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Preparation method of 2,2-bis(3,4-dimethylphenyl)hexafluoropropane

A technology of hexafluoropropane and xylyl, which is applied in the field of preparation of 2,2-dihexafluoropropane, which can solve the problems of strong toxicity and difficult transportation of hexafluoroacetone

Inactive Publication Date: 2017-05-24
ZHEJIANG LANTIAN ENVIRONMENTAL PROTECTION HI TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction yield is only 67%, and the raw material hexafluoroacetone used is extremely toxic and difficult to transport

Method used

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  • Preparation method of 2,2-bis(3,4-dimethylphenyl)hexafluoropropane
  • Preparation method of 2,2-bis(3,4-dimethylphenyl)hexafluoropropane

Examples

Experimental program
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Effect test

Embodiment 1

[0024] In a 500mL three-neck flask equipped with magnetic stirring, condenser, oil bath heating, and water separator, add 82g (0.372mol) of hexafluoroacetone trihydrate and 80g (0.754mol) of o-xylene, layer, stir, and react The liquid is a milky white mixture, warming up to the reflux temperature, water is separated out in the water separator (about 40g o-xylene is added in the water separator), and the heating is continued to reflux until basically no water is released, and the liquid in the reaction bottle is colorless and transparent, which is o-xylene. Mixture of xylene and hexafluoroacetone monohydrate; middle and lower layer of water trap 15g, 11.9mL, density 1.26g / cm 3 , a small amount of hexafluoroacetone trihydrate separated out.

[0025] Add the mixture of o-xylene and hexafluoroacetone monohydrate obtained above into a 0.5L autoclave, add 127g (6.35mol) of hydrofluoric acid, start stirring, raise the temperature to 115°C for about 17h, and the reaction pressure is a...

Embodiment 2

[0028] In a 500mL three-neck flask equipped with magnetic stirring, condenser, oil bath heating, and water separator, add 82g (0.372mol) of hexafluoroacetone trihydrate and 80g (0.754mol) of o-xylene, layer, stir, and react The liquid is a milky white mixture, warming up to the reflux temperature, water is separated out in the water separator (about 40g o-xylene is added in the water separator), and the heating is continued to reflux until basically no water is released, and the liquid in the reaction bottle is colorless and transparent, which is o-xylene. Mixture of xylene and hexafluoroacetone monohydrate; middle and lower layer of water trap 15g, 11.9mL, density 1.26g / cm 3 , a small amount of hexafluoroacetone trihydrate separated out.

[0029] Add the mixture of o-xylene and hexafluoroacetone monohydrate obtained above into a 0.5L autoclave, add 150g (7.5mol) of hydrogen fluoride and hydrofluoric acid, start stirring, raise the temperature to 125°C for about 25 hours, and ...

Embodiment 3

[0032] In a 500mL three-neck flask equipped with magnetic stirring, condenser, oil bath heating, and water separator, add 82g (0.372mol) of hexafluoroacetone trihydrate and 90g (0.85mol) of o-xylene, layer, stir, and react The liquid is a milky white mixture, warming up to the reflux temperature, water is separated out in the water separator (about 40g o-xylene is added in the water separator), and the heating is continued to reflux until basically no water is released, and the liquid in the reaction bottle is colorless and transparent, which is o-xylene. Mixture of xylene and hexafluoroacetone monohydrate; middle and lower layer of water separator 16g, 12.3mL, density 1.30g / cm 3 , a small amount of hexafluoroacetone trihydrate separated out.

[0033] Add the mixture of o-xylene and hexafluoroacetone monohydrate obtained above into a 0.5L autoclave, add 111g (5.58mol) of hydrogen fluoride and hydrofluoric acid, start stirring, raise the temperature to 100°C for about 13 hours,...

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Abstract

The invention discloses a method used for preparing 2,2-bis(3,4-dimethylphenyl)hexafluoropropane. According to the method, 2,2-bis(3,4-dimethylphenyl)hexafluoropropane is obtained via liquid phase reaction of o-xylene with hexafluoroacetone monohydrate under the action of hydrogen fluoride. The raw materials of the method are low in toxicity; reaction pressure is low; operation is convenient; reaction selectivity and yield are high; and the method is suitable for industrialized production. 2,2-bis(3,4-dimethylphenyl)hexafluoropropane prepared via the method can be taken as an intermediate to synthesize fluorine-containing polyimide.

Description

technical field [0001] The invention relates to a preparation method of 2,2-bis(3,4-xylyl)hexafluoropropane. Background technique [0002] 2,2-bis(3,4-xylyl)hexafluoropropane is an important monomer whose structural formula is as follows: [0003] [0004] It can be used to synthesize 2,2-bis(3,4-dicarboxylic acid)hexafluoropropane dianhydride (6-FDA). The fluorine-containing polyimide synthesized from 2,2-bis(3,4-dicarboxylic acid) hexafluoropropane dianhydride (6-FDA) has good properties, such as low dielectric constant and low absorption And good thermodynamic stability, it can be used not only as a dielectric in coatings and electronic applications, but also as the main component of other polymers such as optical fibers and liquid crystals. [0005] For the preparation method of 2,2-bis(3,4-xylyl)hexafluoropropane, following reports are arranged in the prior art: [0006] Chinese patent CN101696199 has reported the preparation method of 2,2-bis(3,4-xylyl)hexafluoro...

Claims

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Application Information

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IPC IPC(8): C07C22/08C07C17/263
CPCC07C17/2637C07C22/08
Inventor 赵卫娟徐卫国杨箭张勇耀
Owner ZHEJIANG LANTIAN ENVIRONMENTAL PROTECTION HI TECH
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