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Method for preparing pentachloroethane by liquid phase chlorination of vinylidene chloride

A technology of vinylidene chloride and pentachloroethane is applied in the field of preparation of pentachloroethane, can solve the problems of high raw materials, high production cost, high production cost, poor economic benefit and the like, and achieves high material utilization rate, simple method, Easy to operate effect

Active Publication Date: 2011-12-28
江西国宏化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The traditional pentachloroethane production process uses trichlorethylene as raw material for production, but its production cost is high and economic benefit is poor
[0004] Patent application number CN200810024583.6 "a preparation method of pentafluoroethane", but it still uses trichlorethylene as raw material, then generates pentachloroethane, and then enters the gas phase fluorination of pentachloroethane to prepare pentafluoroethane Fluoroethane, so its raw material, production cost of this method are still on the high side

Method used

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  • Method for preparing pentachloroethane by liquid phase chlorination of vinylidene chloride
  • Method for preparing pentachloroethane by liquid phase chlorination of vinylidene chloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] In a 250ml four-necked flask, a chlorine inlet pipe, a reflux condenser, a thermometer and an electric stirrer are respectively installed, and 147ml (180 grams) of high-purity vinylidene chloride liquid is added into the flask from the feeding port, and the addition of a weight percentage is 80% ferric chloride, 20% cesium chloride, 0.9 gram of catalyst A mixed with 150~250 mesh solid powder, under stirring, feed into the tube from chlorine gas, lead to 2~3 kg / cm Pressure chlorine gas, and partial The molar ratio of vinyl chloride to chlorine gas is 1:1.1~1.4, the initial reaction temperature is 20~25°C, and the temperature is gradually raised to 70°C~80°C, and the prepared chlorinated liquid is tested once every two hours of reaction. When the content of vinyl chloride is less than 1%, the reaction of the first stage is terminated, the reaction time is 15.5 hours, and cooled to room temperature through a heat exchanger, then adding 75% aluminum chloride and 25% cesium c...

Embodiment 2

[0018] In the four-necked flask of 1000ml, respectively install chlorine inlet pipe, reflux condenser, thermometer and electric stirrer, add liquid vinylidene chloride liquid 590ml (700 grams) in the flask from the feeding port, and add the 75% by weight Ferric chloride, 15% antimony chloride, 10% cesium chloride, and 3.6 grams of catalyst A mixed with 150-250 mesh solid powder are passed into the tube from chlorine gas under stirring, and the pressure is 2-3 kg / cm 2 Chlorine under pressure, and the molar ratio of vinylidene chloride to chlorine is 1:1.1~1.4, the initial reaction temperature is 20~25°C, and the temperature is gradually raised to 65°C~75°C, and the reaction is detected once every two hours. Chlorinated liquid, when the content of vinylidene chloride is less than 1%, the first stage reaction is terminated, the reaction time is 17 hours, cooled to room temperature through a heat exchanger, and then added with 70% aluminum chloride, 15% Antimony chloride, 15% cesi...

Embodiment 3

[0020] at 10 meters 3 Drop into 7000 kilograms of liquid vinylidene chlorides in the chlorination reactor, add the ferric chloride of 75%, 25% cesium chloride, mix 35 kilograms of catalyst A with 150~250 purpose solid powders, under stirring from The chlorine gas inlet pipe is passed at 2 to 3 kg / cm 2 Chlorine under pressure, and the molar ratio of vinylidene chloride to chlorine is 1:1.1~1.4, the initial reaction temperature is 20~25°C, and the temperature is gradually raised to 75°C~less than 85°C, and the reaction time is detected once every two hours. The obtained chlorinated liquid, when the content of vinylidene chloride was less than 1%, was the termination of the first-stage reaction, and the reaction time was 20 hours, and was cooled to room temperature through a heat exchanger, and then adding weight percent was 80% aluminum chloride, Mix 10% antimony chloride and 10% cesium chloride with 150-250 mesh solid powder to form 35 kg of catalyst B, heat the reaction solut...

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Abstract

The invention provides a method for preparing pentachloroethane by liquid phase chlorination of vinylidene chloride. The method comprises the following steps: putting vinylidene chloride into a reactor and adding metal halides comprising one or combination, serving as a catalyst A, of more than two of ferric chloride, aluminum chloride, cobalt chloride, copper chloride, calcium chloride, manganese chloride, chromic chloride, barium chloride, cesium chloride and antimony chloride, introducing nitrogen under the conditions of mixing and stirring, carrying out intermittent reaction at the temperature of 20-less than 85 DEG C at normal pressure so as to prepare tetrachlorethane; adding one or combination, serving as a catalyst B, of more than two of metal halides, introducing pressure chlorine under the conditions of mixing and stirring, carrying out intermittent reaction at the temperature of 85-130 DGE C at normal pressure so as to prepare a pentachloroethane crude product; and directlycarrying out water alkali washing and rectification on the crude product so as to prepare a pentachloroethane finished product. According to the invention, the problem that the costs of raw materialsin the original production are relatively high is fundamentally solved because vinylidene chloride is used as the raw material; and simultaneously, a novel, high-quality and inexpensive method is provided for preparation of pentachloroethane, and the method is simple, is easy to operate and is suitable for industrial production in large batch, and the purity and yield of the product are high.

Description

technical field [0001] The invention relates to a method for preparing pentachloroethane, in particular to a method for preparing pentachloroethane by liquid-phase chlorination of vinylidene chloride. Background technique [0002] Because pentachloroethane is a main organic chlorine product, it is the main raw material for the production of tetrachloroethylene (PCE) and refrigerant pentafluoroethane (HFC125), and tetrachloroethylene has a wide range of industrial uses, mainly It is used for fabric dry cleaning and metal degreasing. It is restricted or banned by a series of international standards along with traditional refrigerants containing chlorinated halogenated alkanes, but it can be used as a substitute for chlorine-free fluoroalkanes. It can also be used as a refrigerant difluoro- Chlorine (HCFC-123) is used as an intermediate of pentafluoroethane HFC125 and HFC134a. Therefore, the demand for tetrachloroethylene (PCE) has increased greatly, and as the main raw materia...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C19/043C07C17/06
Inventor 黄志强汪国良
Owner 江西国宏化工有限公司
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