Preparation method of 2-bromo-2,2-difluoroacetyl chloride and 2-bromo-2,2-difluoro acetate and recycling method of waste difluoro trichloroethane

A technology of difluorotrichloroethane and difluorodichlorodibromoethane, which is applied in the field of preparation of fluorine-containing organic intermediates, can solve the problems of post-processing difficulties, difficulties, and many amplification problems, so as to reduce environmental pollution and Hazards to the health of operators, the effect of realizing recycling and reducing production costs

Inactive Publication Date: 2015-07-08
JIANGXI SUNWAY CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is a feasible synthetic route, but there are selectivity problems: there are by-products of bromodichloroacetate and its derivatives, and there are also difluorodichlorodibromoethane raw materials that are not easy to obtain, and oxygen oxidation engineering is used Amplification has many problems, and it is not easy to achieve industrialized mass production
[0033] The inventor found in the course of the experiment that using mercury salt as a catalyst and using the same amount of sulfur trioxide, even if the reaction exceeds 72 hours, difluorodichlorodibromoethane cannot be completely converted into 2-bromo-2,2-dibromoethane. Fluoroacetyl chloride requ

Method used

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  • Preparation method of 2-bromo-2,2-difluoroacetyl chloride and 2-bromo-2,2-difluoro acetate and recycling method of waste difluoro trichloroethane
  • Preparation method of 2-bromo-2,2-difluoroacetyl chloride and 2-bromo-2,2-difluoro acetate and recycling method of waste difluoro trichloroethane
  • Preparation method of 2-bromo-2,2-difluoroacetyl chloride and 2-bromo-2,2-difluoro acetate and recycling method of waste difluoro trichloroethane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 2

[0078] Install a 5-liter three-neck flask with a reflux condenser, a mechanical stirring device, and a constant pressure dropping funnel. During the reaction, control the temperature of the cooling water in the reflux condenser at 0 to 30°C, and add waste difluorotrifluorotrifluoride to the constant pressure dropping funnel. Ethyl chloride (R122, content 90.3%) 1872 grams, add 1500 grams of dehydrated alcohol in reaction flask, 467 grams of potassium hydroxide, heating and dissolving, be mixed with the potassium hydroxide solution of ethanol, adopt oil bath heating reaction flask, adopt The electronic temperature controller controls the reaction temperature to 80±5°C, and R122 is added dropwise under stirring, and the drop is completed in about 7 hours, and then the reaction is kept for 2 hours. Add 450 milliliters of solvent dichloromethane and 1373 grams (440 milliliters) of bromine into the second 5-liter three-necked flask equipped with a reflux condenser and a mechanical s...

Embodiment 12

[0103] Example 12 (purification of 2-bromo-2,2-difluoroacetyl chloride by rectification)

[0104] Install a rectification column, a fractionating head with an adjustable reflux ratio-reflux condenser, and a 2-liter three-neck flask (rectification kettle) with magnetic stirring, add 3012 grams of crude 2-bromo-2,2-difluoroacetyl chloride, During rectification, control the circulation temperature of the cooling water in the reflux condenser to be between 0 and 10°C, connect the receiving bottle of the product, use an oil bath to heat the reaction bottle, and use an electronic temperature controller to control the temperature of the oil bath to 75 to 80°C. The distillate between 49-51 ℃ was collected by adjusting the reflux ratio to obtain 2620 grams, the rectification yield was 87%, and the gas chromatography content of the pure product was 99.6%.

Embodiment 13

[0105] Example 13 (preparation of 2-bromo-2,2-difluoroacetic acid)

[0106] Install a 3-liter three-necked flask with a reflux condenser, a mechanical stirring device, and a constant pressure dropping funnel. During the reaction, control the circulating temperature of the cooling water in the reflux condenser between 0 and 10°C, and connect the tail gas absorption device. Use sodium hydroxide aqueous solution to absorb the tail gas of the reaction, add 330 grams of water to the reaction bottle, control the reaction temperature between 0 and 20 °C, add 2901 grams of 2-bromo-2,2-difluoroacetyl chloride dropwise in 10 hours, drop After adding and keeping warm for 2 hours, change the experimental device into a rectifying device, install a rectifying column, a fractionating head-reflux condenser, and a magnetic stirring device that can adjust the reflux ratio on a 3-liter there-necked flask, and use an oil bath to heat the reaction bottle. The temperature of the oil bath is control...

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Abstract

The invention relates to a preparation method of 2-bromo-2,2-difluoroacetyl chloride and 2-bromo-2,2-difluoro acetate and a recycling method of waste difluoro trichloroethane. The preparation method comprises the following steps: with waste difluoro trichloroethane produced in the production process of dichlorotrifluoroethane as a raw material, carrying out dehydrochlorination to obtain difluoro dichloroethylene, carrying out addition reaction on difluoro dichloroethylene and bromine to obtain difluoro dichlone dibromoethane; reacting difluoro dichlone dibromoethane with sulfur trioxide to obtain 2-bromo-2,2-difluoroacetyl chloride; and reacting 2-bromo-2,2-difluoroacetyl chloride with alcohol or phenol to obtain 2-bromo-2,2-difluoro acetate series products. According to the preparation method and the recycling method, recycling of waste difluoro trichloroethane is realized; 2-bromo-2,2-difluoroacetyl chloride and 2-bromo-2,2-difluoro acetate are prepared by a temperature oscillation method, so that the production cost is reduced; and meanwhile, the preparation method is an environment-friendly technique for producing products.

Description

technical field [0001] The invention belongs to the technical field of preparation of fluorine-containing organic intermediates, and relates to a preparation method and waste of 2-bromo-2,2-difluoroacetyl chloride, 2-bromo-2,2-difluoroacetic acid and ester series compounds Recovery and treatment of difluorotrichloroethane. Background technique [0002] The problem of environmental protection in the chemical production process has always been a topic that chemical technicians need to continuously study and improve. If the waste generated in the chemical production process is discharged directly, it will seriously pollute the environment. [0003] In order to solve this problem, on the one hand, through the continuous improvement of the chemical reaction process route, the use of green and environmentally friendly production technology can reduce or even eliminate the generation and discharge of pollutants in the chemical production process. Another way is to collect the poll...

Claims

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Application Information

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IPC IPC(8): C07C53/48C07C51/58C07C51/64C07C69/63C07C67/08C07C67/54C07C53/18C07C51/04B09B3/00
CPCB09B3/00C07C17/04C07C17/25C07C51/04C07C51/58C07C51/64C07C53/48C07C67/08C07C67/14C07C67/54C07C69/63C07C21/18C07C19/14C07C53/18
Inventor 康茹茹赵艳格严妍向绍基朱兆江徐永进石华兴李凤娇
Owner JIANGXI SUNWAY CHEM CO LTD
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