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Preparation method of fluorobromoethylene

A technology of difluoroethylene and difluoroethane, applied in the fields of dehydrohalogenation preparation, organic chemistry, etc., can solve the problems of difficult acquisition of raw materials, high cost, and difficult industrial scale implementation, and achieve high yield effect

Inactive Publication Date: 2013-01-16
SHANGHAI 3F NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] (i) The raw materials used are difficult to obtain and the cost is relatively high;
[0006] (ii) It will generate a large amount of zinc bromide industrial waste, which is difficult to implement on an industrial scale

Method used

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  • Preparation method of fluorobromoethylene
  • Preparation method of fluorobromoethylene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] 1. Preparation of 1,2-dibromo-1,1-difluoroethane

[0057] Add 10kg of bromine into a 10L reactor, heat it to 40°C, slowly feed 4.3kg of vinylidene fluoride, react for a total of 6 hours, and the reaction pressure is 0.3MPa. After the reaction, the excess vinylidene fluoride is collected in the recovery tank and separated It can be reused, and 14.09kg of the product 1,2-dibromo-1,1-difluoroethane was obtained from the reactor. The purity was 85.2% and the molar yield was 85.8% according to GC chromatography analysis.

[0058] After testing, the boiling point of the obtained product: 92.1°C / 760mmHg; mass spectrum MS molecular weight = 223.8; nuclear magnetic resonance NMR H 1 , chemical shift δ4.1; NMR F 19 , chemical shift δ-50.2.

[0059] 2. Preparation of 1-bromo-2,2-difluoroethylene

[0060] In 0.5m with -35℃ brine 2 Add 2kg of potassium hydroxide and 3kg of water into the 10L reaction kettle of the condenser with condensation area, heat to 60°C, and slowly feed 5...

Embodiment 2

[0063] 1. Preparation of 1,2-dibromo-1,1-difluoroethane

[0064] Add 10kg of bromine into a 10L reactor, heat it to 70°C, slowly feed 4.2kg of vinylidene fluoride, react for a total of 3 hours, and the reaction pressure is 0.2MPa. It can be reused, and 14.02kg of the product 1,2-dibromo-1,1-difluoroethane was obtained from the reaction kettle. After analysis, the purity was 86.5%, and the molar yield was 86.6%.

[0065] 2. Preparation of 1-bromo-2,2-difluoroethylene

[0066] In 0.5m with -35℃ brine 2 The 10L reactor of the condenser with the condensing area is transformed into a packed tower pipeline with a theoretical plate number of 20 in the pipeline from the rising steam to the condenser. Add 2kg of potassium hydroxide and 4kg of water to the reactor, heat it to 60°C, and slowly pass it into 5.5 kg of the above 96.5% purity 1,2-dibromo-1,1-difluoroethane was reacted for 5 hours in total, and 3.42 kg of the product was collected during the reaction, with a purity of 92.7%...

Embodiment 3

[0068] 1. Preparation of 1,2-dibromo-1,1-difluoroethane

[0069] Add 10kg of bromine into a 10L reactor, heat it to 60°C, slowly feed 4.3kg of vinylidene fluoride, react for a total of 4 hours, and the reaction pressure is 0.4MPa. It can be reused. A total of 14.03kg of the product 1,2-dibromo-1,1-difluoroethane was obtained from the reactor. The purity was 87.3% after analysis, and the molar yield was 87.5%.

[0070] 2. Preparation of 1-bromo-2,2-difluoroethylene

[0071] In 0.5m with -35℃ brine 2 The 10L reactor of the condenser with the condensing area is transformed into a packed tower pipeline with a theoretical plate number of 20 in the pipeline from the rising steam to the condenser. Add 2kg of potassium hydroxide, 3kg of water, and 0.5kg of ethanol to the reactor, and heat it to 60°C , 5.5kg of 1,2-dibromo-1,1-difluoroethane with a purity of 97% was slowly introduced, and the reaction lasted for 4 hours. During the reaction, 3.37kg of product was collected, with a pu...

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Abstract

The invention provides a method for a novel process route of 1-bromo-2,2-difluoroethylene. The method comprises the following steps of (i) preparing 1,2-dibromo-1,1-difluoroethane (CF2Br-CH2Br) with high selectivity by employing a catalytic addition reaction of 1,1-difluoroethylene (CF2=CH2); and (ii) adding 100-350 mol% of an alkaline water solution according to a molar weight of 1,2-dibromo-1,1-difluoroethane, performing selective dehydrobromination reaction on the 1,2-dibromo-1,1-difluoroethane and the alkaline water solution at a temperature of 30-150 DEG C by using a professionally designed reaction refinery system to obtain 1-bromo-2,2-difluoroethylene.

Description

technical field [0001] The present invention relates to an important bromine-containing fluoroethylene compound -- 1-bromo-2,2-difluoroethylene (CF 2 =CHBr) preparation method, the reaction process route of the method of the present invention can obtain high yield, is a kind of green process method, is suitable for industrialized production. Background technique [0002] 1-Bromo-2,2-difluoroethylene is an important intermediate of fluorine-containing compounds and the third monomer of fluorine-containing polymers. It can be used as an intermediate of various fluorine-containing fine chemicals for the synthesis of fluorine-containing medicines ; It can be used as the third monomer of fluoropolymers to improve the vulcanization method and performance of fluoroelastomers, improve the melt processing performance of fluoropolymers and produce special properties. [0003] The prior art proposes many methods for the preparation of 1-bromo-2,2-difluoroethylene. For example, Davis ...

Claims

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Application Information

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IPC IPC(8): C07C21/18C07C17/25
Inventor 陈焱锋李作铭张智勇吴君毅
Owner SHANGHAI 3F NEW MATERIAL
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