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Silicon-acrylic tri-block copolymer with low surface energy and preparing method thereof

A silicon-acrylic triblock and block copolymer technology, which is applied in the field of silicon-acrylic tri-block copolymers with low surface energy and its preparation, can solve the problem of many side reactions of anionic polymerization, difficulty in separation and purification, and inability to contain oxygen And water and other problems, to achieve the effect of narrow molecular weight distribution, less side reactions, and low surface energy

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, Therefore, there is a high demand for purification
2. There are many anionic polymerization side reactions of acrylates, and it is difficult to separate and purify after the reaction

Method used

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  • Silicon-acrylic tri-block copolymer with low surface energy and preparing method thereof
  • Silicon-acrylic tri-block copolymer with low surface energy and preparing method thereof
  • Silicon-acrylic tri-block copolymer with low surface energy and preparing method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0023] 1) Under the protection of a nitrogen atmosphere, 1 part of monomethanol-terminated polydimethylsiloxane, 1.5 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 30 hours. After the reaction, it was filtered, the filtrate was distilled under reduced pressure to remove the solvent, and the filtrate was 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;

[0024] 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 mo...

Embodiment 2

[0027]1) Under the protection of argon atmosphere, 1 part of monomethanol-terminated polydimethylsiloxane, 4.0 parts of 2-bromoisobutyryl bromide and 5.5 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;

[0028] 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;

[0029] 3) Except that the reaction temperature is 60°C, the others are the same as step 3) in E...

Embodiment 3

[0031] 1) Except that the reaction temperature is 15h, everything else is the same as step 1) in Example 1;

[0032] 2) Except that the monomer is 30 parts, the others are the same as step 2) in Example 2;

[0033] 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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Abstract

The invention relates to a silicon-acrylic three-block copolymer with low surface energy and a process for preparation, which relates to the synthesis of silicon-acrylic low-surface-energy three-block copolymer. The invention provides a silicon-acrylic three-block copolymer with low surface energy, whose structure of reaction product is accurate, and the original skeleton construction of each block is kept. The invention relates to a dimethyl silicone polymer-b- polymethyl methacryate-b-poly n-butyl methacrylate. And the process for preparation comprises first, preparing dimethyl silicone polymer macromolecule initiating agent of the dead ends of bromine atoms, second, preparing two-block macromolecule initiating agent of copolymer dimethyl silicone polymer-b-polymethyl methacryate, third, preparing two-block copolymer macromolecule initiating agent of dimethyl silicone polymer-b- polymethyl methacryate, finally, preparing three-block novel copolymer of dimethyl silicone polymer-b- polymethyl methacryate-b-poly n-butyl methacrylate.

Description

Technical field [0001] The invention relates to the synthesis of a silicon-acrylic low-surface-energy triblock copolymer, in particular to a polydimethylsiloxane synthesized by atom transfer radical polymerization by using macromolecular polydimethylsiloxane as an initiator Oxyane-b-polymethyl methacrylate diblock copolymer, and then use the diblock copolymer as a macroinitiator to initiate polymerization of butyl methacrylate monomer to synthesize the target polymer polydimethylsiloxane The preparation method of -b-polymethyl methacrylate-b-polybutyl methacrylate. 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. In the polymerization process, attention must be paid to the use of polydimethylsiloxane. The alkane block initiates the polymerization of acrylic monomers, and vice versa. Acrylic resin has excellent heat resistance, we...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F293/00
Inventor 罗正鸿何腾云
Owner XIAMEN UNIV
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