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A kind of preparation method of fluorine-containing emulsifier

A technology of emulsifiers and catalysts, applied in chemical instruments and methods, organic chemistry, chemical/physical processes, etc., can solve the problems of failing to meet the requirements of the application field, reducing transmission, thermal stability and other performance degradation, and achieving product The effect of quality improvement, low labor intensity and high activity

Active Publication Date: 2018-04-20
JUHUA GROUP TECH CENT +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In method 4), although the reactive surfactant is transferred to the fluororesin through the polymerization reaction, which avoids contact with water and soil, or reduces the transmission with the environment, the fluororesin itself introduces a hydrophilic group, which is thermally stable. The performance such as sex is reduced, so it may not meet the requirements of the application field
[0008] It can be seen that, in fact, so far, the problem of replacing PFOA has not been well solved in the field of fluororesin preparation.

Method used

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  • A kind of preparation method of fluorine-containing emulsifier
  • A kind of preparation method of fluorine-containing emulsifier

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preparation example Construction

[0026] A preparation method of fluorine-containing emulsifier, comprising the following reaction steps:

[0027] (1) Using pentafluoroiodosulfane as a telomer, under the catalysis of catalyst Hg, tetrafluoroethylene is telomerized, and pentafluorosulfanyl perfluoroalkyl iodide is obtained under radiation conditions, and pentafluorosulfane The general structural formula of perfluoroalkyl iodide is SF 5 -(CF 2 -CF 2 )n-I.

[0028] (2) react pentafluorosulfanyl perfluoroalkyl iodide and sulfite in a solvent to generate corresponding sulfonate, control the reaction temperature at 100-140°C, preferably 110-130°C, and the reaction time The reaction time is 2 to 24 hours, the preferred reaction time is 4 to 10 hours, the reaction pressure is 0.05 to 0.2 MPa, the sulfite is sodium sulfite or potassium sulfite, pentafluorosulfanyl perfluoroalkyl iodide and sulfite and sulfite The reaction ratio is 1.0:(1.0~3.0), the preferred reaction ratio is 1.0:(1.5~2.0), the solvent used is the...

example 1

[0041] Add SF to 500mL autoclave 5 -CF 2 -CF 2 -CF 2 -CF 2 -CF 2 -CF 2 -I mass 55.38g (0.1mol), Na 2 SO 3 37.8g (0.3mol), vacuumize, then add 150ml of deionized water and 150ml of NMP through the auxiliary pump, and then heat the temperature of the reaction kettle to 120°C. At this time, the pressure is about 0.01MPa, and the reaction is 6h. After the reaction, filter to remove sulfite; after the filtrate is cooled to room temperature, filter; filter with 150ml of deionized water for three times to obtain SF 5 -CF 2 -CF 2 -CF 2 -CF 2 -CF 2 -CF 2 -SO 3 Na crude product. The crude product was recrystallized with a 1:1 mixed solution of deionized water and NMP, and then dried in a vacuum oven for 24 hours to finally obtain 45.37 g of the product with a yield of 85.6%.

example 2

[0043] Add SF to 500mL autoclave 5 -CF 2 -CF 2 -CF 2 -CF 2 -I quality 45.38g (0.1mol), K 2 SO 3 15.8g (0.3mol), vacuumize, then add 200ml of deionized water and 100ml of DMF through the auxiliary pump, and then heat the temperature of the reaction kettle to 130°C. At this time, the pressure is about 0.05MPa, and the reaction takes 2 hours. After the reaction, filter to remove sulfite; after the filtrate is cooled to room temperature, filter; filter with 150ml of deionized water for three times to obtain SF 5 -CF 2 -CF 2 -CF 2 -CF 2 -SO 3 K Crude. The crude product was recrystallized with a 2:1 mixed solution of deionized water and DMF, and then dried in a vacuum oven for 24 hours to finally obtain 33.67 g of the product with a yield of 75.5%.

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Abstract

The invention discloses a preparation method of a fluorine-containing emulsifier, which comprises the following reaction steps: (1) using iodothiopentafluoropentane as a telomer, under the catalytic action of a catalyst Hg, tetrafluoroethylene is telomerized, and Under irradiation conditions, pentafluorosulfanyl perfluoroalkyl iodides can be obtained. (2) React pentafluorosulfanyl perfluoroalkyl iodide and sulfite in a solvent to generate the corresponding sulfonate, and then recrystallize and purify to obtain fluorine-containing monomer that can be used for emulsion polymerization of fluorine-containing monomers. emulsifier. The preparation method is simple, the labor intensity is low, and the product quality is obviously improved. The carbon number of the main chain of the prepared fluorine-containing emulsifier is less than 8, and still has relatively high activity. The -SF5 in the fluorine-containing emulsifier prepared by the present invention has larger fluorine volume and chemical stability than -CF3, and the prepared corresponding fluorine-containing emulsifier has stronger surface activity. Since the number of main chains is 4 or 6, its bioaccumulation is greatly reduced, and it is superior to traditional hydrocarbon fluorinated emulsifiers in terms of efficiency or effectiveness.

Description

technical field [0001] The invention relates to a fluorine-containing emulsifier, in particular to a preparation method of a fluorine-containing emulsifier. Background technique [0002] PFOA / PFOS perfluorinated emulsifiers are gradually restricted by Swiss, EU and US environmental protection agencies because of their long biodegradation half-life, accumulative properties in organisms, biological carcinogenicity, and regional expansion. The U.S. EPA proposed a voluntary reduction plan for PFOA in 2001, and large companies producing fluorine-containing resins also responded positively, and in 2015 they will implement restrictions on the use of PFOA / PFOS. Research and development of PFOA / PFOS alternative technology in fluorine-containing resin emulsion polymerization has become a common problem faced by the fluorine chemical industry. In China, the use of PFOA has not been completely restricted, but products containing PFOA in the field of coatings related to the food industr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C381/00B01F17/00C09K23/00
CPCC07C381/00C09K23/00
Inventor 汪星平余晓斌王树华
Owner JUHUA GROUP TECH CENT