Perfluoro surfactant and preparation method thereof

A technology of fluorosurfactant and perfluoropolyetheryl fluoride, which is applied in the field of perfluorosurfactant and its preparation, can solve the problems of low average molecular weight and easy breakage of fluoropolymers, reduce surface tension and improve weather resistance , Reduce the effect of side reaction optical coupling reaction

Active Publication Date: 2019-02-26
INNER MONGOLIA HUANSHENG TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The object of the present invention is to provide a kind of perfluorosurfactant and preparation method thereof, to solve the non-fluorine atom chemical bond in the fluorine-containing surfactant in the prior art is easy to break under high temperature and pressure, resulting in the fluoropolymer emulsion process Problems such as low average molecular weight of the prepared fluoropolymer

Method used

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  • Perfluoro surfactant and preparation method thereof
  • Perfluoro surfactant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0067] Preparation of perfluoropolyetheryl fluoride P1:

[0068] Such as figure 2 Shown, the continuous flow microchannel reaction system comprises three first microchannel reactors 1 and four second microchannel reactors 2, wherein, the third first microchannel reactor 1 and the first second microchannel reactor The reactor 2 is connected, and the fourth second microchannel reactor 2 is connected with the gas-liquid separation tank 3 .

[0069] During the reaction, hexafluoropropylene was pumped into the reaction system with a flow rate of 30ml / min by a plunger pump, and ozone was pumped into the reaction system with a flow rate of 10ml / min, and hexafluoropropylene and ozone were carried out in three first microchannel reactors 1 The ozonation reaction gives The reaction temperature of the first microchannel reactor 1 is controlled at 10°C. Pump oxygen into the first second microchannel reactor 2 with the flow rate of 10ml / min afterwards, hexafluoropropylene, oxygen and ...

Embodiment 2

[0078] Preparation of perfluoropolyetheryl fluoride P2:

[0079] The continuous flow microchannel reaction system comprises two first microchannel reactors 1 and eight second microchannel reactors 2, wherein the second first microchannel reactor 1 and the first second microchannel reactor 2 Connection, the eighth second microchannel reactor 2 is connected with the gas-liquid separation tank 3.

[0080] During the reaction, hexafluoropropylene was pumped into the reaction system with a flow rate of 30ml / min by a plunger pump, and ozone was pumped into the reaction system with a flow rate of 5ml / min, and hexafluoropropylene and ozone were carried out in two first microchannel reactors 1 The ozonation reaction gives The reaction temperature of the first microchannel reactor 1 is controlled at 10°C. Pump oxygen into the first second microchannel reactor 2 with the flow rate of 10ml / min afterwards, hexafluoropropylene, oxygen and active intermediate The perfluoropolyetheryl fl...

Embodiment 3

[0090] Perfluorosurfactant stability verification experiment:

[0091] The perfluorosurfactant S1 prepared in Example 1 was verified by the polymerization scheme disclosed in the patent CN103936906B.

[0092] Include the following steps:

[0093] (S01) prepare the aqueous solution of the ammonium salt of perfluorosurfactant S1:

[0094] Add 700g of deionized water and 100g of 25% ammonia water in a 2000ml glass beaker, then slowly and uniformly drop 200g of perfluorosurfactant S1 into the deionized water through a glass dropping funnel, stir while adding, and the stirring speed is 80rpm, to obtain the ammonium salt aqueous solution of perfluorosurfactant S1 for subsequent use, wherein the weight ratio of ammonium salt of dicarboxylic acid-terminated perfluoropolyether to water is 20:100;

[0095] (S02) Polymerization preparation: replace the high-pressure polymerization kettle with nitrogen to exhaust oxygen, so that the high-pressure polymerization kettle is evacuated until...

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Abstract

The invention discloses a perfluoro surfactant and a preparation method thereof. When the perfluoro surfactant is used as an emulsifier of a fluorine polymer reaction, a carbon fluorine band is not liable to break, and the average molecular weight of a fluorine polymer generated from the fluorine polymer reaction can be remarkably increased. The preparation method is implemented in a continuous micro channel reaction system, the retention time of a reactant in the reaction system can be greatly shortened to minutes or even seconds, a back mixing phenomenon in the reaction system can be basically eliminated, and a side reaction, namely a photonic coupled reaction, can be greatly reduced. Reaction sections comprise an ozonization reaction and a photonic oxidation reaction, a user is allowedto control the amount and the existing time of ozone in the whole reaction system by adjusting the reaction time in an ozonization reaction module and a photonic oxidation reaction module, and the addition amount of ozone and oxygen, furthermore the ratio of main and side reactions is controlled, and the yield of diacyl fluoride end perfluoro polyether is remarkably increased.

Description

technical field [0001] The invention relates to the field of fluorinated surfactants, in particular to a perfluorosurfactant and a preparation method thereof. Background technique [0002] Fluorosurfactant, referred to as FSA, is a surfactant with a fluorocarbon chain as a non-polar group, that is, a part or all of the hydrogen atoms on the hydrocarbon chain are replaced by fluorine atoms. Fluorocarbon surfactants have high surface activity, high thermodynamic and chemical stability. [0003] At present, fluorosurfactants are widely used in the production process of fluoropolymer emulsion polymerization. However, the existing fluorosurfactants have perfluorooctanoic acid with an 8-carbon straight chain structure, which is biologically toxic and can cause cancer. At the same time, perfluorooctanoic acid and its salts are not easy to be decomposed by nature and are easy to accumulate in the natural environment. Therefore, it is necessary to develop a fluorosurfactant that do...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/00C08F114/26C08F2/24
CPCC08F2/24C08F114/26C08G65/007C08F14/26C08G2650/48C08G65/2603C08F2/26C09K23/007
Inventor 陈艾
Owner INNER MONGOLIA HUANSHENG TECH CO LTD
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