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The preparation method of 1,3,6-hexanetrinitrile

A technology of hexanetrinitrile and hexene, 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 simple reaction control

Active Publication Date: 2017-08-29
SHIJIAZHUANG SAN TAI CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • The preparation method of 1,3,6-hexanetrinitrile

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Effect test

Embodiment 1

[0020] The preparation method of 1,3,6-hexanetrinitrile comprises the following steps:

[0021] A. Preparation of 1,6-dicyano-2-hexene: With 1,4-dioxane as the reaction solvent, 1mol 1,6-dichloro-2-hexene, 0.5g CuCl and 2mol NaCN Place in 1,4-dioxane, and carry out substitution reaction at 40°C for 2 hours to obtain 1,6-dicyano-2-hexene;

[0022] B. Preparation of 1,3,6-hexanetrinitrile: react the 1,6-dicyano-2-hexene prepared in step A with 90g HCl methanol solution at 40°C for 4h, then add NaCN to it at 40°C The substitution reaction was carried out at °C for 2 hours to obtain 1,3,6-hexanetrinitrile with a calculated yield of 52.1%. The purity of the product was 99.55%, the product color number APHA was 15, and the product moisture content was 16PPM.

Embodiment 2

[0024] The preparation method of 1,3,6-hexanetrinitrile comprises the following steps:

[0025] Preparation of A, 1,6-dicyano-2-hexene: 1mol 1,6-dichloro-2-hexene, 0.5g Cu 2 O and 2.5mol NaCN were placed in 1,4-dioxane, and the substitution reaction was carried out at 80°C for 5 hours to obtain 1,6-dicyano-2-hexene;

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

Embodiment 3

[0028] The preparation method of 1,3,6-hexanetrinitrile comprises the following steps:

[0029] A. Preparation of 1,6-dicyano-2-hexene: With 1,4-dioxane as the reaction solvent, 1mol 1,6-dichloro-2-hexene, 0.5g CuBr and 2.3mol NaCN Place in 1,4-dioxane, and carry out substitution reaction at 101°C for 7 hours to obtain 1,6-dicyano-2-hexene;

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

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Abstract

Provided is a method for preparing 1,3,6-hexanetricarbonitrile, comprising the following steps: A. preparation of 1,6-dicyano-2-butylene; and B. preparation of the 1,3,6-hexanetricarbonitrile. Provided is a new method for preparing 1,3,6-hexanetricarbonitrile. In addition to being a preparation method which is completely different from a traditional process, the preparation method also overcomes the safety problem present in the preparation of the 1,3,6-hexanetricarbonitrile in the presence of sodium, thus enabling the process to be safer, and at the same time, also achieving the requirements of large-scale industrial production. In addition, the preparation method of the present invention also has the advantages such as a high yield, easily available raw materials, a simple reaction control, and a high product purity.

Description

technical field [0001] The invention belongs to the technical field of compound preparation, and in particular relates to a preparation method of 1,3,6-hexanetrinitrile. Background technique [0002] 1,3,6-Hexanetrinitrile is mainly used as organic synthesis intermediate, high boiling point solvent, and electrolyte additive. At present, 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, and the continuous decomposition of the electrolyte will seriously affect the performance of the battery. It is imminent to add electrolyte additives to the electrolyte to improve the performance of the battery. [0003] The Journal of Applied Chemistry of the USSR (Journal of Applied Chemistry of the USSR, 1972, 2683-2684) discloses the preparation of 1,3,6- T...

Claims

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Application Information

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Patent Type & Authority Patents(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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