: react the 1,6-dianitrile-2-butene prepared in step A with 90g HCl methanol solution at 50℃ for 5h, and then add NaCN to 80 The substitution reaction was carried out at ℃ for 5 hours to obtain 1,3,6-hexanetrinitrile. The calculated yield was 61.2%. The purity of the tested product was 99.63%, the product color number APHA was 13, and the product moisture was 18PPM.

Embodiment 3

[0028] The preparation method of 1,3,6-hexane trinitrile includes the following steps:

[0029] A. Preparation of 1,6-Dicyano-2-butene: Using 1,4-dioxane as the reaction solvent, place 1mol1,6-dichloro-2-butene, 0.5gCuBr and 2.3molNaCN in In 1,4-dioxane, the substitution reaction was carried out at 101°C for 7 hours to obtain 1,6-dianitrile-2-butene;

[0030] B. Preparation of 1,3,6-hexane trinitrile: The 1,6-dianitrile-2-butene prepared in step A was reacted with 90g HCl methanol solution at 60°C for 6h, and then NaCN was added to it at 101 The substitution reaction was carried out at ℃ for 7 hours to obtain 1,3,6-hexanetrinitrile. The calculated yield was 57.5%. The purity of the tested product was 99.54%, the product color number APHA was 17, and the product moisture was 16PPM.

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Abstract

The invention relates to a preparation method of 1,3,6-hexanetricarbonitrile, which comprises the following steps: A. preparation of 1,3-dicyano-2-butylene; and B. preparation of the 1,3,6-hexanetricarbonitrile. The invention provides a new preparation method of 1,3,6-hexanetricarbonitrile, which is completely different from the traditional technique and solves the safety problem in the 1,3,6-hexanetricarbonitrile preparation process in the presence of sodium. Thus, the technique is safer, and satisfies the demands for large-scale industrial production. Besides, the preparation method has the advantages of high yield, accessible raw materials, simple reaction control, high product purity and the like.

Description

Technical field [0001] The invention belongs to the technical field of compound preparation, and specifically relates to a preparation method of 1,3,6-hexanetrinitrile. Background technique [0002] 1,3,6-Hexanetrinitrile is mainly used as an organic synthesis intermediate, high boiling point solvent, and electrolyte additive. With the development of pure electric vehicles and electric bicycles, the energy density of lithium-ion batteries can no longer meet the demand. The development of high voltage is one of the future research directions. The traditional carbonate electrolyte will decompose above 4,5V voltage. The continuous decomposition of the electrolyte will seriously affect the battery performance. It is imminent to add electrolyte additives to the electrolyte to improve the battery performance. [0003] The Journal of Applied Chemistry of the USSR (Journal of Applied Chemistry of the USSR, 1972, 2683-2684) discloses a method for preparing 1,3,6-hexanetrinitrile from 2-am...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C255/05C07C253/14H01M10/0567
CPCC07C253/14C07C255/05H01M10/0567Y02E60/10B01J23/72B01J27/10C07C253/10C07C253/32C07C255/09
Inventor 刘鹏田丽霞梅银平
Owner SHIJIAZHUANG SAN TAI CHEM CO LTD
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