Method for preparing fluorine-silicon triblock copolymer by employing one-kettle process

A tri-block, polymer technology, applied in biocide-containing paints, coatings, antifouling/underwater coatings, etc., to achieve the effect of less reaction steps, high conversion rate, and avoiding the steps of catalyst removal

Inactive Publication Date: 2014-07-09
SKSHU PAINT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The common ATRP method has many problems in industrialization

Method used

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  • Method for preparing fluorine-silicon triblock copolymer by employing one-kettle process
  • Method for preparing fluorine-silicon triblock copolymer by employing one-kettle process
  • Method for preparing fluorine-silicon triblock copolymer by employing one-kettle process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Add 1 mol of macroinitiator PDMS-Br, 100 mol of toluene, 100 mol of methyl methacrylate (MMA), 0.005 mol of copper bromide, 0.02 mol of ligand PMDETA and 0.05 mol of stannous octoate into the reaction flask, and feed nitrogen For 10 minutes, heat to 60°C. Stir under the closed system, when the monomer conversion rate reaches 85%, slowly add the mixture of 100mol heptafluorobutyl methacrylate (HFBMA) and 0.05mol stannous octoate diluted with 100mol toluene to the reaction flask, feed nitrogen gas for 10 Minutes, heated to 60°C, reacted in a closed system, and when the monomer conversion rate reached 85%, stirred in the open, and the main component of the obtained product was the triblock polymer PDMS-b-PMMA-b-PHFBMA-Br.

Embodiment 2

[0030]Add 1mol of macromolecular initiator PDMS-Br, 250mol of xylene, 250mol of methyl methacrylate (MMA), 0.05mol of nickel bromide, 0.4mol of ligand TPMA and 0.5mol of glucose into the reaction flask, and feed nitrogen gas for 30 Minutes, heated to 80°C. Stir in a closed system, and when the monomer conversion rate reaches 90%, slowly add a mixture of 250 mol of heptafluorobutyl methacrylate (HFBMA) diluted with 250 mol of xylene and 0.5 mol of glucose into the reaction flask, and feed nitrogen for 30 minutes , heated to 80°C, and reacted in a closed system. When the monomer conversion rate reached 90%, it was stirred openly, and the main component of the obtained product was the triblock polymer PDMS-b-PMMA-b-PHFBMA-Br.

Embodiment 3

[0032] 1mol macroinitiator PDMS-Br, 500mol anisole, 500mol methyl methacrylate (MMA), 0.1mol iron bromide, 0.8mol ligand Me 6 Add TREN and 1mol ascorbic acid together into the reaction flask, pass through nitrogen for 60 minutes, and heat to 95°C. Stir in a closed system, and when the monomer conversion rate reaches 95%, slowly add a mixture of 500 mol of heptafluorobutyl methacrylate (HFBMA) and 1 mol of ascorbic acid diluted with 500 mol of anisole into the reaction flask, and feed nitrogen for 60 minutes , heated to 95°C, and reacted in a closed system when the monomer conversion rate reaches 95%, and stirred with the open door, the main component of the obtained product is the triblock polymer PDMS-b-PMMA-b-PHFBMA-Br.

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Abstract

The invention belongs to the technical field of high-molecular chemical synthesis, and specifically relates to a method for preparing a fluorine-silicon triblock copolymer by employing a one-kettle process. The reaction is controlled by employing an electron transfer regeneration activator and atom transfer free radical polymerization, the concentration of a metal catalyst in the system is extremely low, side reactions between free radicals and the catalyst and between free radicals and free radicals are effectively inhibited and reduced, and the activity of terminal groups is relatively well kept. A macro-molecule initiator is taken as a first chain segment, a monomer and a reducing agent are added, when the conversion rate of the monomer is relatively high, a second monomer and a reducing agent are added, so that the triblock copolymer is prepared by employing the one-kettle process. The preparation method for the fluorine-silicon triblock copolymer by employing the one-kettle process is low in required catalyst concentration, mild in reaction conditions, simple in operation steps and suitable for industrialization, and has important meaning on preparation of efficient ocean anti-fouling paint, improving of ocean fishery and even enhancement of naval capability.

Description

technical field [0001] The invention belongs to the technical field of macromolecule chemical synthesis, and in particular relates to a kind of one-pot multi-step regenerated activator-atom transfer radical polymerization (Activators regenerated by electron transfer atom transfer radical polymerization, ARGET ATRP) under low catalyst concentration A method for preparing a base material of fluorosilicon coating-fluorosilicon triblock polymer polydimethylsiloxane-b-polymethyl methacrylate-b-polyheptafluorobutyl methacrylate. Background technique [0002] Marine biofouling poses enormous challenges to ships and marine equipment. Seaweed, lime worms and other marine organisms adhere to the hull and propeller, which will increase the weight of the hull and the frictional resistance of driving, resulting in reduced speed and increased energy consumption. According to literature reports, attachments can increase frictional resistance by 0.25-5% per day. An ocean-going freighter o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F293/00C08F220/14C08F220/22C09D153/00C09D5/16
Inventor 洪杰魏川叶映林
Owner SKSHU PAINT
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