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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AI-Extracted 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 ...
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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.

Technology Topic

BromineButyl methacrylate +8

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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(12)

Example Embodiment

[0020] Example 1
[0021] 1) Under the protection of a nitrogen atmosphere, 1 part of monomethanol-terminated polydimethylsiloxane, 1.2 parts of 2-bromoisobutyryl bromide and 2.5 parts of triethylamine are reacted at 5°C. Then the above solution was stirred and reacted for 30h. After the reaction, it was filtered, the filtrate was distilled under reduced pressure to remove the solvent, and then dissolved in dichloromethane, washed with saturated sodium bicarbonate solution several times, separated, and the organic layer Dry with anhydrous magnesium sulfate to remove water, then filter, and finally distill the filtrate under reduced pressure to remove the methylene chloride solvent to obtain an oily yellow macroinitiator;
[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-pyridine methylamine as catalyst ligand React with 10 parts of methyl methacrylate as the monomer at 40°C. Before heating, the reactant solution undergoes 4 cycles of freezing-vacuum-thawing, heating the solution, and reacting for 4h, the synthesized polymer Dilute with tetrahydrofuran solvent, and then pass the diluted solution through an alumina column to remove the catalyst. Use a rotary evaporator to remove the solvent from the filtrate. When a certain concentration is reached, it is precipitated into the precipitating agent. Repeated dissolution-precipitation 4 times before obtaining The product is dried in a vacuum drying oven at 40°C (vacuum degree is 0.08Mpa) to obtain polydimethylsiloxane-b-polymethyl methacrylate copolymer.
[0023] 3) The reaction system must be strictly deoxygenated. 1 part of polydimethylsiloxane-b-polymethyl methacrylate macroinitiator, 1 part of cuprous bromide as a catalyst, 2 parts of N-( n-propyl)-2-pyridine methylamine as the catalyst ligand and 30 parts of heptafluorobutyl acrylate as the monomer react at 50°C. Before heating, the reactant solution undergoes 4 times of freezing-vacuuming-thawing After the circulation, the solution is heated and reacted for 5 hours. The synthesized polymer is diluted with tetrahydrofuran solvent. The diluted solution is passed through an alumina column to remove the catalyst. The filtrate is used to remove the solvent with a rotary evaporator. Precipitate into the precipitating agent, repeat the dissolution-precipitation 4 times, and then place the obtained product in a 50℃ vacuum drying oven (vacuum degree is 0.1MPa) to dry to obtain polydimethylsiloxane-b-polymethyl Methyl acrylate-b-polyheptafluorobutyl methacrylate triblock copolymer.

Example Embodiment

[0024] Example 2
[0025]1) Under the protection of argon atmosphere, 1 part of monomethanol-terminated polydimethylsiloxane, 1.5 parts of 2-bromoisobutyryl bromide and 2.8 parts of triethylamine are reacted at 10°C. Then the above solution was stirred and reacted for 20 hours. After the reaction, it was filtered, the filtrate was distilled under reduced pressure to remove the solvent, and then dissolved in dichloromethane, washed with saturated sodium bicarbonate solution several times, separated, and the organic layer Dry with anhydrous magnesium sulfate to remove water, then filter, and finally distill the filtrate under reduced pressure to remove the dichloromethane solvent to obtain an oily yellow macroinitiator;
[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 temperature is 60° C. and the reaction time is 15 hours, the others are the same as step 3) in Example 1.

Example Embodiment

[0028] Example 3
[0029] 1) Except that 2-bromoisobutyryl bromide is 3.6 parts and triethylamine is 4.6 parts, the others are the same as step 1) in Example 1;
[0030] 2) Except that the monomer is 30 parts, the others are the same as step 2) in Example 2;
[0031] 3) Except that the reaction temperature is 70°C and the ligand is 1,1,4,7,7-pentamethyldivinyltriamine, the others are the same as step 3) in Example 2.
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Description & Claims & Application Information

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