Method for combined production of 1,1,2-trifluorotrichloroethane and 1,1,1-trifluorodichloroethane

A technology of 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, complex operation, and many by-products, and achieve the effects of easy control of reaction temperature, rich source of raw materials, and easy separation.

Active Publication Date: 2016-01-13
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 ad

Method used

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  • Method for combined production of 1,1,2-trifluorotrichloroethane and 1,1,1-trifluorodichloroethane
  • Method for combined production of 1,1,2-trifluorotrichloroethane and 1,1,1-trifluorodichloroethane
  • Method for combined production of 1,1,2-trifluorotrichloroethane and 1,1,1-trifluorodichloroethane

Examples

Experimental program
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Effect test

Example Embodiment

[0034] Example 1

[0035]In a 1L reaction autoclave, add 250g (1.05mol) of hexachloroethane, 250g (1.51mol) of tetrachloroethylene, 100g (0.33mol) of antimony pentachloride as a catalyst, and 400g (20mol) of hydrofluoric acid at one time. Stir, heat up to 90 ℃, and react for 8 hours. During the reaction, the pressure should be released regularly to keep the pressure at 1.5Mpa. When the pressure indicated that the number remained unchanged, the heating was stopped and the temperature was lowered. When the temperature drops below 25°C, the material is discharged, washed with water, washed with alkali, rectified and purified respectively 1,1,2-trifluorotrichloroethane and 1,1,1-trifluorodichloroethane. 168.12 g of 1,1,2-trifluorotrichloroethane were obtained with a yield of 85.2%, and 205.54 g of 1,1,1-trifluorodichloroethane with a yield of 89.2%.

Example Embodiment

[0036] Example 2

[0037] In a 1L reaction autoclave, add 250g (1.05mol) of hexachloroethane, 250g (1.51mol) of tetrachloroethylene, 100g (0.46mol) of antimony pentafluoride as a catalyst, and 400g (20mol) of hydrofluoric acid at one time. Stir, heat up to 120 ℃, and react for 7 hours. During the reaction, the pressure should be released regularly to keep the pressure at 1.5Mpa. When the pressure indicated that the number remained unchanged, the heating was stopped and the temperature was lowered. When the temperature drops below 25°C, the material is discharged, washed with water, washed with alkali, rectified and purified respectively 1,1,2-trifluorotrichloroethane and 1,1,1-trifluorodichloroethane. 178.65 g of 1,1,2-trifluorotrichloroethane were obtained with a yield of 90.33%, and 214.54 g of 1,1,1-trifluorodichloroethane with a yield of 94.2%.

Example Embodiment

[0038] Example 3

[0039] In a 1L reaction autoclave, add 300g (1.27mol) of hexachloroethane, 200g (1.2mol) of tetrachloroethylene, 100g (0.33mol) of antimony pentachloride as a catalyst, and 400g (20mol) of hydrofluoric acid at one time. Stir, heat up to 120 ℃, and react for 8 hours. During the reaction, the pressure should be released regularly to keep the pressure at 1.5Mpa. When the pressure indicated that the number remained unchanged, the heating was stopped and the temperature was lowered. When the temperature drops below 25°C, the material is discharged, washed with water, washed with alkali, rectified and purified respectively 1,1,2-trifluorotrichloroethane and 1,1,1-trifluorodichloroethane. 222.15 g of 1,1,2-trifluorotrichloroethane were 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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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
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