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Method for removing hexafluoro-chlorobutylene from trifluoro-dichloroethane

A technology of trifluorodichloroethane and hexafluorochlorobutene is applied in the field of purification using photocatalytic oxidation, which can solve the problems such as failure to solve the recycling and reuse of adsorbents, and achieves fast reaction speed, high processing efficiency, and high retention rate. short time effect

Active Publication Date: 2013-12-04
福建舜跃科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it failed to solve the problem of recycling and reuse of adsorbents, and a large amount of solid waste containing hexafluorochlorobutene caused a certain pressure on the environment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add 3L of R123 containing about 1% hexafluorochlorobutene in a 5L glass reactor, pass in about 17g of chlorine gas under stirring to dissolve in the bottom liquid, and then pass oxygen into the reactor at a speed of 200 ml / min , the molar ratio of oxygen to hexafluorochlorobutene is 1:1, and the high-pressure mercury lamp is turned on, and the mercury lamp is placed in the middle of the quartz tube, and the lamp tube is cooled with compressed air. Under the control of mercury lamp heating and air cooling or water cooling, the photocatalytic liquid phase oxidation reaction is carried out at 20°C, the substance A produced by the reaction and the mixed gas produced by the vaporization of R123 due to the heat of the mercury lamp and the heat of reaction flow from the top of the reactor Continuous discharge, the discharged gas is cooled at -20°C, R123 is condensed and returned to the reactor, and the uncondensed substance A is collected after compression and condensation.

...

Embodiment 2

[0030] The reaction is carried out in a φ50mm, L=500mm glass reactor, a φ25mm, L=400mm quartz tube is placed in the middle of the reactor, a 500w mercury lamp is placed in the middle of the quartz tube, and the lamp tube is cooled with compressed air. Add chlorine gas with a molar ratio of 1% (based on R123) to R123 containing about 1% hexafluorochlorobutene by mass ratio, mix uniformly and vaporize, and enter the reactor after being measured by a flow meter with a flow rate of 1200ml / min. Feed oxygen into the reactor, the flow rate of oxygen is 20ml / min, the molar ratio of oxygen to hexafluorochlorobutene is 2: 1, and a 500W mercury lamp is turned on to carry out photocatalytic gas-phase oxidation reaction at 100°C; the reacted substance A is three Fluoroacetyl chloride gas is hydrolyzed and absorbed, and trifluoroacetyl chloride is hydrolyzed into trifluoroacetic acid. After concentration, the finished product of trifluoroacetic acid is obtained. Hexafluorochlorobutene impur...

Embodiment 3

[0032]Add 3L of R123 containing about 1ppm hexafluorochlorobutene in a 5L glass reactor as the bottom liquid, then pass oxygen into the reactor at a speed of 20 ml / min, the molar ratio of oxygen to hexafluorochlorobutene The ratio is 5:1, and a 400w high-pressure mercury lamp is turned on to carry out photocatalytic liquid-phase oxidation reaction at 0°C. The substance A produced by the reaction and the mixed gas produced by the gasification of R123 due to the heat of the mercury lamp and the heat of reaction are continuously discharged from the top of the reactor. After the discharged gas is cooled at -20°C, R123 is condensed and returned to the reactor, and the uncondensed substance A is collected after being compressed and condensed. The bottom liquid was analyzed by chromatography, and no hexafluorochlorobutene impurity was detected.

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Abstract

The invention relates to a method for purifying trifluoro-dichloroethane, in particular to a purifying method adopting photo-catalytic oxidation. Oxygen is bubbled into a reaction vessel, under the ordinary pressure, the photo-catalytic oxidation is carried out on the trifluoro-dichloroethane containing hexafluoro-chlorobutylene, under the photo-catalytic oxidation, the hexafluoro-chlorobutylene is oxidized into a substance A, the reaction can be carried out in the gas phase or the liquid phase, and the molar ratio between the oxygen and the hexafluoro-chlorobutylene is 1-5:1. Under the situation of the method, hexafluoro-chlorobutylene which is a toxicity controlled substance can be rapidly oxidized into the substance A, and the substance A is safe, reliable, free of toxicity and capable of being recycled after analysis. Hazardous substances are not generated in the whole production process, and the method is green and environmentally friendly.

Description

technical field [0001] The invention relates to a purification method of trifluorodichloroethane, in particular to a purification method using photocatalytic oxidation. Background technique [0002] 1,1,1-Trifluoro-2,2-dichloroethane, referred to as trifluorodichloroethane, is commercially referred to as R123, and its ODP value and GWP value are both 0.02. It is the main refrigerant working fluid Used to replace R11 as a refrigerant for large chillers; in the fire protection industry, R123 is mixed with other components and can be used as a substitute for Halon 1301. In addition, R123 can also be used as a raw material for foaming agent, cleaning agent and other fine fluorine chemical products such as R125 and trifluoroacetic acid. At present, there are two main process routes for the production of R123 in my country. One is to first synthesize trifluoro-chloroethane by fluorination with trichloroethylene as the starting material, and then to synthesize R123 by chlorination...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C19/12C07C17/395C07C53/18C07C51/04C01B7/01
Inventor 崔觉剑韩箴贤徐梦甜赵建明
Owner 福建舜跃科技股份有限公司
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