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Preparation method of 2-bromo-1,1-difluoroethylene

A technology of vinylidene fluoride and vinylidene fluoride, which is applied in the field of preparation of 2-bromo-1,1-difluoroethylene, can solve the problems of strong corrosion of bromine and high requirements for equipment materials, achieve high purity, simple method, Post-processing simple effects

Active Publication Date: 2019-02-22
湖南有色郴州氟化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The bromine used in this process is highly corrosive and requires high equipment materials

Method used

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  • Preparation method of 2-bromo-1,1-difluoroethylene
  • Preparation method of 2-bromo-1,1-difluoroethylene

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[0020] The invention provides a preparation method of 2-bromo-1,1-difluoroethylene, comprising the following steps:

[0021] Under the copper catalyst, react N-bromosuccinimide and vinylidene fluoride in the presence of base and organic solvent to obtain 2-bromo-1,1-difluoroethylene.

[0022] The invention adopts N-bromosuccinimide and vinylidene fluoride as reaction raw materials to prepare 2-bromo-1,1-difluoroethylene, the method is simple, the post-treatment is simple and no waste water is required, and the by-products are directly recovered by suction filtration, which is environmentally friendly. Friendly, and the purity of the prepared product is high. The raw material vinylidene fluoride used is an industrial product, which is cheap and easy to obtain.

[0023] In the present invention, the vinylidene fluoride has the structure of formula I:

[0024]

Embodiment 1

[0039] Put 8.6g of cuprous bromide, 256.3g of NBS, 10.9g of cesium fluoride and 500ml of carbon tetrachloride into the 2L stainless steel reaction kettle in sequence, cool down to the internal temperature of 0°C, fill with vinylidene fluoride to 1.8MPa, and keep the temperature until pressure drops to zero;

[0040] The reaction liquid in the kettle is released, and the product 2-bromo-1,1-difluoroethylene is collected by low-temperature rectification, with a purity of more than 99.5%.

[0041] 105.2 g of cuprous bromide and succinimide were recovered by filtration of the rectification raffinate.

[0042] figure 1 The H NMR spectrum of 2-bromo-1,1-difluoroethylene prepared in Example 1 of the present invention;

[0043] figure 2 The H NMR spectrum of 2-bromo-1,1-difluoroethylene prepared by the preparation method provided in Example 1 of the present invention; image 3 The carbon nuclear magnetic resonance spectrum of 2-bromo-1,1-difluoroethylene prepared by the preparati...

Embodiment 2

[0045] Put 5.2g of cuprous bromide, 320.4g of NBS, 23.4g of cesium carbonate and 500ml of carbon tetrachloride into the 2L stainless steel reaction kettle in sequence, cool down to the internal temperature of 0°C, fill with vinylidene fluoride to 1.8MPa, keep warm and react to pressure down to zero;

[0046] The reaction liquid in the kettle was discharged, and the product 2-bromo-1,1-difluoroethylene was collected by low-temperature rectification, 121.3g, with a yield of 70.7% and a purity of more than 99.5%;

[0047] The rectification raffinate was suction-filtered, and 110.7 g of cuprous bromide and succinimide were recovered.

[0048] As can be seen from the above examples, the present invention provides a preparation method of 2-bromo-1,1-difluoroethylene, comprising the following steps: under a copper catalyst, N-bromosuccinimide and vinylidene fluoride are In the presence of a base and an organic solvent, react to obtain 2-bromo-1,1-difluoroethylene. The invention ado...

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Abstract

The invention provides a preparation method of 2-bromo-1,1-difluoroethylene. The preparation method comprises the following step: under a copper catalyst, taking N-bromosuccinimide and vinylidene fluoride to react in the presence of alkali and an organic solvent to obtain the 2-bromo-1,1-difluoroethylene. According to the preparation method, the N-bromosuccinimide and the vinylidene fluoride are used as raw materials of the reaction to prepare the 2-bromo-1,1-difluoroethylene; the method is simple, post-treatment is simple and no wastewater is produced; byproducts are directly filtered and recycled so that the preparation method is environmentally friendly; the purity of a prepared product is relatively high. The raw material vinylidene fluoride is an industrial product and is cheap and easy to obtain. An experiment result shows that the purity of the 2-bromo-1,1-difluoroethylene prepared by the method is 99.5 percent or more.

Description

technical field [0001] The invention belongs to the technical field of organic fluorine fine chemicals, and in particular relates to a preparation method of 2-bromo-1,1-difluoroethylene. Background technique [0002] 2-Bromo-1,1-difluoroethylene is an important fluorochemical intermediate and fluoropolymer monomer. As an intermediate of fluorine-containing compounds, it is mainly used in the manufacture of fine chemicals such as fluorine-containing medicines and fluorine-containing pesticides; as a monomer of fluorine-containing polymers, it is mainly used in the manufacture of fluorine-containing polymer materials, which can effectively improve fluoroelastomers The vulcanization method and performance can be improved to improve the melt processability and other special properties of fluoropolymers. [0003] The existing 2-bromo-1,1-difluoroethylene, its preparation process is mainly through the addition of vinylidene fluoride and bromine to obtain 1,1-difluoro-2,2-dibromoe...

Claims

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Application Information

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IPC IPC(8): C07C17/10C07C21/18
CPCC07C17/10C07C21/18
Inventor 王刚彭智敏李军刘斌李志鹏苏万里石芙蓉张振华
Owner 湖南有色郴州氟化学有限公司
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