A kind of method for continuously preparing trifluoroacetic acid by hydrolysis of trifluoroacetyl chloride

A technology of trifluoroacetyl chloride and trifluoroacetic acid, applied in the directions of acid halide preparation, organic chemistry, etc., can solve problems such as low hydrolysis and absorption efficiency of trifluoroacetyl chloride, and achieve the advantages of improving mixing efficiency, short reaction time and improving conversion rate. Effect

Active Publication Date: 2022-06-17
中化蓝天氟材料有限公司 +2
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  • Abstract
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AI Technical Summary

Problems solved by technology

[0010] In order to solve the problem of low hydrolysis and absorption efficiency of trifluoroacetyl chloride in the process of preparing trifluoroacetic acid by the hydrolysis reaction of trifluoroacetyl chloride and water, the present invention provides a method capable of improving the mixing efficiency of trifluoroacetyl chloride and water to improve The hydrolysis absorption efficiency of trifluoroacetyl chloride makes it have the characteristics of high conversion rate of raw materials, short reaction time, safe and controllable reaction and suitable for industrial scale-up

Method used

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  • A kind of method for continuously preparing trifluoroacetic acid by hydrolysis of trifluoroacetyl chloride
  • A kind of method for continuously preparing trifluoroacetic acid by hydrolysis of trifluoroacetyl chloride
  • A kind of method for continuously preparing trifluoroacetic acid by hydrolysis of trifluoroacetyl chloride

Examples

Experimental program
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Effect test

Embodiment 1

[0037] optional figure 2 1 piece of corning straight channel module (as premix preheating module 3), 6 pieces of corning "heart-shaped" microchannel reaction module, 1 piece of corning straight channel module (as quenching module 10). According to the attached image 3 The reaction scheme shown constitutes a continuous flow microchannel reaction system. The reaction heat exchange medium adopts heat conduction oil. According to the principle of forced heat transfer in the microchannel reactor, only two temperature measurement points are set at the inlet and outlet of the reactor. Before the reaction, the microchannel reaction system and the connecting pipeline were dewatered and dried respectively, and the air tightness of 1.0 MPa was checked. by attaching image 3 A liquid phase pump (such as a diaphragm metering pump) in the microchannel reaction system continuously and stably adds raw water to the microchannel reaction system. by attaching image 3 2 gas mass flow meters...

Embodiment 2

[0041] The same Corning microchannel reactor was used as in Example 1, and the same connection method and control method were used. This example changes the reaction conditions.

[0042] The heat exchanger temperature was set at 70°C, that is, the reaction temperature, and the reaction pressure was set at 0.1 MPa. The feed rate of raw material water is 2.25g / min, the feed rate of trifluoroacetyl chloride gas is 3.31g / min, the residence time of the reaction is 8s, and the molar ratio of water and trifluoroacetyl chloride is 5:1. The reaction raw materials enter the "heart-shaped" micro-channel reaction module 4 through the micro-channel premixing preheating module 3, and the trifluoroacetyl chloride gas directly enters the "heart-shaped" micro-channel reaction module 4 through the gas mass flowmeter. In microchannel reaction modules 4-9, trifluoroacetyl chloride reacts with water. The crude reaction product was collected by quenching module 10 to obtain crude trifluoroacetic ac...

Embodiment 3

[0045] The same Corning microchannel reactor was used as in Example 1, and the same connection method and control method were used. This example changes the reaction conditions.

[0046] The heat exchanger temperature was set to 50°C, that is, the reaction temperature, and the reaction pressure was set to 0MPa. The feed rate of raw material water is 3.60g / min, the feed rate of trifluoroacetyl chloride gas is 5.30g / min, the residence time of the reaction is 10s, and the molar ratio of water and trifluoroacetyl chloride is 5:1. The reaction raw materials enter the "heart-shaped" micro-channel reaction module 4 through the micro-channel premixing preheating module 3, and the trifluoroacetyl chloride gas directly enters the "heart-shaped" micro-channel reaction module 4 through the gas mass flowmeter. In microchannel reaction modules 4-9, trifluoroacetyl chloride reacts with water. The crude reaction product was collected by quenching module 10 to obtain crude trifluoroacetic ac...

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Abstract

The invention discloses a method for preparing trifluoroacetic acid by hydrolyzing trifluoroacetyl chloride. In a microchannel reactor, raw materials trifluoroacetyl chloride and water are mixed and reacted in a reaction module, and trifluoroacetic acid is obtained after quenching the module. acetic acid. The method provided by the invention is easy to operate, short in reaction time, safe and controllable in reaction and suitable for industrial scale-up.

Description

technical field [0001] The invention relates to a preparation method of trifluoroacetic acid, in particular to a method for preparing trifluoroacetic acid by hydrolysis of trifluoroacetyl chloride. Background technique [0002] Trifluoroacetic acid is a highly acidic organic acid, which can dissolve many inorganic and organic substances, making it widely used in medicine, pesticides, dyes, amino acid protection, organic synthesis, material processing and other fields. Trifluoroacetic acid is also a very useful intermediate for fluorine-containing medicines, pesticides and dyes. The introduction of trifluoromethyl groups into medicines, pesticides and dyes can show excellent activity and has been used in heterocyclic herbicides. has been widely used. [0003] For the preparation method of trifluoroacetic acid, there are following reports in the prior art: [0004] (1) US4022824 discloses the method for preparing trifluoroacetic acid by electrolytic fluorination of acetyl fl...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C53/18C07C51/04
CPCC07C51/04C07C53/18
Inventor 肖恒侨徐卫国章祺李华蒋强
Owner 中化蓝天氟材料有限公司
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