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Liquid phase purification method for 1,1- difluoroethane

A kind of technology of difluoroethane and purification method, applied in 1 field, can solve the problem that high purity cannot be satisfied

Inactive Publication Date: 2011-06-22
SINOCHEM LANTIAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method can basically purify 1,1-difluoroethane to more than 99.9%, the total olefin content is more than tens or even hundreds of ppm, and the content of vinyl chloride is more than 5 ppm, which still cannot meet the requirements of high-purity 1,1. - Requirements for difluoroethane

Method used

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  • Liquid phase purification method for 1,1- difluoroethane
  • Liquid phase purification method for 1,1- difluoroethane

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Add 108g of silica gel to the reaction tube, specific surface area: 750-850m 2 / g, average pore diameter: 22- Heating to keep the temperature in the reaction tube at about 10°C, and the pressure at about 2 atmospheres, feed chlorine gas into the reaction tube at a flow rate of 0.05 L / min for 2 hours, close the valve of the reaction tube, and seal it for 2 hours. Heating was stopped, the valve was opened, the reaction tube was purged with nitrogen, vacuumized, and the reaction tube was naturally cooled to normal temperature. Pass 97g of 1,1-difluoroethane crude product containing vinyl chloride into the reaction tube, the content of 1,1-difluoroethane is 99.992%, the content of vinyl chloride is 0.00201%, and the content of total olefins is 0.00219% , close the valve, and take a sample for gas chromatography analysis after contacting for 40 minutes. The content of 1,1-difluoroethane is 99.995%, the content of total olefins is 0.00032%, and the content of vinyl chloride...

Embodiment 2

[0030] Add 115g molecular sieve to the reaction tube, specific surface area: 830-860m 2 / g, average pore diameter: 14- Heating to keep the temperature in the reaction tube at about 350°C, and the pressure at about 5 atmospheres, feed chlorine gas into the reaction tube at a flow rate of 0.05 L / min for 3 hours, close the valve of the reaction tube, and seal it for 2 hours. Heating was stopped, the valve was opened, the reaction tube was purged with nitrogen, vacuumized, and the reaction tube was naturally cooled to normal temperature. 150 g of 1,1-difluoroethane crude product containing vinyl chloride was passed into the reaction tube, the content of 1,1-difluoroethane was 99.992%, the content of vinyl chloride was 0.00201%, and the content of total olefins was 0.00219%. Close the valve, take a sample after 40 minutes of contact and conduct gas chromatography analysis. The content of 1,1-difluoroethane is 99.995%, the content of total olefins is 0.00002%, and the content of v...

Embodiment 3

[0032] Add 85g zeolite to the reaction tube, specific surface area: 620-750m 2 / g, average pore diameter: 22- Heating to keep the temperature in the reaction tube at about 25°C, and the pressure at about 8 atmospheres, feed chlorine gas into the reaction tube at a flow rate of 0.05 L / min for 10 hours, close the valve of the reaction tube, and seal it for 2 hours. Heating was stopped, the valve was opened, the reaction tube was purged with nitrogen, vacuumized, and the reaction tube was naturally cooled to normal temperature. Pass 140 g of crude 1,1-difluoroethane containing vinyl chloride into the reaction tube, the content of 1,1-difluoroethane is 99.992%, the content of vinyl chloride is 0.00201%, and the content of total olefins is 0.00219% , close the valve, and take a sample after 40 minutes of contact for gas chromatography analysis. The content of 1,1-difluoroethane is 99.994%, the content of total olefins is 0.00016%, and the content of vinyl chloride is 0.00014%.

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Abstract

The invention relates to a method for purifying 1,1-difluoroethane through liquid phase adsorptive separation. An adsorbent which is one or a combination of more of silica gel, activated aluminium oxide, activated magnesium oxide and aluminosilicate absorbents and a carbon-based adsorbent is used, and an adsorbent, which has the BET surface area of more than or equal to 400m<2> / g and the single-point average pore size of about 5 and is capable of reducing the content of total olefins in crude chloroethylene-containing 1,1-difluoroethane to below 10ppm and reducing the content of chloroethylene to below several ppm and even below 1 ppm, is preferred. The 1,1-difluoroethane can be independently used, and also can be mixed with other materials to serve as a low temperature refrigerant, a foaming agent, a propellant, an etching gas, a cleaning agent or an intermediate of other fluorocarbon compounds.

Description

technical field [0001] The invention relates to a method for purifying 1,1-difluoroethane, especially a method for liquid phase adsorption separation. Background technique [0002] 1,1-difluoroethane (HFC-152a), boiling point at normal pressure -24.023°C, ODP value (ozone depletion potential value) is 0, GWP value (greenhouse effect potential value) is 0.03, is an excellent ozone depleting Substances (ODS) substitutes that can be used alone or mixed with other materials as cryogenic refrigerants, blowing agents, propellants, etching gases, cleaning agents or as intermediates for other fluorocarbons. [0003] The production methods of 1,1-difluoroethane (HFC-152a) mainly include acetylene method and vinyl chloride method. When vinyl chloride is used as raw material, 1,1-difluoroethane (HFC-152a) -152a) In addition to the product, there are unreacted vinyl chloride, hydrogen fluoride, vinyl fluoride and other organic by-products such as 1-fluoro-1-chloroethane). Most of the ...

Claims

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Application Information

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IPC IPC(8): C07C19/08C07C17/389B01J20/34
Inventor 潘彦郭荔赵卫娟柳彩波洪慧能黄友良
Owner SINOCHEM LANTIAN
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