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Preparation method of 2,2-difluoro-1,3-propanediol

A technology of difluoropropanol and propylene glycol, which is applied in the field of preparation of 2,2-difluoro-1,3-propanediol, can solve the problems of high synthesis cost, limited practical application, and difficulty in obtaining raw materials, and achieves good stability, Simple equipment requirements and easy availability of raw materials

Active Publication Date: 2017-11-28
山东飞源新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] 2,2-difluoro-1,3-propanediol, with a boiling point of 250.9°C and a density of 1.334g / ml, can be used in the synthesis of various drugs, new polyester PTT, pharmaceutical intermediates and new antioxidants, and can be used in fluorine-containing materials , fluorine-containing medicines, and pesticides have unknown application potentials, but due to the high cost of synthesis and the difficulty of obtaining raw materials, their practical application is still relatively limited

Method used

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  • Preparation method of 2,2-difluoro-1,3-propanediol

Examples

Experimental program
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Effect test

Embodiment 1

[0024] 1.1 Preparation of 2-chloro-1,1-difluoroethylene

[0025] Add 1200g of 30% sodium hydroxide aqueous solution and 2.5g of tetrabutylammonium bromide into a 2000ml three-necked flask, and add 500g of 1,2-dichloro-1,1-difluoroethane while stirring with a dropping funnel, React at 30°C for 6h, then pass the gas through the condenser tube into the collection bottle of carbon tetrachloride, and the collection bottle is cooled to minus 20°C by dry ice. The weight of the collection bottle increased by about 300g; the purity of the reaction gas 2-chloro-1,1-difluoroethylene detected by gas chromatography was 98%;

[0026] 1.2 Preparation of 3-chloro-2,2-difluoropropanol

[0027] The 3L reaction kettle was condensed and cooled by the coil, vacuumized, and 500g of carbon tetrachloride solution of 2-chloro-1,1-difluoroethylene with a mass concentration of 22.6% in the cold well was sucked into the kettle, which contained 2-chloro- Add 113g of 1,1-difluoroethylene, add 1101g of me...

Embodiment 2

[0031] 2.1 Preparation of 2-chloro-1,1-difluoroethylene

[0032] In a 2000ml three-necked flask, add 1166g of 30% aqueous sodium hydroxide solution, 5g of tetrabutylammonium bromide, and add 1,2-dichloro-1,1-difluoroethane 500g while stirring with a dropping funnel, in React at 30°C for 6 hours, then pass the gas through the condenser tube into the collection bottle with 1 kg of carbon tetrachloride remaining, and cool the collection bottle to minus 25°C with dry ice. The weight of the collection bottle increased by about 300g; the purity of the reaction gas 2-chloro-1,1-difluoroethylene detected by gas chromatography was 99%;

[0033] 2.2 Preparation of 3-chloro-2,2-difluoropropanol

[0034] The 3L reaction kettle was condensed and cooled by the coil, vacuumized, and 500g of carbon tetrachloride solution of 2-chloro-1,1-difluoroethylene with a mass concentration of 22.6% in the cold well was sucked into the kettle, which contained 2-chloro- Add 113g of 1,1-difluoroethylene,...

Embodiment 3

[0038] 3.1 Preparation of 2-chloro-1,1-difluoroethylene

[0039] Add 1200g of 30% sodium hydroxide aqueous solution and 3.8g of tetrabutylammonium bromide into a 2000ml three-necked flask, and add 500g of 1,2-dichloro-1,1-difluoroethane while stirring with a dropping funnel, React at 30°C for 6h, then pass the gas through the condenser tube into the collecting bottle with 1kg of carbon tetrachloride remaining, and the collecting bottle is cooled to minus 25°C by dry ice. The weight of the collection bottle increased by about 300g; the purity of the reaction gas 2-chloro-1,1-difluoroethylene detected by gas chromatography was 98%;

[0040] 3.2 Preparation of 3-chloro-2,2-difluoropropanol

[0041] The 3L reaction kettle was condensed and cooled by the coil, vacuumized, and 500g of carbon tetrachloride solution of 2-chloro-1,1-difluoroethylene with a mass concentration of 22.6% in the cold well was sucked into the kettle, which contained 2-chloro- Add 113g of 1,1-difluoroethyle...

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Abstract

The invention relates to the technical field of fluorine chemical engineering, in particular to a preparation method of 2,2-difluoro-1,3-propanediol. The preparation method is concretely characterized in that a sodium hydroxide water solution is used as a base solution; tetrabutylammonium bromide is added; 1,2-dichloro-1,1-difluoroethane is added; after reaction, the materials are introduced into a container containing carbon tetrachloride; dry ice cooling is performed to obtain 2-chloro-1,1-difluoroethylene; condensing and temperature reduction are performed; vacuumization is performed, so that a tetrachloromethane solution of the 2-chloro-1,1-difluoroethylene is sucked into a kettle; methyl alcohol, initiating agents, lauryl mercaptan and nanometer basic zinc carbonate are added; temperature rise reaction is performed; after the reaction is finished, reduced pressure distillation is performed to obtain 3-chloro-2,2-difluoro propyl alcohol; the 3-chloro-2,2-difluoro propyl alcohol is added into potassium hydroxide and N,N-dimethylformamide; after the reaction is finished, filtering is performed; filtering liquid is subjected to reduced pressure distillation to obtain the product. The preparation method has the advantages that the process is simple; the stability is good; the requirements on equipment are low; the preparation method is suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of fluorine chemical industry, in particular to a preparation method of 2,2-difluoro-1,3-propanediol. Background technique [0002] 1,2-Dichloro-1,1-difluoroethane is an important by-product of the industrial production of difluorochloroethane (142b). In recent years, with the application of fluorine-containing material PVDF, the waste of fluorine resources caused by 1,2-dichloro-1,1-difluoroethane has become more and more prominent. There are many reports at home and abroad on the synthesis of ethyl difluorobromoacetate, an intermediate of anticancer drug gemcitabine, by using 1,2-dichloro-1,1-difluoroethane. This route is an important way to turn waste into treasure. [0003] 2,2-difluoro-1,3-propanediol, with a boiling point of 250.9°C and a density of 1.334g / ml, can be used in the synthesis of various drugs, new polyester PTT, pharmaceutical intermediates and new antioxidants, and can be used in fluorin...

Claims

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Application Information

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IPC IPC(8): C07C29/00C07C31/42C07C29/36C07C31/36C07C17/25C07C21/18
CPCC07C17/25C07C29/00C07C29/36C07C31/42C07C31/36C07C21/18
Inventor 魏坤肖玉岭
Owner 山东飞源新材料有限公司
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