Method for synthesizing organic silicon di-block copolymers

A technology of block copolymers and synthesis methods, which is applied in the field of synthesis of silicone diblock copolymers, can solve the problems of reaction influence, high purity requirements, and the inability to contain oxygen and water, etc., and achieve mild reaction conditions and mild reactions Conditions, 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

At present, the method for synthesizing this type of polymer by anionic polymerization mainly has the following disadvantages: 1. Anionic polymerization requires high purity of the reaction system, not only the system cannot contain oxygen and water, but even other impurities have a greater impact on the reaction , so there is a high requirement for purification
2. There are many anionic polymerization side reactions of acrylates, and it is difficult to separate and purify after the reaction
[0003] Polydimethylsiloxane-b-polyethylmethacrylate is a novel low-surface-energy silicone block copolymer whose synthesis has not been reported so far

Method used

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  • Method for synthesizing organic silicon di-block copolymers
  • Method for synthesizing organic silicon di-block copolymers

Examples

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Embodiment 1

[0020] 1) Under the protection of a nitrogen atmosphere, 1 part of monomethanol-terminated polydimethylsiloxane, 1.5 parts of 2-bromoisobutyryl bromide and 2.7 parts of triethylamine are reacted at 0°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;

[0021] 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 30 parts of ethyl methacrylate as a monomer at 40°C. Bef...

Embodiment 2

[0023] 1) Under the protection of an argon atmosphere, 1 part of monomethanol-terminated polydimethylsiloxane, 1.8 parts of 2-bromoisobutyryl bromide and 3 parts of triethylamine are reacted at 5°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 twice with sodium bicarbonate solution, separated, and the organic layer Dry 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;

[0024] 2) The reaction system must strictly remove oxygen, using 1 part of macromolecule as initiator, 1 part of cuprous chloride as catalyst, and 2 parts of 1,1,4,7,7-pentamethyldivinyltriamine The catalyst ligand reacts with 40 parts of ethyl methacrylate as the monomer at 50°C. Before heating, the reac...

Embodiment 3

[0026] 1) Under the protection of a nitrogen atmosphere, 1 part of monomethanol-terminated polydimethylsiloxane, 2.5 parts of 2-bromoisobutyryl bromide and 4 parts of triethylamine are reacted at 15°C. Then, the above solution was stirred and reacted for 18 hours. After the reaction, it was filtered, the filtrate was distilled under reduced pressure to remove the solvent, and then dissolved in dichloromethane, washed twice with saturated sodium bicarbonate solution, 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;

[0027] 2) The reaction system must strictly remove oxygen, using 1 part of macromolecule as initiator, 1 part of cuprous bromide as catalyst, and 2 parts of 1,1,4,7,7-pentamethyldivinyltriamine The catalyst ligand reacts with 55 parts of ethyl methacrylate as the monomer at 70°C. Bef...

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Abstract

The invention relates to a process for synthesizing an organosilicon two-block copolymer, which relates to the synthesis of a novel organosilicon low-surface energy two-block copolymer, in particular relates to process for preparing target polymer namely dimethyl silicone polymer-b-poly ethyl methacrylate through atoms transfer and free radical polymerization under the co-catalysis of utilizing macromolecule dimethyl silicone polymer to be macromolecule initiating agent, utilizing Cu(I)Br to be catalyst and utilizing N-(n-propyl)-2-pyridine methanamine to be catalyst ligand. And the invention provides a process for synthesizing an organosilicon two-block copolymer which has the advantages of separated micro phase, moderate reaction temperature, accurate structure of reaction products, and simple operation. And the invention relates to the copolymer of dimethyl silicone polymer-b--polymethyl methacryate-b-poly seven-fluorine butyl methacrylate ester. The process for preparation comprises first preparing preparing dimethyl silicone polymer macromolecule initiator of the sealing end of bromine atom, second, preparing a novel silicon-acrylic two-block material of the dimethyl silicone polymer-b-polyethyl methacrylate.

Description

Technical field [0001] The invention relates to the synthesis of a new type of low surface energy diblock copolymer of organosilicon, in particular to a kind of macromolecular polydimethylsiloxane as a macromolecular initiator, Cu(I)Br as a catalyst, N Preparation method for synthesizing target polymer polydimethylsiloxane-b-polyethyl methacrylate through atom transfer radical polymerization reaction under the co-catalysis of -(n-propyl)-2-pyridine methylamine as catalyst ligand . Background technique [0002] Copolymers containing polydimethylsiloxane blocks and polyacrylate blocks at the same time are rarely reported. Such polymers can be synthesized by anionic polymerization, and attention must be paid to the use of polydimethylsiloxane during the polymerization process. The alkyl block initiates the polymerization of acrylic monomers, and vice versa. Acrylic resin has excellent heat resistance, weather resistance, corrosion resistance, stain resistance, high adhesion and good...

Claims

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Application Information

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IPC IPC(8): C08F293/00
Inventor 罗正鸿何腾云于海江
Owner XIAMEN UNIV
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