Fluorine silicon di-block copolymers and preparation method thereof

A technology of block copolymer and copolymer, which is applied in the field of fluorosilicon two-block copolymer and its preparation, can solve the problems of destroying the side chain structure of polysiloxane, etc., and achieves high product yield, few side reactions, mild Effects of reaction conditions

Inactive Publication Date: 2008-08-06
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

These three methods have their own disadvantages: for example, the method of grafting polysiloxane macromonomers to the fluorocarbon backbone and the method of grafting perfluoroside chains onto the polysiloxane backbone usually require high-temperature catalysis by noble metals. The reaction ...

Method used

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  • Fluorine silicon di-block copolymers and preparation method thereof
  • Fluorine silicon di-block copolymers and preparation method thereof
  • Fluorine silicon di-block copolymers and preparation method thereof

Examples

Experimental program
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Embodiment 1

[0019] 1) Under the protection of nitrogen atmosphere, react 1 part of monomethanol-terminated polydimethylsiloxane, 1.35 parts of 2-bromoisobutyryl bromide and 2.52 parts of triethylamine at 0°C. Then the above solution was stirred and reacted for 24 hours. After the reaction was completed, it was filtered, and the filtrate was distilled off under reduced pressure to remove the solvent, and then dissolved in dichloromethane, washed several times with saturated sodium bicarbonate solution, separated, and the organic layer was Use anhydrous magnesium sulfate to dry and remove water, then filter, and finally the filtrate is distilled off under reduced pressure to remove the methylene chloride solvent to obtain an oily yellow macromolecular initiator;

[0020] 2) The reaction system must be strictly deoxygenated, using 1 part of macromolecule as initiator, 1 part of cuprous bromide as catalyst, and 2 parts of N-(n-propyl)-2-pyridinemethanamine as catalyst ligand React with 15 par...

Embodiment 2

[0022] 1) Under the protection of argon atmosphere, react 1 part of monomethanol-terminated polydimethylsiloxane, 1.5 parts of 2-bromoisobutyryl bromide and 3 parts of triethylamine at 5°C. Then the above solution was stirred and reacted for 20 hours. After the reaction was completed, it was filtered, and the filtrate was distilled off under reduced pressure to remove the solvent, and then dissolved in dichloromethane, washed twice with sodium bicarbonate solution, separated, and the organic layer was used Anhydrous magnesium sulfate is dried to remove water, then filtered, and finally the filtrate is distilled off under reduced pressure to remove the dichloromethane solvent to obtain an oily yellow macromolecular initiator;

[0023] 2) The reaction system must be strictly deoxygenated, with 1 part of macromolecule as initiator, 1 part of cuprous chloride as catalyst, 2 parts of 1,1,4,7,7-pentamethyldivinyltriamine The catalyst ligand was reacted with 20 parts of heptafluorobu...

Embodiment 3

[0025] 1) Under the protection of nitrogen atmosphere, react 1 part of monomethanol-terminated polydimethylsiloxane, 1.8 parts of 2-bromoisobutyryl bromide and 3 parts of triethylamine at 15°C. Then the above solution was stirred and reacted for 18 hours. After the reaction was completed, it was filtered, and the filtrate was distilled off under reduced pressure to remove the solvent, then dissolved in dichloromethane, washed twice with saturated sodium bicarbonate solution, separated, and the organic layer was Use anhydrous magnesium sulfate to dry and remove water, then filter, and finally the filtrate is distilled off under reduced pressure to remove the methylene chloride solvent to obtain an oily yellow macromolecular initiator;

[0026] 2) The reaction system must be strictly deoxygenated, with 1 part of macromolecule as initiator, 1 part of cuprous bromide as catalyst, 2 parts of 1,1,4,7,7-pentamethyldivinyltriamine The catalyst ligand was reacted with 20 parts of hepta...

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Abstract

A fluorine silicon diblock copolymer and a relative preparation method relate to a fluorine silicon low surface energy diblock copolymer. The invention provides a fluorine silicon diblock copolymer (dimethyl silicone polymer-b-polyheptafluorobutyric methacrylate ester copolymer) and a relative preparation method, with mild reaction conditions, definite product structure, kept skeleton structure of each block and simple operation, wherein the fluorine silicon diblock copolymer is dimethyl silicone polymer-b-polyheptafluorobutyric methacrylate ester copolymer. The preparation method comprises preparing dimethyl silicone polymer macromolecule inducer terminated by bromine atom and preparing dimethyl silicone polymer-b-polyheptafluorobutyric methacrylate ester copolymer.

Description

technical field [0001] The present invention relates to a kind of fluorine-silicon low surface energy diblock copolymer, especially relate to a kind of macromolecule polydimethylsiloxane as macroinitiator, in Cu(I)Br as catalyst, N-(n -Propyl)-2-pyridinemethylamine is a preparation method for synthesizing target polymer polydimethylsiloxane-b-polyheptafluorobutyl methacrylate through atom transfer radical polymerization under the co-catalysis of catalyst ligands. Background technique [0002] Polydimethylsiloxane-b-polyheptafluorobutyl methacrylate is a new type of low surface energy fluorosilicone block copolymer, which has not been reported so far. It has a low surface energy and is expected to be used in antifouling coatings , The field of surface modifiers has been widely used. Silicone polymers have some special excellent properties, such as high elasticity, extremely low glass transition temperature, low surface tension, high gas permeability, high heat resistance and...

Claims

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Application Information

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IPC IPC(8): C08F283/12C08G77/442
Inventor 罗正鸿何腾云戴李宗
Owner XIAMEN UNIV
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