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Composite catalyst and process for preparing fluorohydrocarbon by liquid-phase fluorination

A combined catalyst and liquid-phase fluorination technology, which is applied in the preparation of halogenated hydrocarbons, organic chemistry, chemical instruments and methods, etc., can solve the problems of rising costs, increasing the amount of three wastes to be treated, unfavorable industrial continuous production, etc., to achieve enhanced activity, The effect of prolonging the service life

Inactive Publication Date: 2004-10-20
苏州联氟化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are also defects in this type of preparation process, that is, when using halogenated hydrocarbons with hydrogen atoms as raw materials to prepare hydrofluorocarbons, the activity of the catalyst will decrease rapidly due to the polymerization of raw materials and the cracking of polymers, which will often lead to This will not only increase the cost and increase the amount of three wastes to be treated, but also is very unfavorable for large-scale industrial continuous production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Embodiment one: the preparation of difluoromethane

[0015] Add 60 g of SbCl to a 1 L autoclave with packed column and reflux condenser 5 , 30 grams of perfluorooctanesulfonyl fluoride, and then add 100 grams of anhydrous hydrogen fluoride. Slowly raise the temperature to 80°C and react for 42 hours, then continuously feed into the reactor at the rate of 1.5 mol / hour of dichloromethane and 3.3 mol / hour of hydrogen fluoride. Adjust the temperature at the top of the tower between 0-5°C, and maintain the pressure at about 15 kg / cm2. The reaction product is continuously drawn from the top of the condenser, washed with water, washed with alkali, analyzed by gas chromatography, and then compressed into the collector for metering. The catalyst activity did not decrease after continuous feeding for 200 hours. The composition of the product is 98.4% of difluoromethane, 1.5% of monochlorofluoromethane, and 0.1% of raw material dichloromethane. Collect 14.98 kilograms of react...

Embodiment 2

[0017] Example 2: Preparation of 1,1-dichloro-1 fluoroethane

[0018] On the same reaction device as in Example 1, prepare in a similar manner, add 60 grams of SnCl 4 , 20 g CF 3 (CF 2 ) 6 SO 2 F, the reaction temperature is at 35°C, according to CCl 2 =CH 2 The rate of 1.5 mol / hour and 1.6 mol / hour of HF were continuously fed into the reactor, and the catalyst activity did not decrease significantly after 200 hours of continuous feeding. The content of 1,1-dichloro-1fluoroethane in the product is 99.1%, and the catalyst efficiency is 674g / g.

Embodiment 3

[0019] Example 3: Preparation of 1-chloro-1,1-difluoroethane

[0020] On the same reaction device as in Example 1, prepare in a similar manner, add 50 grams of SnCl 4 , 25 g CF 3 (CF 2 ) 3 COF, reaction temperature at 45°C, press CCl 2 =CH 2 1.5 mol / hour and HF 3.15 mol / hour were continuously fed into the reactor, and the catalyst activity did not decrease significantly after 200 hours of continuous feeding. The content of 1-chloro-1,1-difluoroethane in the product was 95.2%, and the catalyst efficiency was 551 g / g.

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PUM

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Abstract

A composite catalyst for preparing fluorohydrocarbon by liquid-phase fluorinating is prepared from lewis acid as primary catalyst and RfCOA or RfSO2A as Co-catalyst through mixing. Its fluorinating process features are that in the presence of said composite catalyst, the chlorocarbon and hydrogen fluoride take part in reaction at 10-15 deg.C. Its advantages are high activity, long service life and high conversion and selectivity of product.

Description

technical field [0001] The invention relates to a combined catalyst used for preparing hydrofluorocarbons by a liquid-phase catalytic fluorination method, and a fluorination process for preparing hydrofluorocarbons using the catalyst. Background technique [0002] The preparation of hydrofluorocarbons by liquid-phase catalytic fluorination of halogenated hydrocarbons with hydrogen fluoride in the presence of a Lewis acid catalyst is a well-known method, and the Lewis acid catalyst commonly used in this method is SbCl 5 , SbF 5 、TiCl 4 , SnCl 4 , TaCl 5 , TaF 5 , NbCl 5 , NbF 5 、FSO 3 H, ClSO 3 H and their mixtures. For example, Chinese patent CN1151724 discloses a method for preparing difluoromethane by liquid-phase fluorination of dichloromethane and hydrogen fluoride in the presence of an antimony pentafluoride catalyst. At a reaction temperature of 100°C and a reaction pressure of 17 kg / cm2, The conversion rate of methane is 99%, and the se...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C17/00C07C17/35C07C19/08
Inventor 徐联福
Owner 苏州联氟化学有限公司