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Method for preparing fluoropolyolefin based on gemini type fluorosurfactant

A surfactant and gemini-type technology, which is applied in the field of gemini-type fluorosurfactants and its preparation, can solve the problems of cumulative toxicity, long carbon chain refractory degradation, etc., and achieve excellent surface activity, high productivity, and high solid content. Effect

Active Publication Date: 2022-05-10
SHENZHEN TAIKE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the long carbon chains in the existing commonly used fluorosurfactants such as PFOS and PFOA are difficult to degrade, accumulate toxicity, and the hydrophobic performance needs to be further improved.

Method used

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  • Method for preparing fluoropolyolefin based on gemini type fluorosurfactant
  • Method for preparing fluoropolyolefin based on gemini type fluorosurfactant
  • Method for preparing fluoropolyolefin based on gemini type fluorosurfactant

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preparation example Construction

[0067] The present invention further discloses the preparation method of the above-mentioned gemini type fluorine-containing surfactant, first forming a block copolymer by coupling method with perfluoropolyether and chlorinated polyethylene glycol monomethyl ether, and further hydrolyzing the block copolymer Condensation obtains gemini type surfactant, specifically comprises the following steps:

[0068] (1) Alkenylation of perfluoropolyether

[0069] a. Prepare acid-binding agent: by weight, dissolve 4-30 parts of inorganic base in 8-300 parts of water to obtain acid-binding agent;

[0070] b. Substitution reaction: by weight, put into the reactor 50~100 parts of perfluoropolyether alcohol, 0.4~1 part of tetrabutylammonium bromide, 50~3000 parts of fluoroalkylbenzene solvent, 4~50 parts of halogen Substituting allyl group, control the temperature at 20-85°C, add the prepared acid-binding agent dropwise, and the dropping time is 30 minutes to 2 hours; after the addition, keep...

Embodiment 1

[0091] (1) Synthesis of chlorosilanized perfluoropolyether

[0092] 5.6g of potassium hydroxide is dissolved in 20g of deionized water to obtain an acid-binding agent for subsequent use;

[0093] A 500mL three-necked flask was equipped with a thermometer, a reflux condenser and a constant pressure dropping funnel, and 170g of 1,3-bistrifluorotoluene, 80g of number-average perfluoropolyether alcohol (molecular weight: 2000, purchased from HEC Group), and 0.5g of four Butylammonium bromide, 5.3g propylene bromide; after stirring to dissolve completely, raise the temperature to 85°C, add the pre-prepared acid-binding agent dropwise, the dropwise addition time is 30 minutes, and keep warm for 4 hours after the addition;

[0094] After the reaction, stand still and separate layers, discard the upper water layer, add 3g of anhydrous magnesium sulfate to the lower oil layer and dry for 12 hours, filter and remove the desiccant to obtain an alkenylated perfluoropolyether solution, whi...

Embodiment 2

[0107] (1) Synthesis of chlorosilanized perfluoropolyether

[0108] 5.6g of potassium hydroxide is dissolved in 20g of deionized water to obtain an acid-binding agent for subsequent use;

[0109] A 500mL three-necked flask was equipped with a thermometer, a reflux condenser and a constant pressure dropping funnel, and 170g of 1,3-bistrifluorotoluene, 120g of number-average perfluoropolyether alcohol (molecular weight of 3000, purchased from HEC Group), and 0.5g of four Butylammonium bromide, 5.3 g propene bromide. After stirring to dissolve completely, raise the temperature to 85°C, add the pre-prepared acid-binding agent dropwise for 30 minutes, and keep it warm for 4 hours after adding;

[0110] After the reaction, stand still and separate layers, discard the upper water layer, add 3g of anhydrous magnesium sulfate to the lower oil layer and dry for 12 hours, filter and remove the desiccant to obtain an alkenylated perfluoropolyether solution, which is transferred to a 500m...

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Abstract

The invention relates to a method for preparing fluoropolyolefins based on a gemini-type fluorosurfactant. In the presence of an initiator and a gemini-type fluorosurfactant, the monomer fluoroolefin is used as a raw material for polymerization reaction to prepare a fluoroolefin polymer ;Use perfluoropolyether-polyethylene glycol-methyl monochlorosilane (PFPE-SiCl-PEG) to hydrolyze and condense to obtain a gemini-type fluorosurfactant, which is directly bonded by an ether bond (-O-) to make Two hydrophobic segments and two hydrophilic segments are tightly coupled to form a compact gemini surfactant structure, which provides excellent surface activity. The fluorine-containing surfactant provided by the invention is applied to the dispersion polymerization of fluoroolefins. The monomer fluoroolefins have strong dispersion in the water phase, and the solid content of a single polymerization tank can reach 25% to 32%, which has the advantage of high productivity.

Description

technical field [0001] The invention relates to a gemini-type fluorine-containing surfactant, its preparation method and application, and belongs to the field of fine chemicals and auxiliary agent synthesis. Background technique [0002] Perfluoropolyethers (Perfluoropolyethers, PFPE) were first discovered in the 1960s. They are a special kind of perfluoropolymer compounds with an average molecular weight ranging from 500 to 15,000. Composed of carbon, fluorine and oxygen elements, the product has a series of characteristics such as heat resistance, oxidation resistance, radiation resistance, corrosion resistance, and non-combustibility. [0003] The prior art discloses a method of polymerizing or copolymerizing fluorinated monomers using a free radical initiator and a fluorinated surfactant in an aqueous dispersion. In order to increase the speed of the polymerization reaction, the reaction is carried out in a neutral It is carried out in the presence of a terminal perfluo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F114/26C08F2/30C08F2/16C08G81/00
CPCC08F114/26C08F2/30C08F2/16C08G81/00
Inventor 李战雄
Owner SHENZHEN TAIKE TECH
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