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Fluorine-silicon tri-block copolymer and preparation method thereof

A triblock and copolymer technology, applied in the field of technical materials, to achieve the effect of reducing side reactions, mild reaction conditions, and reducing costs

Inactive Publication Date: 2013-12-11
SKSHU PAINT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In the current literature, there is only a common ATRP method for the preparation of polydimethylsiloxane-b-polymethyl methacrylate-b-polyheptafluorobutyl methacrylate triblock polymer, which will be difficult in industrialization. have a lot of questions

Method used

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Step 1: Preparation of PDMS-Br

[0039] 1 mol of monohydroxyl-terminated polydimethylsiloxane and 1.1 mol of pyridine were added to 1 mol of toluene. 1.1 mol of 2-bromoisobutyryl bromide diluted with the same volume of toluene was slowly added dropwise at low temperature. After 1 hour, it was slowly raised to room temperature and stirred for another 1 hour. The mixture was concentrated, dissolved in dichloromethane, and washed successively with saturated aqueous sodium bicarbonate solution and sodium chloride aqueous solution. After drying the organic phase, it was concentrated and dried to obtain the product macroinitiator PDMS-Br.

[0040] Step 2: Preparation of PDMS-b-PMMA-Br (the ratio of transition metal salt to monomer is 50ppm)

[0041] Add 1 mol macroinitiator PDMS-Br, 50 mol monomer methyl methacrylate, 0.0025 mol copper bromide, 0.01 mol tris(2-pyridyl)methylamine and 50 mol toluene into the reaction flask, stir at 60°C, Then add 0.025mol stannous octoate. ...

Embodiment 2

[0045] Step 1: Preparation of PDMS-Br

[0046] Add 1 mol of monohydroxyl-terminated polydimethylsiloxane and 10 mol of pyridine to 100 mol of toluene. At low temperature, 10 mol of 2-bromoisobutyryl bromide diluted with the same volume of toluene was slowly added dropwise. After 3 hours, it was slowly raised to room temperature, and stirred for another 24 hours. The mixture was concentrated, dissolved in dichloromethane, and washed successively with saturated aqueous sodium bicarbonate solution and sodium chloride aqueous solution. After drying the organic phase, it was concentrated and dried to obtain the product macroinitiator PDMS-Br.

[0047] Step 2: Preparation of PDMS-b-PMMA-Br (the ratio of transition metal salt to monomer is 200ppm)

[0048] Add 1 mol macromolecular initiator PDMS-Br, 500 mol monomer methyl methacrylate, 0.1 mol copper bromide, 0.4 mol tris(2-pyridyl)methylamine and 500 mol toluene into the reaction flask, and pass nitrogen gas for 60 minutes, stirre...

Embodiment 3

[0052] Step 1: Preparation of PDMS-Br

[0053] Add 1 mol of monohydroxyl-terminated polydimethylsiloxane and 2 mol of triethylamine to 2 mol of toluene. 2 mol of 2-bromoisobutyryl chloride diluted with the same volume of toluene was slowly added dropwise at low temperature. After 2 hours, it was slowly raised to room temperature and stirred for another 24 hours. The mixture was concentrated, dissolved in dichloromethane, and washed successively with saturated aqueous sodium bicarbonate solution and sodium chloride aqueous solution. After drying the organic phase, it was concentrated and dried to obtain the product macroinitiator PDMS-Br.

[0054] Step 2: Preparation of PDMS-b-PMMA-Br (the ratio of transition metal salt to monomer is 100ppm)

[0055] Add 1 mol macromolecular initiator PDMS-Br, 200 mol monomer methyl methacrylate, 0.02 mol copper bromide, 0.10 mol tris(2-pyridyl)methylamine and 200 mol toluene into the reaction flask, and blow nitrogen gas for 30 minutes, stir...

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Abstract

The invention specifically relates to a method for preparing a fluorine-silicon tri-block copolymer through activators regenerated by electron transfer-atom transfer radical polymerization (ARGET ATRP) under the condition of a low catalyst concentration, belonging to the field of technical materials. According to the invention, an excess weak reducing agent is used to continuously reduce a passivating agent in a system, and an activator prepared through in-situ reaction catalyzes atom transfer radical polymerization of a monomer; in such a process, a small amount of oxygen hard to thoroughly remove in the system can be consumed in situ; the amount of a catalyst used in a polymerization system is substantially reduced at the same time; and the step of removal of copper in subsequent operation can be avoided. The preparation method for the fluorine-silicon tri-block copolymer has the advantages of a low catalyst concentration, mild reaction conditions and suitability for industrial production.

Description

technical field [0001] The invention belongs to the field of technical materials, in particular to a base for preparing a fluorosilicon coating by using an electron transfer regeneration activator-atom transfer radical polymerization (Activators regenerated by electron transfer atom transfer radical polymerization, ARGET ATRP) at a low catalyst concentration. Material—fluorosilicon triblock polymer polydimethylsiloxane-b-polymethyl methacrylate-b-polyheptafluorobutyl methacrylate. Background technique [0002] Polydimethylsiloxane-b-polymethyl methacrylate-b-polyheptafluorobutyl methacrylate is a newly developed tri-block polymer recently, as a new type with low surface energy The base material of the fluorosilicon coating has broad application prospects (LuoZ.; HeT.; YuH.; DaiL., Macromol.React.Eng., 2008, 2, 398–406; Chinese patent: Luo Zhenghong, He Tengyun, Dai Lizong, Publication number: CN101215364A). Such block polymers have several advantages. PHFBMA fluorine-cont...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F293/00C08F220/14C08F220/22C08G77/385
Inventor 洪杰魏川叶映林
Owner SKSHU PAINT
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