Preparation method of difluoroacetic acid

A technology of difluoroacetic acid and difluoroethane, which is applied in the field of preparation of difluoroacetic acid, can solve the problems of flammability of tetrafluoroethylene, long reaction time, and reduced reaction feeding load, so as to reduce raw material consumption, short process, and reduce The effect of energy consumption

Active Publication Date: 2019-03-29
SHANDONG HUAAN NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has the disadvantage that the raw material tetrafluoroethylene is flammable. In order to prevent the combustion of tetrafluoroethylene during the reaction, an inert gas needs to be introduced for dilution, which reduces the reaction feeding load, and the reaction time is also longer.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) 200g catalyst is put into the reactor, feed nitrogen to replace the air in the reactor;

[0028] (2) Heating the reactor to 120°C with a heating rate of 2°C / min;

[0029] (3) Continue to feed nitrogen into the reactor, so that the pressure in the reactor is raised to 0.4MPa;

[0030] (4) Pass hydrogen peroxide at a flow rate of 50ml / h and 2-chloro-1,1-difluoroethane at a flow rate of 18ml / h into the reaction kettle with a constant pressure pump for a contact reaction, and the contact time is 15s;

[0031] (5) Perform rectification operation on the reaction product to obtain difluoroacetic acid.

Embodiment 2

[0033] (1) 200g catalyst is put into the reactor, feed nitrogen to replace the air in the reactor;

[0034] (2) Heating the reactor to 130°C with a heating rate of 2°C / min;

[0035] (3) Continue to feed nitrogen into the reactor, so that the pressure in the reactor is raised to 0.8MPa;

[0036] (4) Pass hydrogen peroxide at a flow rate of 100ml / h and 2-chloro-1,1-difluoroethane at a flow rate of 18ml / h into the reaction kettle with a constant pressure pump for a contact reaction, and the contact time is 15s;

[0037] (5) Perform rectification operation on the reaction product to obtain difluoroacetic acid.

Embodiment 3

[0039] (1) 200g catalyst is put into the reactor, feed nitrogen to replace the air in the reactor;

[0040] (2) Heating the reactor to 140°C with a heating rate of 2°C / min;

[0041] (3) Continue to feed nitrogen into the reactor, so that the pressure in the reactor is raised to 0.8MPa;

[0042] (4) Pass hydrogen peroxide at a flow rate of 300ml / h and 2-chloro-1,1-difluoroethane at a flow rate of 50ml / h into the reaction kettle with a constant pressure pump for contact reaction, and the contact time is 20s;

[0043] (5) Perform rectification operation on the reaction product to obtain difluoroacetic acid.

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Abstract

The invention relates to a preparation method of difluoroacetic acid, and belongs to the technical field of fluorine chemical engineering. According to the preparation method of the difluoroacetic acid, KMnO4 / C solid catalysts are added into a fixed bed reaction kettle; nitrogen gas is introduced to perform replacement on the air in the reaction kettle; the temperature is raised to a fixed temperature; then, hydrogen peroxide and 2-chlorine-1,1-difluoroethane are introduced by a voltage stabilizing pump to perform contact reaction; after a product is separated, the product of difluoroacetic acid is finally obtained. The preparation method of the difluoroacetic acid has the advantages that the process is simple; the flow process is short; the technical flow process is simplified; the energyconsumption is greatly reduced; the method is suitable for industrialized production; the used raw materials are all common reagents, the resources of the materials are wide, and the price is low; the reaction process can be easily controlled; the obtained difluoroacetic acid product has high yield and has wide application and popularization values.

Description

technical field [0001] The invention relates to a preparation method of difluoroacetic acid, which belongs to the technical field of fluorine chemical industry. Background technique [0002] Difluoroacetic Acid (Difluoroacetic Acid), C 2 h 2 f 2 o 2 , Molecular formula 96.03, colorless to light yellow liquid, is a fluorine-containing derivative of acetic acid, as a fine intermediate, mainly used for the synthesis of fluorine-containing medicines, pesticides and dyes, and can also be used as a raw material for glass coating process; it is an esterification reaction Catalyst for and condensation reaction, protective agent for hydroxyl and amino groups, used in the synthesis of sugars and polypeptides; it is a good solvent for many organic compounds and an excellent solvent for organic reactions, and has a good market prospect. [0003] There are safety problems in the preparation method of difluoroacetic acid in the prior art. For example, Japanese Patent JP06228043 discl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C53/18C07C51/285
CPCC07C51/285C07C53/18
Inventor 王瑞英徐甲超孟翔田勇王永千王欢
Owner SHANDONG HUAAN NEW MATERIAL
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