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Method for preparing hexafluoropropylene oxide trimer

A technology of hexafluoropropylene oxide dimer alcohol and hexafluoropropylene oxide, which is applied in the field of preparing hexafluoropropylene oxide trimer, and can solve the problem of insufficient meeting the needs of industrialized production, dispersion of product polymerization degree, and insufficient selectivity. Advanced problems, to achieve the effect of suitable for large-scale industrial production, high selectivity and high conversion rate

Active Publication Date: 2019-07-23
DONGGUAN DONGYANG SOLAR SCI RES & DEV CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Publication No. US5399754 mentioned in the U.S. patent that fluoride alkali metal salts are used as catalysts and sulfone or ether compounds are used as solvents to prepare hexafluoropropylene oxide trimer with a selectivity higher than 60%; but its There is also the disadvantage that the selectivity is not high enough to meet the needs of industrial production
[0004] The preparation method of hexafluoropropylene oxide trimer disclosed in the existing patent technology has the problems of relatively dispersed degree of polymerization and low selectivity

Method used

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  • Method for preparing hexafluoropropylene oxide trimer
  • Method for preparing hexafluoropropylene oxide trimer

Examples

Experimental program
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Effect test

Embodiment 1

[0054] Add 200ml of tetraethylene glycol dimethyl ether, 37.1g of potassium alkoxide of hexafluoropropylene oxide dimer, 11.6g of potassium fluoride and 5g of trifluoroacetic acid into a 2L reaction kettle with a condensing jacket. Control the temperature in the kettle; feed 1 kg of hexafluoropropylene oxide monomer into the reaction kettle through a metering device, the feeding rate is controlled at 400 sccm, pump the reaction kettle to -1 bar, and maintain the temperature in the kettle at -15°C. After the completion of feeding, the reaction was stirred and kept stirring for 3h.

[0055] After the reaction, the crude product was taken out from the reactor, and the product in the lower layer was removed after liquid separation, and filtered to obtain 0.998 kg of the crude product, and the calculated conversion rate of hexafluoropropylene oxide was 99.8%. Take a small amount of the obtained crude product, add excess methanol for methyl esterification, stir at room temperature f...

Embodiment 2

[0057] Add 200ml of diethylene glycol dimethyl ether, 35.5g of sodium hexafluoropropylene oxide dimer alkoxide, 12.6g of sodium fluoride and 5g of trifluoroacetic acid into a 2L reaction kettle with a condensing jacket. Control the temperature in the kettle; feed 1 kg of hexafluoropropylene oxide monomer into the reaction kettle through a metering device, the feeding rate is controlled at 400 sccm, pump the reaction kettle to -1 bar, and maintain the temperature in the kettle at -15°C. After the completion of feeding, the reaction was stirred and kept stirring for 3h.

[0058] After the reaction, the crude product was taken out from the reaction kettle, and the product in the lower layer was removed after liquid separation, and filtered to obtain 0.991 kg of the crude product, and the conversion rate of hexafluoropropylene oxide was calculated to be 99.1%. Take a small amount of the obtained crude product, add excess methanol for methyl esterification, stir at room temperature...

Embodiment 3

[0060] Add 200ml of acetonitrile, 37.1g of potassium alkoxide of hexafluoropropylene oxide dimer, 11.6g of potassium fluoride and 10g of perfluorohexanoic acid into a 2L reaction kettle with a condensation jacket, and control the temperature inside the kettle through an external circulation refrigeration pump; 1 kg of hexafluoropropylene oxide monomer was fed into the reaction kettle through a metering device, the feeding rate was controlled at 400 sccm, the reaction kettle was pumped to -1 bar, and the temperature inside the kettle was maintained at -15°C. After the completion of feeding, the reaction was stirred and kept stirring for 3h.

[0061] After the reaction, the crude product was taken out from the reaction kettle, and the product in the lower layer was removed after liquid separation, and filtered to obtain 0.995 kg of the crude product, and the conversion rate of hexafluoropropylene oxide was calculated to be 99.5%. Take a small amount of the obtained crude product...

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Abstract

The invention relates to the field of fluorine-containing fine chemistry, in particular to a method for preparing a hexafluoropropylene oxide trimer. Hexafluoropropylene oxide is used as a raw material, hexafluoropropylene oxide dimer alkoxide and fluorinated alkali metal salt are used as composite catalytic initiators, a chain transfer polymerization inhibitor is added, and the hexafluoropropylene oxide trimer is prepared after a reaction. The conversion rate of hexafluoropropylene oxide and the selectivity of the hexafluoropropylene oxide trimer are high in the method, and the operation method is simple, feasible, easy to control industrially and suitable for mass industrial production.

Description

technical field [0001] The invention relates to the field of fluorine-containing fine chemistry, in particular to a method for preparing hexafluoropropylene oxide trimer. Background technique [0002] Hexafluoropropylene oxide trimer is a colorless and transparent liquid at room temperature and is an important fluorine-containing active intermediate. For example, hexafluoropropylene oxide trimer can be prepared into carboxylic acid by hydrolysis. It is a kind of fluorine-containing surfactant with excellent performance. Emulsifiers, electroplating additives, aqueous film-forming foam fire extinguishing agents and other fields. By introducing a coupling group to the end of the hexafluoropropylene oxide trimer, it can be prepared as an excellent fluorine-containing surface protective agent, which is suitable for the surface waterproof, oil-proof and anti-fouling treatment of the substrate. [0003] At present, there are many patents on the preparation of hexafluoropropylene ...

Claims

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Application Information

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IPC IPC(8): C07C51/58C07C53/50
CPCC07C51/58C07C29/68C07C53/50C07C31/30
Inventor 李义涛阳峰侯琴卿贾渊王亮石玲
Owner DONGGUAN DONGYANG SOLAR SCI RES & DEV CO LTD
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