Purification method of, 1, 1-difluoroethane

A technology of difluoroethane and dichloroethane, applied in 1 field, can solve the problems of shortened catalyst life, short catalyst life, high equipment cost, etc.

Inactive Publication Date: 2006-12-13
SHOWA DENKO KK
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the purification method by extractive distillation requires many expensive facilities such as distillation towers, which disadvantageously results in high equipment costs, etc.
Also, the purification

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0073] Preparation example of crude 1,1-difluoroethane (raw material example 1)

[0074] Introduce 1,1-dichloroethane and hydrogen fluoride into a reactor filled with a catalyst (mainly containing trivalent chromium oxide), and react at a temperature of 290°C to produce mainly 1,1-difluoroethane, hydrogen chloride and unreacted hydrogen fluoride gas. Then, hydrogen fluoride and hydrogen chloride are removed by distillation or the like to obtain crude 1,1-difluoroethane.

[0075] CH 3 CHF 2

99.9461

CH 2 =CH 2

0.0018

CH 2 = CHF

0.0143

CH 3 CHClF

0.0013

CH 2 =CHCl

0.0261

CH 3 CHClF

0.0089

CH 2 =CCl 2

0.0012

CH 3 CHCl 2

0.0003

[0076] (unit: volume %)

[0077] Also, in the obtained crude 1,1-difluoroethane, the water content was 25 vol ppm, and the hydrogen fluoride content was 6 vol ppm.

Embodiment 2

[0079] Preparation example of crude 1,1-difluoroethane (raw material example 2)

[0080] The crude 1,1-difluoroethane obtained in Example 1 (Material Example 1) was further distilled according to a known method to obtain crude 1,1-difluoroethane.

[0081] CH 3 CHF 2

99.9666

CH 2 =CH 2

0.0006

CH 2 =CHF

0.0083

CH 3 CHClF

0.0011

CH 2 =CHCl

0.0178

CH 3 CHClF

0.0052

CH 2 =CCl 2

0.0004

[0082] (unit: volume %)

[0083] Also, in the obtained crude 1,1-difluoroethane, the water content was 23 vol ppm, and the hydrogen fluoride content was 6 vol ppm.

Embodiment 3

[0086] (unit: volume %)

[0087] Also, the water content in 1,1-difluoroethane obtained after purification was analyzed by the Karl Fischer method (water content analyzer), the result was 3 vol ppm, and the hydrogen fluoride content was measured by ion chromatography, the result was 1volppm.

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PUM

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Abstract

Crude 1,1-difluoroethane containing at least one compound selected from the group consisting of unsaturated compounds each having two carbon atoms within the molecule and saturated chlorine-containing compounds each having two carbon atoms within the molecule is brought into contact with a zeolite and/or a carbonaceous adsorbent, or crude 1,1-difluoroethane containing hydrogen fluoride and, as impurities, at least one compound selected from the group consisting of unsaturated compounds each having two carbon atoms within the molecule is brought into contact with a fluorination catalyst in a gas phase state. High-purity 1,1-difluoroethane usable as a cryogenic refrigerant, or as an etching gas, can be produced in an industrially advantageous manner.

Description

technical field [0001] The present invention relates to a purification method, production method and use of 1,1-difluoroethane. Background technique [0002] 1,1-Difluoroethane (CH 3 CHF 2 ) have attracted attention as, for example, cryogenic refrigerants or etching gases. [0003] For the production and purification methods of 1,1-difluoroethane, the following methods are generally employed, such as (1) a method of reducing chlorinated fluorinated hydrocarbons with hydrogen in the presence of a catalyst (see Japanese Unexamined Patent Publication No. 7 -126197 (JP-A-7-126197)), and (2) reacting chlorine in the gas phase by using a fluorination catalyst and reacting unsaturated compounds contained as impurities with oxides of copper, cobalt, silver, magnesium, etc. Ethylene (CH 2 =CHCl), 1-chloro-1-fluoroethane and other fluorinated methods (see European Unexamined Patent Publication No. 0370688). [0004] For example, CH produced by the method of reacting 1,1-dichloroe...

Claims

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Application Information

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IPC IPC(8): C07C17/389C07C19/08
Inventor 大野博基
Owner SHOWA DENKO KK
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