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A method for co-producing 1,1,2-trifluorotrichloroethane and 1,1,1-trifluorodichloroethane

A technology for trifluorodichloroethane and trifluorotrichloroethane, applied in the field of co-production of 1,1,2-trifluorotrichloroethane and 1,1,1-trifluorodichloroethane, It can solve the problems of low equipment production capacity, many by-products, and low selectivity, and achieve the effects of easy control of reaction temperature, easy separation and extraction, and easy reaction feed

Active Publication Date: 2019-01-15
JUHUA GROUP TECH CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that a large amount of by-product 1,1,1,2-tetrafluoroethane is generated, which causes the selectivity of F123 to be very low, less than 15%.
The first method is intermittent operation, and it is solid feeding, which is troublesome. In addition, the production capacity of the equipment is low, and the treatment of three wastes is also troublesome.
The second method produces many by-products, low selectivity of the target product, cumbersome separation and purification, high cost, complicated operation, etc.

Method used

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  • A method for co-producing 1,1,2-trifluorotrichloroethane and 1,1,1-trifluorodichloroethane
  • A method for co-producing 1,1,2-trifluorotrichloroethane and 1,1,1-trifluorodichloroethane
  • A method for co-producing 1,1,2-trifluorotrichloroethane and 1,1,1-trifluorodichloroethane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035]In a 1L reaction autoclave, add 250g (1.05mol) of hexachloroethane, 250g (1.51mol) of tetrachloroethylene, 100g (0.33mol) of catalyst antimony pentachloride, and 400g (20mol) of hydrofluoric acid at one time, and start Stir, heat up to 90°C, and react for 8 hours. During the reaction, the pressure should be released regularly to keep the pressure at 1.5Mpa. When the pressure indication remains unchanged, stop heating and cool down. When the temperature drops below 25°C, discharge the material, wash with water, wash with alkali, rectify and purify 1,1,2-trifluorotrichloroethane and 1,1,1-trifluorodichloroethane respectively. 168.12 g of 1,1,2-trifluorotrichloroethane was obtained, with a yield of 85.2%, and 205.54 g of 1,1,1-trifluorodichloroethane, with a yield of 89.2%.

Embodiment 2

[0037] In a 1L reaction autoclave, add 250g (1.05mol) of hexachloroethane, 250g (1.51mol) of tetrachloroethylene, 100g (0.46mol) of catalyst antimony pentafluoride, and 400g (20mol) of hydrofluoric acid at one time. Stir, heat up to 120°C, and react for 7 hours. During the reaction, the pressure should be released regularly to keep the pressure at 1.5Mpa. When the pressure indication remains unchanged, stop heating and cool down. When the temperature drops below 25°C, discharge the material, wash with water, wash with alkali, rectify and purify 1,1,2-trifluorotrichloroethane and 1,1,1-trifluorodichloroethane respectively. 178.65 g of 1,1,2-trifluorotrichloroethane was obtained, with a yield of 90.33%, and 214.54 g of 1,1,1-trifluorodichloroethane, with a yield of 94.2%.

Embodiment 3

[0039] In a 1L reaction autoclave, add 300g (1.27mol) of hexachloroethane, 200g (1.2mol) of tetrachlorethylene, 100g (0.33mol) of catalyst antimony pentachloride, and 400g (20mol) of hydrofluoric acid at one time, and start Stir, heat up to 120°C, and react for 8 hours. During the reaction, the pressure should be released regularly to keep the pressure at 1.5Mpa. When the pressure indication remains unchanged, stop heating and cool down. When the temperature drops below 25°C, discharge the material, wash with water, wash with alkali, rectify and purify 1,1,2-trifluorotrichloroethane and 1,1,1-trifluorodichloroethane respectively. 222.15 g of 1,1,2-trifluorotrichloroethane was obtained, with a yield of 93.6%, and 162.77 g of 1,1,1-trifluorodichloroethane, with a yield of 88.35%.

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Abstract

The invention discloses a method for combined production of 1,1,2-trifluorotrichloroethane and 1,1,1-trifluorodichloroethane. The method comprises the following steps: adding reaction raw materials comprising hydrofluoric acid, hexachloroethane and tetrachloroethylene into a reaction autoclave according to a molar ratio of (10-40):(0.8-2.5):(1.2-3.6), reacting, adding a catalyst for catalysis, reacting at 30-250DEG C under 0.3-3.0Mpa for 2-12h, washing with water, washing with an alkali, and carrying out rectifying purification to obtain the products 1,1,2-trifluorotrichloroethane and 1,1,1-trifluorodichloroethane, wherein the catalyst can be metal fluoride or metal chloride, the metal fluoride comprises AlF3, SbF3, SbF5 and ZnF2, and the metal chloride comprises SbCl5. The synthetic method has the advantages of abundant sources and low price of the raw materials, high reaction yield, easy reaction feeding, easy separation and extraction of the generated products, and realization of industrial continuous production.

Description

technical field [0001] The present invention relates to a kind of method that co-production prepares 1,1,2-trifluorotrichloroethane and 1,1,1-trifluorodichloroethane, especially relates to a method for combining hexachloroethane and tetrachloroethylene Process for the preparation of 1,1,2-trifluorotrichloroethane and 1,1,1-trifluorodichloroethane. Background technique [0002] 1,1,1-Trifluorodichloroethane, the molecular formula is CF 3 CCl 2 H, referred to as F123, has excellent physical and chemical properties, ODS value of 0.02, GWP value of 92, no adverse effects on the atmospheric ozone layer, is a new type of polyurethane foaming agent, can be used as a refrigerant to replace CFC-11, and can also be As a cleaning agent instead of CFC-113. [0003] Patent WO95 / 16654 describes the reaction of F133a with chlorine and hydrogen fluoride to generate F123 at a temperature of 340°C and metal chromium as a catalyst. The disadvantage of this method is that a large amount of ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C19/12C07C17/087C07C17/35
Inventor 王宗令朱宏宇王树华周强罗孟飞方伟
Owner JUHUA GROUP TECH CENT