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Continuous preparation method of trifluoroacetyl fluoride

A technology of trifluoroacetyl fluoride and trifluoroethyl fluoride, which is applied in the field of continuous preparation of trifluoroacetyl fluoride, can solve the problems of high equipment cost, unfavorable industrial implementation, high cost of electrolytic plate production, low electrolytic efficiency and product purity, and achieves Avoid recycling and waste liquid pollution, easy large-scale industrial production, and high product yield

Active Publication Date: 2021-03-16
天津长芦新材料研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In US5672748 trifluoroacetyl chloride is substituted for trifluoroacetyl fluoride, hydrofluoric acid is required, and the device is complicated; in US2717871, the electrolytic synthesis method has relatively cheap raw materials, but the electrolytic efficiency is very low, and it is difficult to avoid the low purity of the product caused by electrolytic impurities. The cost of board manufacturing is expensive, and the high cost of equipment is not conducive to industrial implementation

Method used

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  • Continuous preparation method of trifluoroacetyl fluoride
  • Continuous preparation method of trifluoroacetyl fluoride

Examples

Experimental program
Comparison scheme
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Embodiment 1

[0020] Example 1: Anhydrous hydrogen fluoride vaporization chamber temperature 25°C, trifluoroacetic acid vaporization chamber temperature 75°C, fluorinating reagent ClCHFCF 2 N(C 2 h 5 ) 2 The temperature of the gasification chamber is 40°C. After gasification of anhydrous hydrogen fluoride, trifluoroacetic acid, and fluorinated reagents, they enter the mixed gas transition chamber through the gas quality controller at the ratio of gas to substance: 1:1:1, and the resulting mixed gas is produced by Slowly pass through the catalyst packing column from bottom to top, the column temperature is 80°C; the packing column is equipped with a high-activity catalyst, wherein the high-activity catalyst is a supported catalyst that uses activated carbon as a carrier and contains catalyst active components; the catalyst active component For three (pentafluorophenyl) borane. The gas obtained from the outlet at the upper end of the catalyst packed column passes through the first cold tra...

Embodiment 2

[0024] Example 2: Anhydrous hydrogen fluoride vaporization chamber temperature 25°C, trifluoroacetic acid vaporization chamber temperature 75°C, fluorinating reagent ClCHFCF 2 N(C 2 h 5 ) 2 The temperature of the gasification chamber is 40°C. After gasification of anhydrous hydrogen fluoride, trifluoroacetic acid, and fluorinated reagents, they enter the mixed gas transition chamber through the gas quality controller at the ratio of gas to substance: 1:1:1, and the resulting mixed gas is produced by Slowly pass through the catalyst packing column from bottom to top, the column temperature is 80°C; the packing column is equipped with a high-activity catalyst, wherein the high-activity catalyst is a supported catalyst that uses activated carbon as a carrier and contains catalyst active components; the catalyst active component For three [3,5-bis (trifluoromethyl) phenyl] borane. The gas obtained from the outlet at the upper end of the catalyst packed column passes through the...

Embodiment 3

[0025] Example 3: Anhydrous hydrogen fluoride vaporization chamber temperature 25°C, trifluoroacetic acid vaporization chamber temperature 75°C, fluorinating reagent ClCHFCF 2 N(C 2 h 5 ) 2 The temperature of the gasification chamber is 40°C. After gasification of anhydrous hydrogen fluoride, trifluoroacetic acid, and fluorinated reagents, they enter the mixed gas transition chamber through the gas quality controller at the ratio of gas to substance: 1:1:1, and the resulting mixed gas is produced by Slowly pass through the catalyst packing column from bottom to top, the column temperature is 80°C; the packing column is equipped with a high-activity catalyst, wherein the high-activity catalyst is a supported catalyst that uses activated carbon as a carrier and contains catalyst active components; the catalyst active component for alumina. The gas obtained from the outlet at the upper end of the catalyst packed column passes through the first cold trap to remove trifluoroacet...

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Abstract

The invention belongs to the field of fluorine chemical industry, and particularly relates to a continuous preparation method of trifluoroacetyl fluoride, which comprises the following steps: 1) gasifying a trifluoroethyl compound and a fluorination reagent, mixing with anhydrous hydrogen fluoride, and introducing into a packed column filled with a high-activity catalyst to perform gas-phase reaction; and 2) cooling and rectifying the gas obtained after the reaction to obtain trifluoroacetyl fluoride with the purity of greater than 99.9%. Wherein the high-activity catalyst is a supported catalyst which takes activated carbon as a carrier and contains catalyst active ingredients; wherein the active component of the catalyst is one of tris(pentafluorophenyl) borane or tris [3,5-bis (trifluoromethyl) phenyl] borane. The preparation method has the advantages that the gas-phase reaction is carried out firstly, the recovery treatment of the solvent and the waste liquid pollution are avoided,the high-value chemical intermediate trifluoroacetyl fluoride is generated under the action of the catalyst, the product yield is high, the reaction conditions are mild, meanwhile, the continuous reaction is realized, the reaction process is simple to operate, and the efficiency is high.

Description

technical field [0001] The invention belongs to the field of fluorine chemical industry, and in particular relates to a continuous preparation method of trifluoroacetyl fluoride. Background technique [0002] Perfluoroacetyl fluoride, also known as trifluoroacetyl fluoride, molecular formula: CF3COF, boiling point: -59°C, is a colorless gas at room temperature, is a kind of compound containing -COF functional group, not easy to store and transport; has high activity, easy to mix with alcohol An esterification reaction occurs, and HF gas and perfluoropropionic acid are generated when it meets water. It can be seen that it is used to prepare various compounds. [0003] Perfluoroacetyl fluoride, as an intermediate for the chemical synthesis of perfluoroalkyl compounds, is an important compound that has attracted much attention as a necessary polymer monomer for the preparation of high-purity fluoropolymers. Its derivatives are widely used in various fields. At present, the pre...

Claims

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Application Information

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IPC IPC(8): C07C53/48C07C51/60C07C51/64
CPCC07C51/60C07C51/64C07C53/48
Inventor 汤峤永姚素梅肖鑫高国红
Owner 天津长芦新材料研究院有限公司
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