Preparation method of amphiphilic segmented copolymer

An amphiphilic block and copolymer technology is applied in the field of amphiphilic block copolymers, which can solve the problems of difficulty in industrialization, difficulty in industrialization, and increase in production cost, and achieve the effects of reducing sensitivity, reducing cost and low dosage.

Inactive Publication Date: 2012-04-04
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The use of a large number of catalysts not only increases the production cost, but also the removal and reuse of the catalyst after polymerization is a problem that is not easy to solve, and the industrialization is difficult and difficult to carry out.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Example 1: Polyethylene glycol monomethyl ether- b - Preparation of polyhexafluorobutyl methacrylate

[0022] (1) Prepare a macroinitiator with polyethylene glycol monomethyl ether with a molecular weight of 1000

[0023] Add 40g (0.040mol) of polyethylene glycol monomethyl ether, 12.1428g (0.120mol) of triethylamine, and 240g of dichloromethane into a 500ml four-neck flask, and stir magnetically in an ice-water bath until the temperature of the system drops below 5°C , and slowly add α-bromoisobutyryl bromide 27.588g (0.120mol) dropwise, and control the temperature below 5°C. After the dropwise addition, the reaction system was reacted at room temperature (20° C. to 30° C.) for 48 hours. After the reaction, add dichloromethane until the solution is transparent, then wash with 5% hydrochloric acid solution, 5% sodium hydroxide solution, and distilled water for 3 to 5 times, separate the lower layer, add anhydrous magnesium sulfate, and let stand to remove water. It...

Embodiment 2

[0027] Example 2:Polyethylene glycol monomethyl ether- b - Preparation of polybutyl acrylate

[0028] (1) Prepare a macroinitiator with polyethylene glycol monomethyl ether with a molecular weight of 1000

[0029] Add 40g (0.040mol) of polyethylene glycol monomethyl ether, 12.1428g (0.120mol) of triethylamine, and 240g of dichloromethane into a 500ml four-neck flask, and stir magnetically in an ice-water bath until the temperature of the system drops below 5°C , and slowly add α-bromoisobutyryl bromide 27.588g (0.120mol) dropwise, and control the temperature below 5°C. After the dropwise addition, the reaction system was reacted at room temperature (20° C. to 30° C.) for 48 hours. After the reaction, add dichloromethane until the solution is transparent, then wash with 5% hydrochloric acid solution, 5% sodium hydroxide solution, and distilled water for 3 to 5 times, separate the lower layer, add anhydrous magnesium sulfate, and let stand to remove water. It was then f...

Embodiment 3

[0033] Example 3: Polyethylene glycol monomethyl ether- b - Preparation of polystyrene

[0034] (1) Prepare a macroinitiator with polyethylene glycol monomethyl ether with a molecular weight of 1000

[0035] Add 40g (0.040mol) of polyethylene glycol monomethyl ether, 12.1428g (0.120mol) of triethylamine, and 240g of dichloromethane into a 500ml four-neck flask, and stir magnetically in an ice-water bath until the temperature of the system drops below 5°C , and slowly add α-bromoisobutyryl bromide 27.588g (0.120mol) dropwise, and control the temperature below 5°C. After the dropwise addition, the reaction system was reacted at room temperature (20° C. to 30° C.) for 48 hours. After the reaction, add dichloromethane until the solution is transparent, then wash with 5% hydrochloric acid solution, 5% sodium hydroxide solution, and distilled water for 3 to 5 times, separate the lower layer, add anhydrous magnesium sulfate, and let stand to remove water. It was then filtere...

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Abstract

The invention which relates to a preparation method of an amphiphilic segmented copolymer belongs to the field of chemical engineering materials. According to the method, polyethylene glycol monomethyl ether with the molecular weight of 200-5000 and alpha-halogenated acyl halide undergo an esterification reaction to obtain a hydrophilic macromolecular initiator; and the segmented copolymer with controllable molecular weight and narrow molecular weight distribution (PDI is equal to or less than 1.5) is obtained by catalyzing ARGET ATRP of a (methyl) acrylic acid ester monomer, a fluorine-containing (methyl)acrylic acid ester monomer or a styrene monomer with the hydrophilic macromolecular initiator as an initiator and a low concentration oxidation state transition metal salt as a catalyst in the presence of an organic reductant. Compared with common atom free radical polymerization methods, the novel atom free radical polymerization method allows the catalyst consumption amount to be less, the sensitivity to a small amount of water and air to be reduced, the obtained polymer to be almost colorless, post-treatment steps to be reduced, even omitted, the production cost to be reduced, and industrialization production requirements to be better satisfied.

Description

technical field [0001] The invention belongs to the field of chemical materials, and relates to amphiphilic synthesis of polyethylene glycol monomethyl ether chain segments with hydrophilicity and polymer chain segments with hydrophobicity by electron transfer regeneration catalyst atom transfer radical polymerization (ARGET ATRP). permanent block copolymers. Background technique [0002] Amphiphilic block polymers have become one of the research hotspots in the field of polymer science because of their special properties and wide applications. Amphiphilic block copolymers refer to polymers containing two different chemical structures of hydrophilic and lipophilic in the same molecular chain. Because of the presence of two blocks of different chemical structures in the same molecule, it shows Many different chemical and physical properties from general block copolymers. The micelles formed by block copolymers can be used as a medium for drug delivery systems; they can also...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F293/00C08F220/22C08F220/18C08F212/08
Inventor 李坚陈豪杰穆关敏
Owner CHANGZHOU UNIV
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