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Method for preparing 1,1,1,4,4,4-hexafluoro-2-butyne through gas phase method

A gas-phase method and butyne technology, which is applied in the field of gas-phase method for preparing 1,1,1,4,4,4-hexafluoro-2-butyne, can solve the problem of metal salt wastewater generation, high raw material price and low purity. problem, to achieve the effect of low cost, reduced production cost and high reaction efficiency

Active Publication Date: 2020-04-03
JUHUA GROUP TECH CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0021] This technical route solves the problems of high raw material price, low selectivity and low purity of 1,1,1,4,4,4-hexafluoro-2-butyne, but it needs to add a certain amount of surface Active agent, and a large amount of metal salt wastewater is generated, which is difficult to dispose of, and the environmental protection is facing challenges

Method used

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  • Method for preparing 1,1,1,4,4,4-hexafluoro-2-butyne through gas phase method
  • Method for preparing 1,1,1,4,4,4-hexafluoro-2-butyne through gas phase method
  • Method for preparing 1,1,1,4,4,4-hexafluoro-2-butyne through gas phase method

Examples

Experimental program
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Effect test

Embodiment 1

[0043] Pass hexafluoro-2-chloro-2-butene at a flow rate of 15.9g / min into a Hastelloy tube fixed-bed reactor with 30ml of barium chloride catalyst and an inner diameter of 30mm, control the contact time for 1s, and the reaction temperature at 100 °C, the crude product was collected and analyzed by chromatography. The conversion rate of hexafluoro-2-chloro-2-butene was 97%, and the selectivity of 1,1,1,4,4,4-hexafluoro-2-butyne was 99%.

Embodiment 2

[0045] Pass hexafluoro-2-chloro-2-butene at a flow rate of 0.53g / min into a silicon carbide tube fixed-bed reactor with 30ml of ferric chloride catalyst and an inner diameter of 30mm, control the contact time for 30s, and the reaction temperature at 300°C , the crude product was collected and analyzed by chromatography, the conversion rate was 96%, and the selectivity of 1,1,1,4,4,4-hexafluoro-2-butyne was 98%.

Embodiment 3

[0047] Pass hexafluoro-2-chloro-2-butene at a flow rate of 3.18g / min into a 30mm lnconel tube fixed-bed reactor equipped with 30ml of cesium fluoride catalyst, control the contact time for 5s, and the reaction temperature at 150°C. After the crude product was collected and analyzed by chromatography, the conversion rate of hexafluoro-2-chloro-2-butene was 95.5%, and the selectivity of 1,1,1,4,4,4-hexafluoro-2-butyne was 99%.

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Abstract

The invention discloses a method for preparing 1,1,1,4,4,4-hexafluoro-2-butyne through a gas phase method, wherein hexafluoro-2-chloro-2-butene as a raw material is subjected to a gas phase dehydrochlorination reaction under the catalytic action of a dechlorination catalyst to obtain 1,1,1,4,4,4-hexafluoro-2-butyne. The method has the advantages of simple process, economy, environmental protectionand easy industrialization.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a method for preparing 1,1,1,4,4,4-hexafluoro-2-butyne by a gas phase method. Background technique [0002] 1,1,1,4,4,4-hexafluoro-2-butyne is an important fluorine-containing fine chemical raw material, which can be used to synthesize key intermediates and As a monomer for fluoropolymers. Its polymer has acid and alkali resistance properties and can be used as a window for high-voltage equipment. Hexafluorobutyne is also a key intermediate for the preparation of the fourth-generation foaming agent cis (Z) hexafluoro-2-butene. [0003] The preparation methods of 1,1,1,4,4,4-hexafluoro-2-butyne in prior art reports mainly include the following: [0004] (1) Preparation of 1,1,1,4,4,4-hexafluoro-2-butyne from perchlorobutadiene [0005] Henne, A.L, Li Zongzhen, Henry N, etc. reported that perchlorobutadiene was used as raw material to fluorinate hexafluoro-2,3-dichlo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C21/22C07C17/23
CPCC07C17/23C07C21/22Y02P20/584
Inventor 王宗令李宏峰蒋琦徐宇宁苏兰辉
Owner JUHUA GROUP TECH CENT
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