Method for preparing difluoroacetyl fluoride

A technology of difluoroacetyl fluoride and tetrafluoroethane, applied in the field of preparation of difluoroacetyl fluoride, can solve the problems of difficult process, constant change of hydrogen fluoride flow, long fluorination treatment time and the like

Active Publication Date: 2018-04-03
SINOCHEM MODERN ENVIRONMENTAL CHEM INDAL XI ANCO +1
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  • Abstract
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  • Application Information

AI Technical Summary

Problems solved by technology

Although when using this γ-alumina catalyst after HF fluorination treatment, the conversion rate reaches more than 99%, and the selectivity is greater than 95%, but the fluorination treatment time of this catalyst is too long and the hydrogen fluoride flow rate constantly changes in the fluorination treatment process. The whole p

Method used

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  • Method for preparing difluoroacetyl fluoride
  • Method for preparing difluoroacetyl fluoride

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Embodiment 1: the preparation of aluminum fluoride catalyst

[0032] Take 81.7g Al(i-PrO) 3 Dissolve in 500ml of isopropanol and stir to form an aluminum solution. At room temperature, dissolve 24.0 g of anhydrous HF in HF-Et 2 O solution (12.5mol / L) was added to the above aluminum solution (Al:HF molar ratio was 1:3), stirred vigorously, stopped stirring after 4 hours of reaction, and left to age for 4 hours. Use a rotary evaporator or a centrifuge to remove the volatile components in the product, and dry them in a vacuum oven to obtain a high specific surface area aluminum fluoride precursor, denoted as AlF 3 -1 Pre.

[0033] Take 10ml of the formed aluminum fluoride precursor and place it in a tubular reactor, firstly in N 2 Under the atmosphere, the temperature was raised to 150° C. at an arbitrary rate and kept for 2 hours. In 20% R22 (difluorochloromethane) / 80% N 2 In the atmosphere, the temperature was raised to 200°C at a rate of 1°C / min, and kept for 1 ...

Embodiment 2

[0035] Embodiment 2: the preparation of aluminum fluoride catalyst

[0036] Using the same experimental steps as in Example 1, the Al:HF molar ratio was changed to 1:2.5, and the prepared precursor and aluminum fluoride were respectively marked as AlF 3 -2Pre, AlF 3 -R22-2 and AlF 3 -HF-2.

Embodiment 3

[0037] Embodiment 3: the preparation of aluminum fluoride catalyst

[0038] Using the same experimental steps as in Example 1, the Al:HF molar ratio was changed to 1:2.0, and the prepared precursor and aluminum fluoride were respectively marked as AlF 3 -3Pre, AlF 3 -R22-3 and AlF 3 -HF-3.

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Abstract

The invention discloses a method for preparing difluoroacetyl fluoride from 1-C1-C8-alkoxy-1,1,2,2-tetrafluoroethane as a raw material by gas-phase catalytic cracking reaction in the presence of an aluminum fluoride catalyst. According to the disclosed preparation method, the reaction route is concise and efficient, fewer by-products are generated, catalytic activity is high, catalyst stability ishigh, and industrial production is facilitated.

Description

technical field [0001] The invention relates to a preparation method of halogenated acid halides, in particular to a preparation method of difluoroacetyl fluoride. Background technique [0002] Alkyl difluoroacetate is a kind of widely used chemical and pharmaceutical intermediates, and its common preparation method is to react difluoroacetyl fluoride with alcohol. For the preparation method of difluoroacetyl fluoride, in the prior art, alkoxytetrafluoroethane is usually obtained by reacting tetrafluoroethylene with alcohol, and then the alkoxytetrafluoroethane is cracked to generate difluoroacetyl fluoride. In the process of cracking alkoxytetrafluoroethane to generate difluoroacetyl fluoride, it is very important to find a suitable catalyst. For catalysts, the prior art has made the following efforts: [0003] Chinese patent CN102218304A discloses a method of using 1,1,2,2-tetrafluoroethyl alkyl ether as a raw material for catalytic cracking to obtain the target product ...

Claims

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Application Information

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IPC IPC(8): C07C55/40B01J27/12B01J35/10C07C51/58
CPCC07C51/58B01J27/12B01J35/1019C07C55/40
Inventor 杨洋刘坤峰许磊曾昌华田保华杨会娥
Owner SINOCHEM MODERN ENVIRONMENTAL CHEM INDAL XI ANCO
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