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Ethylperfluorohexyl acetic acid and synthesizing method thereof

A synthetic method, perfluorohexyl technology, applied in chemical instruments and methods, carboxylate preparation, carboxylate preparation, etc., can solve the problems of high corrosion, highly toxic oxidant, high cost, etc., and achieve high heat resistance stability , high chemical stability, and easy industrial mass production

Active Publication Date: 2019-02-15
陈敏
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  • Summary
  • 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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  • Ethylperfluorohexyl acetic acid and synthesizing method thereof
  • Ethylperfluorohexyl acetic acid and synthesizing method thereof
  • Ethylperfluorohexyl acetic acid and synthesizing method thereof

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preparation example Construction

[0025] A kind of synthesis method of ethylene-perfluorohexylacetic acid provided by the embodiment of the present invention comprises the following steps:

[0026] (1) Mix hexafluoropropylene dimer D2, phenol, organic solvent and fluorine salt and heat to 50°C-70°C, then add BrCH in batches 2 CO 2 R, R includes -CH 3 or -CH 2 CH 3 , and then heating the formed mixed reaction system to 75° C. to 90° C. and keeping it warm for esterification reaction. After the reaction, 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 esterified product is separated therein;

[0028] (3) hydrolyzing the esterified product obtained in step (2) with a base to obtain a salt;

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

[0030] In some embodiments, the step (1) specifically includes: mixing hexafluo...

Embodiment 1

[0051] Embodiment 1: the ethylene-perfluorohexylacetic acid synthetic method of the present embodiment comprises following specific 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 are pumped into the head tank through a diaphragm pump for subsequent esterification. 60 parts by weight of DMF, 6 parts by weight of phenol, and 50 parts by weight of polymer solution are pumped into the esterification kettle using a diaphragm pump. Put 30 parts by weight of potassium fluoride into the kettle and start stirring, turn on the electric heating jacket to start heating and set the temperature to 65°C. When the temperature of the material in the kettle rises to a certain te...

Embodiment 2

[0066] Embodiment 2: the synthetic method of the ethylene-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 are pumped into the head tank through a diaphragm pump for subsequent esterification, 40 parts by weight of DMF, 2 parts by weight of phenol, and 70 parts by weight of polymer solution are pumped into the esterification kettle using a diaphragm pump. Put 10 parts by weight of potassium fluoride into the kettle and start stirring, turn on the electric heating jacket to start heating and set the temperature to 70°C. When the temperature of the material in the kettle rises to a...

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Abstract

The invention discloses ethylperfluorohexyl acetic acid and a synthesizing method thereof. The synthesizing method comprises the following steps: mixing and heating hexafluoropropylene dipolymer D2, phenol, an organic solvent and villiaumite; adding BrCH2CO2R into the mixture in batches, wherein R comprises -CH3 or -CH2CH3; performing esterification reaction; cooling an obtained reaction mixed system to room temperature, performing fractionation treatment, and separating an esterification substance out from the reaction mixed system; performing hydrolyzing on the obtained esterification substance and an alkaline to obtain a salt; and finally, performing neutralizing on the obtained salt and an acid to obtain the ethylperfluorohexyl acetic acid. Compared with the prior art, the ethylperfluorohexyl acetic acid disclosed by the invention has the characteristics of high surface activity, high heat resistance stability, high chemical stability and the like; and moreover, the synthesizing method is simple and facilitates industrial mass production.

Description

technical field [0001] The invention relates to the technical field of ethylene-perfluorohexylacetic acid, in particular to a ethylene-perfluorohexylacetic acid and a synthesis method thereof. Background technique [0002] Compared with traditional surfactants, fluorine-containing surfactants have more advantages, such as: high surface activity, high heat resistance and high chemical stability, and its fluorine-containing hydrocarbon groups are both hydrophobic and oil-repellent, so Fluorosurfactants are by far the most active of all surfactants. The addition of very low levels of fluorosurfactants can greatly reduce the surface tension of water. Solve some phenomena such as edge shrinkage, shrinkage cavity, and crater caused by low surface energy or oily surface, which is difficult to wet and spread. [0003] A commonly used fluorine-containing surfactant is perfluorooctanoic acid, which has hydrophobic and oleophobic properties, and its chemical structure is more stable ...

Claims

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Application Information

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