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Fluorine silicon tri-block copolymers and preparation method thereof

The technology of block copolymer and triblock is applied in the field of fluorosilicon triblock copolymer and its preparation. The effect of narrow molecular weight distribution

Inactive Publication Date: 2008-07-09
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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 is completed and the side chain structure of the polysiloxane is destroyed; and the copolymer obtained by copolymerizing two or more vinyl monomers containing siloxane and organic fluorine has no polysilicon in the main chain at all. Oxane backbone, thus losing some of the advantages of polysiloxane

Method used

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] 1) Under the protection of nitrogen atmosphere, react 1 part of monomethanol-terminated polydimethylsiloxane, 1.2 parts of 2-bromoisobutyryl bromide and 2.5 parts of triethylamine at 5°C. Then the above solution was stirred and reacted for 30 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;

[0022] 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 10 parts...

Embodiment 2

[0025]1) Under the protection of argon atmosphere, react 1 part of monomethanol-terminated polydimethylsiloxane, 1.5 parts of 2-bromoisobutyryl bromide and 2.8 parts of triethylamine at 10°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 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;

[0026] 2) Except that the ligand is 1,1,4,7,7-pentamethyldivinyltriamine, the monomer is 20 parts, and the reaction temperature is 50° C., the others are the same as step 2 in Example 1);

[0027] 3) Except that the reaction temperatur...

Embodiment 3

[0029] 1) Except that 2-bromoisobutyryl bromide is 3.6 parts and triethylamine is 4.6 parts, other are the same as step 1 in Example 1);

[0030] 2) except that the monomer is 30 parts, other is the same as step 2 in the embodiment 2);

[0031] 3) Except that the reaction temperature is 70° C. and the ligand is 1,1,4,7,7-pentamethyldivinyltriamine, the procedure is the same as step 3) in Example 2.

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PUM

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Abstract

The invention relates to a fluorine-silicon three-block copolymer and a process for preparation, which relates to the synthesis of fluorine low-surface three-block copolymer. The invention provides a fluorine-silicon three-block copolymer and a process for preparation, whose reaction condition is moderate, the structure of the reaction products is accurate, the original skeleton construction of each block is kept, the production has micro-phase separation structure, and the operation is simple and convenient. The invention is named as dimethyl silicone polymer-b-polymethyl methacryate-b-poly seven-fluorine butyl methacrylate ester, the process for preparation comprises first, preparing dimethyl silicone polymer macromolecule initiator of the sealing end of bromine atom, second, preparing two-block copolymer macromolecule initiator of the dimethyl silicone polymer-b-polymethyl methacryate, finally, preparing the fluorine-silicon three-block copolymer of the dimethyl silicone polymer-b-polymethyl methacryate-b-poly seven-fluorine butyl methacrylate ester.

Description

technical field [0001] The present invention relates to the synthesis of a fluorine-silicon low-surface-energy tri-block copolymer, in particular to a synthesis of polydimethylsiloxane through atom transfer radical polymerization using macromolecular polydimethylsiloxane as a macroinitiator. base siloxane-b-polymethyl methacrylate two-block copolymer, and then use the two-block copolymer as a macroinitiator to initiate the polymerization of heptafluorobutyl methacrylate monomer to synthesize the target polymer polydimethylmethacrylate The preparation method of siloxane-b-polymethyl methacrylate-b-polyheptafluorobutyl methacrylate. Background technique [0002] Research on low surface energy materials as antifouling coatings is becoming more and more popular. Polydimethylsiloxane-b-polymethyl methacrylate-b-polyheptafluorobutyl methacrylate is a new type of fluorosilicon triblock with microphase separation structure and low surface energy Copolymer, which has not been repor...

Claims

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Application Information

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IPC IPC(8): C08F293/00
Inventor 罗正鸿何腾云戴李宗
Owner XIAMEN UNIV
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