1-chloro-2,2-difluoroethylene preparation method

A technology of difluoroethylene and R122, which is applied in the field of preparation of 1-chloro-2,2-difluoroethylene, can solve the problems of large amount of reaction solvent, expensive raw materials, poor reaction selectivity, etc., and achieves low cost and low raw material cost. Low, mild response

Active Publication Date: 2013-03-27
SINOCHEM LANTIAN +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0017] In summary, the existing methods for preparing 1-chloro-2,2-difluoroethylene have the disadvantages of expensive catalysts, poor reaction selectivity, expensive raw materials, high cost, large amount of reaction solvent, low product yield, or A series of problems such as a large amount of three wastes are produced in the reaction process, which makes it difficult to realize the industrial production of 1-chloro-2,2-difluoroethylene

Method used

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Examples

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Embodiment 1

[0052] Example 1 Zinc powder pretreatment

[0053] Stir 1.2kg of zinc powder with 3 L 2% hydrochloric acid for 1 hour, filter to remove the acid, put the zinc powder in a 5 L beaker, wash once with 3 L 2% hydrochloric acid, and then wash three times with distilled water (each time 3 L), then washed twice with 95% ethanol (2 L each time), and finally washed once with 2 L of anhydrous ether. Filter after each wash to remove the wash solution. The treated zinc powder is thoroughly dried under the protection of nitrogen, and the lumps are ground in a mortar. After the treatment, the zinc powder was obtained under the protection of nitrogen for standby use.

[0054]

Embodiment 2

[0056] A two-stage reflux condenser is connected to a 5-liter there-necked bottle equipped with a mechanical stirrer and a constant-pressure dropping funnel, wherein the first-stage reflux condenser is cooled by tap water, and the second-stage reflux condenser is condensed by circulating alcohol in a refrigerator. Control the temperature of the alcohol at -10~-20°C, the generated product is exported through the reflux condenser, and the product is collected into a steel cylinder by circulating anhydrous alcohol in a refrigerator, and the temperature of the absolute alcohol is controlled at -50~-60°C. The reaction bottle was heated by an oil bath, and the reaction temperature was controlled by an electronic temperature controller.

[0057] Replace the above device with nitrogen, add 1 liter of sulfolane (industrial product, Liaoyang Guanghua Chemical Co., Ltd.), 113 grams of activated zinc powder (analytical pure, Shanghai Shenxiang Chemical Reagent Co., Ltd.) Sodium sulfite, r...

Embodiment 3

[0062] A two-stage reflux condenser is connected to a 5-liter there-necked bottle equipped with a mechanical stirrer and a constant-pressure dropping funnel, wherein the first-stage reflux condenser is cooled by tap water, and the second-stage reflux condenser is condensed by circulating alcohol in a refrigerator. Control the temperature of the alcohol at -10~-20°C, the generated product is exported through the reflux condenser, and the product is collected into a steel cylinder by circulating anhydrous alcohol in a refrigerator, and the temperature of the absolute alcohol is controlled at -50~-60°C. The reaction bottle was heated by an oil bath, and the reaction temperature was controlled by an electronic temperature controller.

[0063] Replace the above device with nitrogen, add 2 liters of 1,4-dioxane (China Wulian Chemical Factory), 325 grams of activated zinc powder (analytical grade, Shanghai Shenxiang Chemical Reagent Co., Ltd.) and 15 grams of sodium dithionite was re...

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Abstract

The invention discloses a method for preparing 1-chloro-2,2-difluoroethylene through treating difluorotrichloroethane which is a byproduct in the production of trifluorodichloroethane as a raw material. The addition of a reaction assistant in a reaction process can substantially improve the raw material conversion rate and the product yield. The prepared 1-chloro-2,2-difluoroethylene is an important fluorine fine chemical engineering raw material, and can be used in the production of fluorine-containing finishing agents, fluorine-containing surfactants and other fluorine-containing fine chemicals as a key intermediate.

Description

technical field [0001] The invention relates to a preparation method of 1-chloro-2,2-difluoroethylene, in particular to a method for preparing 1-chloro-2,2-difluoroethylene by using difluorotrichloroethane as a raw material. [0002] Background technique [0003] Trifluorodichloroethane (HCFC-123) is a new type of refrigerant. During its production process, a certain amount of difluorotrichloroethane (HCFC-122) will be produced as a by-product. After product distillation and purification, it can be obtained HCFC-122 by-products with a purity greater than 95%. At present, the by-products of HCFC-122 are mainly disposed of by incineration, which is a waste from the perspective of resource utilization. [0004] 1-Chloro-2,2-difluoroethylene is an important fluorine fine chemical raw material and a key intermediate in the production of fluorine-containing finishing agents, fluorine-containing surfactants and other fluorine-containing fine chemicals. It can be used in heat ex...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C21/18C07C17/23C01G9/04
Inventor 付庆向绍基姚汉清刘建鹏孔小林
Owner SINOCHEM LANTIAN
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