A kind of preparation method of fluoropolymer surfactant

A technique for surfactants and polymers, applied in the field of preparation of fluoropolymer surfactants, to achieve the effects of narrow molecular weight distribution, low critical micelle concentration, and broad application prospects

Inactive Publication Date: 2015-09-23
广州市科灵精细化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, to the best of our knowledge, the synthesis of fluorine-containing amphiphilic block copolymer polymeric surfactants using RAFT polymerization technology is rarely reported.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Step 1: At room temperature, azobisisobutyronitrile: N, N dimethylaminoethyl methacrylate: 1,4-dioxane: 2-(ethoxycarbonyl) isopropyl ester according to the mass ratio of 4 : 350: 1050: 21 was added to a four-necked flask equipped with a reflux condenser, an air guide tube, and a thermometer, in which 1,4-dioxane was used as a solvent to obtain a mixture of N,N dimethylaminoethyl acrylate ;

[0017] Step 2: Pass argon to the mixture of N,N dimethylaminoethyl acrylate obtained in the above step 1 for 30 minutes at a rate of 200ml / min, then heat to raise the temperature to 60°C, and react under the protection of argon 8h, obtain polymethacrylate N,N dimethylaminoethyl ester;

[0018] Step 3: Mix azobisisobutyronitrile: 1,4-dioxane: hexafluorobutyl acrylate in a mass ratio of 1.5:1500:450 to obtain a mixture;

[0019] Step 4: Add the mixture obtained in the above step 3 into a four-necked bottle filled with N,N dimethylaminoethyl methacrylate, pass argon for 30 minutes, a...

Embodiment 2

[0024] Step 1: At room temperature, mix azobisisobutyronitrile: N,N dimethylaminoethyl methacrylate: 1,4-dioxane: cumyl dithiobenzoate according to the mass ratio of 6:700 : 1050: 42 was added to a four-neck flask equipped with a reflux condenser, an air guide tube, and a thermometer, wherein 1,4-dioxane was used as a solvent to obtain a mixture of N,N dimethylaminoethyl acrylate;

[0025] Step 2: Pass argon gas through the mixture of N,N dimethylaminoethyl acrylate obtained in the above step 1 for 30 minutes at a rate of 200ml / min, then heat to raise the temperature to 70°C, and react under the protection of argon 5h, obtain polymethacrylic acid N, N dimethylamino ethyl ester;

[0026] Step 3: Mix azobisisobutyronitrile: 1,4-dioxane: hexafluorobutyl acrylate according to the mass ratio of 4.5:3000:850 to obtain a mixture;

[0027] Step 4: Add the mixture obtained in the above step 3 into a four-necked bottle filled with N,N dimethylaminoethyl methacrylate, pass argon for 30 ...

Embodiment 3

[0032] Step 1: At room temperature, mix azobisisobutyronitrile: N,N dimethylaminoethyl methacrylate: 1,4-dioxane: 2-{[(dodecylthio)methylthio Acyl]sulfanyl}succinic acid was added into a four-necked flask equipped with a reflux condenser, air guide tube, and thermometer according to the mass ratio of 8:1050:2100:63, wherein 1,4-dioxane was used as a solvent to obtain A mixture of N,N dimethylaminoethyl acrylate;

[0033] Step 2: Pass argon gas through the mixture of N,N dimethylaminoethyl acrylate obtained in the above step 1 for 30 minutes at a rate of 200ml / min, then heat to raise the temperature to 80°C, and react under the protection of argon 4h, obtain polymethacrylate N,N dimethylaminoethyl ester;

[0034] Step 3: Mix azobisisobutyronitrile: 1,4-dioxane: hexafluorobutyl acrylate in a mass ratio of 7.5:4500:1250 to obtain a mixture;

[0035] Step 4: Add the mixture obtained in the above step 3 into a four-necked bottle filled with N,N dimethylaminoethyl methacrylate, pa...

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Abstract

The invention discloses a preparation method of a fluorine-containing high-molecular surfactant, and the preparation method comprises the following steps: enabling an initiator, methacrylic acid-N,N-ethyl dimethylamide, a chain transfer agent and 1,4-dioxane to react at 60-90 DEG C in the presence of the argon to obtain polymethylacrylic acid-N,N-ethyl dimethylamide; adding the initiator, hexafluorobutyl acrylate and 1,4-dioxane, and reacting for 2-8 hours at 65-95 DEG C in the presence of argon; precipitating in n-hexane; drying to obtain the fluorine-containing high-molecular surfactant. By adopting an RAFT polymerization technology, the prepared fluorine-containing high-molecular surfactant contains a fluorine-containing unit similar to the structure of a fluorine-containing monomer, has the characteristics of narrow molecular weight distribution, adjustable structure, low critical micelle concentration, good emulsibility, low foamability and the like, and has broad application prospect in emulsion polymerization.

Description

technical field [0001] The invention belongs to the technical field of fluorine chemical industry, and in particular relates to a preparation method of a fluoropolymer surfactant. Background technique [0002] Traditional emulsifiers are enriched on the surface of monomers or particles through physical adsorption. Therefore, when subjected to high shear force, centrifugal force, high temperature and low temperature, the emulsifier layer is easy to desorb and fall off, resulting in poor emulsification ability. Polymer surfactants generally refer to polymer compounds with a relative molecular mass of more than several thousand and surface active functions. They contain both hydrophilic groups and lipophilic groups. Much smaller than ordinary polyelectrolytes with the same relative molecular mass. Compared with ordinary small molecule emulsifiers, polymer surfactants have the characteristics of poor foaming, low critical micelle concentration, good emulsifying power, excellent...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F293/00C08F220/34C08F220/22C08F2/38C08F2/30
Inventor 周建华王海龙马建中鲁妮
Owner 广州市科灵精细化工有限公司
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