Preparation of high purity, 1,1,1-trifluoro-2,2,-dichloroethane

A technology for trifluorochloroethane and dichloroethane, which is applied in the field of high purity 1, can solve the problems of unsatisfactory olefin impurity effect and poor selectivity, and achieves the advantages of improving energy and chlorine utilization efficiency, convenient regeneration, and simplifying process flow. Effect

Active Publication Date: 2006-09-06
中化蓝天氟材料有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the common activated carbon catalyst has an unsatisfactory effect of removing olefin impurities, and the selectivity is poor. In the prior art trifluorodichloroethane purification process, there is no alternative activated carbon catalytic chlorination method to purify the trifluorodichloroethane product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Fluorination and chlorination: Trifluorochloroethane (R133a) is synthesized by fluorination of trichlorethylene, and after thermal chlorination, trifluorochloroethane (R133a), trifluorodichloroethane (R123), and trifluorotrifluoroethane are obtained. The mixed gas of ethyl chloride (R113a) and other impurities, after deacidification, olefin impurities ≥ 2000ppm.

[0027] Coconut shell activated carbon preparation: choose granular coconut shell activated carbon with an average particle diameter of 2-4 mm, and first fully soak it with a 30% hydrofluoric acid solution. Then wash with distilled water, and send the cleaned activated carbon to an oven for drying at a temperature of at least 120°C or higher to fully remove moisture; first use nitrogen to activate at the reaction temperature to further remove possible moisture or Ashes, and then activated with chlorine for a period of time to achieve full adsorption of chlorine on the surface of the activated carbon catalyst, ...

Embodiment 2

[0034] The reaction temperature of catalytic chlorination keeps 200 ℃ constant, and the mixed gas obtained by chlorine gas and thermal chlorination is controlled feed rate when respectively 1 / 40, 1 / 20, 1 / 10 by weight ratio, and all the other are the same as embodiment 1.

[0035] The results of each test are shown in Table 2.

[0036] components

Embodiment 3

[0038] See Table 3 for the amounts of R113a, R133a, R123, and R1326 contained in the mixed gas obtained by thermal chlorination.

[0039] When the reaction temperature of the catalytic chlorination reaction is 200°C, the weight ratio of the mixed gas feed obtained by controlling the chlorine gas and thermal chlorination is 2 / 30, 2 / 20, 1 / 10, 1 / 20 respectively, and the rest are the same as in Example 1 .

[0040] When the reaction temperature of the catalytic chlorination reaction is 180° C., the feed weight ratios of the chlorine gas and the mixed gas are controlled to be 1 / 10 respectively, and the rest are the same as in Example 1.

[0041] The liquid chromatography analysis results of the main components of each reaction product are shown in Table 3.

[0042] T

[0043] The items ticked in the remarks column in the table are the analysis results of R113a, R133a, R123, and R1326 in the mixed gas obtained after thermal chlorination.

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Abstract

Production of high-purity 1,1,1-triflu-2,2dichloroethane. It is carried out by fluoridizing, thermal fluoridizing triclene, obtaining the mixed gas containing fluothane, trifluo-dichloroethane and trifluo-trichlorineethane, catalytic chlorinating reacting the mixed gas under 160-250deg.C by coir active carbon, alkali washing the reacted gas by water, fractional distilling and condensing, and obtaining the purified product. It advantages include simple process, to improve energy utilizing rate, lower process load, and realize clean production.

Description

technical field [0001] The invention belongs to the technical field of organic fluorine chemical industry, and particularly relates to the catalytic chlorination method to purify trifluorochloroethane, trifluorodichloroethane, trifluorotrichloro Mixed gas of ethane to prepare high-purity 1,1,1-trifluoro-2,2 dichloroethane (R123) product method, Background technique [0002] 1,1,1-Trifluoro-2,2-dichloroethane, referred to as trifluorodichloroethane, the trade name is HCFC-123 or R123, the GWP and ODP of the product are both 0.02. R123 has a wide range of applications. In the refrigerant, R123 is mainly 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; At the same time, R123 can replace R113 as a cleaning agent and foaming agent; it can also be used as a raw material to produce pentafluoroethane (R125) and trifluoroacetic acid, etc....

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C19/08C07C17/04
Inventor 柳彩波白占旗
Owner 中化蓝天氟材料有限公司
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