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B-perfluorohexylacetic acid and its synthesis method

A technology of perfluorohexyl and synthesis method, which is applied in the field of ethylene-perfluorohexylacetic acid and its synthesis, can solve the problems of high cost, high corrosion, and highly toxic oxidant, and achieve easy industrial mass production, high heat resistance stability, The effect of high chemical stability

Active Publication Date: 2022-03-25
陈敏
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] As one of the substitutes for perfluorooctanoic acid, perfluorohexylacetic acid and its salts have low surface tension and good emulsifying properties for the polymerization of fluorine-containing olefins, but their existing preparation methods have some shortcomings, for example, some of them synthesize The process requires the use of highly corrosive, highly toxic oxidants, and produces a large amount of waste gas and waste water. Some synthesis processes require the use of a large amount of expensive catalysts, which are costly but low in yield.
[0005] In addition, when the existing perfluorohexylacetic acid and its salts are used as surfactants, their comprehensive properties such as surface activity, heat resistance stability and chemical stability need to be improved.

Method used

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  • B-perfluorohexylacetic acid and its synthesis method
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  • B-perfluorohexylacetic acid and its synthesis method

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preparation example Construction

[0025] A kind of synthetic method of ethyl-perfluorohexylacetic acid provided in the embodiment of the present invention, comprises the following steps:

[0026] (1) Mix the hexafluoropropylene dimer D2, phenol, organic solvent and fluorine salt, heat to 50℃~70℃, then add BrCH in batches 2 CO 2 R, R includes -CH 3 or -CH 2 CH 3 , and then heat the formed mixed reaction system to 75 ℃~90 ℃ and keep warm to carry out the esterification reaction, and after the reaction is completed, the obtained reaction mixed system is lowered to room temperature;

[0027] (2) fractional distillation is carried out to the reaction mixture system obtained in step (1), and the ester compound is separated out;

[0028] (3) hydrolysis reaction is carried out with the obtained ester compound of step (2) and alkali to obtain salt;

[0029] (4) neutralizing the salt obtained in step (3) with acid to obtain ethyl-perfluorohexylacetic acid.

[0030] In some embodiments, the step (1) specifically in...

Embodiment 1

[0051] Embodiment 1: the ethyl-perfluorohexylacetic acid synthesis method of the present embodiment comprises the following concrete steps:

[0052] (1) Esterification reaction

[0053] Raw materials include: C 6 F 12 (D2), methyl bromoacetate, DMF, potassium fluoride, phenol. The reaction formula is as follows:

[0054] C 6 F 12 +KF+BrCH 2 CO 2 R→C 6 F 13 CH 2 CO 2 R+KBr(R=CH 3 , CH 2 CH 3 )

[0055] The reaction temperature is 50-85°C. 40 parts by weight of methyl bromoacetate is pumped into the head tank through a diaphragm pump for subsequent esterification, 60 parts by weight of DMF, 6 parts by weight of phenol, 50 parts by weight of polymer solutions are pumped into the esterification kettle using a diaphragm pump, Put 30 parts by weight of potassium fluoride into the kettle, start stirring, open the jacket and start electric heating to start heating. The set temperature is 65°C. When the temperature of the material in the kettle rises to a certain tempe...

Embodiment 2

[0066] Embodiment 2: the synthetic method of the ethyl-perfluorohexylacetic acid of the present embodiment comprises the following concrete steps:

[0067] (1) Esterification reaction

[0068] Raw materials include: C 6 F 12 (D2), methyl bromoacetate, DMF, potassium fluoride, phenol. The reaction formula is as follows:

[0069] C 6 F 12 +KF+BrCH 2 CO 2 R→C 6 F 13 CH 2 CO 2 R+KBr(R=CH 3 , CH 2 CH 3 )

[0070] The reaction temperature is 50-85°C. 30 parts by weight of methyl bromoacetate was pumped into the overhead tank for subsequent esterification, and 40 parts by weight of DMF, 2 parts by weight of phenol, and 70 parts by weight of polymer solutions were pumped into the esterification kettle using a diaphragm pump, Put 10 parts by weight of potassium fluoride into the kettle, start stirring, open the jacket and start electric heating to start heating. The set temperature is 70°C. When the temperature of the material in the kettle rises to a certain temperatu...

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Abstract

The invention discloses a ethylene-perfluorohexylacetic acid and a synthesis method thereof. The synthesis method includes: mixing and heating hexafluoropropylene dimer D2, phenol, organic solvent and fluorine salt, and then adding BrCH in batches 2 CO 2 R, R includes ‑CH 3 or-CH 2 CH 3 , and then carry out esterification reaction, then the obtained reaction mixture system is lowered to room temperature, and fractional distillation is carried out to separate the esterified product therein; then the obtained esterified product is hydrolyzed with a base to obtain a salt; finally the obtained Salt and acid neutralization reaction to obtain B-perfluorohexylacetic acid. Compared with the prior art, the ethylene-perfluorohexylacetic acid of the present invention has the characteristics of high surface activity, high heat resistance stability and high chemical stability, and its synthesis method is simple and easy for industrial mass production.

Description

technical field [0001] The invention relates to the technical field of ethyl-perfluorohexylacetic acid, in particular to a kind of ethyl-perfluorohexylacetic acid and a synthesis method thereof. Background technique [0002] Compared with traditional surfactants, fluorosurfactants have more advantages, such as high surface activity, high thermal stability and high chemical stability. Its fluorocarbon group is both hydrophobic and oil repellent, so Fluorosurfactants are by far the most surface active of all surfactants. Adding a very low amount of fluorosurfactant can greatly reduce the surface tension of water. Solve some phenomena such as shrinkage, shrinkage, and crater caused by low surface energy or oil on the surface, which is difficult to wet and spread. [0003] A commonly used type of fluorosurfactant is perfluorooctanoic acid, which has hydrophobic and oleophobic properties, its chemical structure is more stable than other surfactants, and it has the advantages of...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C27/02C07C51/02C07C53/21
CPCC07C51/02C07C51/09C07C53/21C07C67/343C07C69/63
Inventor 王亮
Owner 陈敏
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