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Method for one-kettle preparation of fluorosilicone block polymer-modified inorganic material

An inorganic material, fluorosilicon block technology, applied in the direction of biocide-containing paints, antifouling/underwater coatings, coatings, etc., can solve the problems of increased cost and many steps, achieve high conversion rate and reduce production costs , the effect of reducing costs

Inactive Publication Date: 2014-07-23
SKSHU PAINT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are many steps in this operation process, which will greatly increase the cost during industrialization

Method used

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  • Method for one-kettle preparation of fluorosilicone block polymer-modified inorganic material
  • Method for one-kettle preparation of fluorosilicone block polymer-modified inorganic material
  • Method for one-kettle preparation of fluorosilicone block polymer-modified inorganic material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Add 1 mol of 2-bromoisobutyrate-modified silica on the surface, 0.0025 mol of copper bromide, 0.01 mol of TPMA and 50 mol of toluene into the reaction flask, blow nitrogen gas for 10 minutes, heat to 60°C, and then Add a mixture of 100mol 3-methacryloxypropyltrimethoxysilane (MPTS) and 0.025mol stannous octoate, and slowly add 100mol heptafluorobutyl methacrylate diluted with 100mol toluene when the monomer conversion rate reaches 85%. The mixture of (HFBMA) and 0.05mol stannous octoate is put into the reaction bottle, feed nitrogen for 10 minutes, heat to 60 ℃, when the closed system reacts until the monomer conversion rate reaches 85%, open and stir, the main component of the obtained product is poly 3-Methacryloxypropyltrimethoxysilane-b-polyheptafluorobutylmethacrylate modified silica.

Embodiment 2

[0036] Diatomaceous earth modified with 1mol2-bromoisobutyramide group on the surface, 0.05mol copper bromide, 0.2molMe 6 Add TREN and 250mol xylene into the reaction flask together, feed nitrogen for 30 minutes, heat to 80°C, then add 250mol 3-methacryloxypropyltrimethoxysilane (MPTS) and a mixture of 0.025-1mol ascorbic acid, When the conversion rate of the monomer reaches 90%, slowly add a mixture of 250 mol of heptafluorobutyl methacrylate (HFBMA) and 0.5 mol of ascorbic acid diluted with 250 mol of xylene into the reaction flask, feed nitrogen gas for 10 to 60 minutes, and heat to 80 ℃, react in a closed system until the conversion rate of the monomer reaches 90%, and stir in the open to obtain a product whose main component is poly-3-methacryloxypropyltrimethoxysilane-b-polyheptafluorobutyl methacrylate Modified silica.

Embodiment 3

[0038] Add montmorillonite with 1 mol of 2-bromopropionate groups on the surface, 0.1 mol of copper bromide, 0.4 mol of TPMA and 500 mol of anisole into the reaction flask, blow nitrogen gas for 60 minutes, heat to 95°C, and then Add a mixture of 500mol 3-methacryloxypropyltrimethoxysilane (MPTS) and 1mol stannous octoate, and slowly add 500mol heptafluorobutyl methacrylate diluted with 500mol anisole when the monomer conversion rate reaches 95%. Put the mixture of base ester (HFBMA) and 1mol stannous octoate into the reaction flask, feed nitrogen gas for 60 minutes, heat to 95° C., and when the closed system reacts to the monomer conversion rate reaches 95%, stir in the open to obtain the main component of the product: Poly(3-methacryloxypropyltrimethoxysilane)-b-polyheptafluorobutyl methacrylate modified silica.

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Abstract

The invention belongs to the technical field of high-molecular chemistry synthesis, and particularly relates to a method for one-kettle preparation of a fluorosilicone block polymer-modified inorganic material. Activators regenerated by electron transfer for atom transfer radical polymerization are adopted to control a reaction, the concentration of a metal catalyst in a system is extremely low, side reactions between radicals and the catalyst and between the radicals can be effectively inhibited or reduced, and end group activity is better kept. Surface functionalized inorganic particles are used as an initiator, a first monomer and a reducing agent are added, and polymerization is initiated; and when the first monomer conversion rate is relatively high, a second monomer and the reducing agent are added and one-kettle preparation of the fluorosilicone block polymer-modified inorganic material can be achieved. The invention provides the technology of one-kettle preparation of the fluorosilicone block polymer-modified inorganic material, wherein the technology has the advantages of being low in catalyst concentration, mild in reaction conditions, simple in operation steps and suitable for industrialization. At the same time, the method has important significance in preparation of high-efficiency marine antifouling coatings, improvement of marine fishery industries, and even enhancement of naval power.

Description

technical field [0001] The invention belongs to the technical field of macromolecule chemical synthesis, in particular to surface initiated activators regenerated by electron transfer atom transfer radical polymerization (SI- ARGET ATRP) technology for preparing fluorine-silicon block copolymer modified inorganic materials. Background technique [0002] Marine biofouling has brought huge economic losses to the maintenance of ships and marine equipment. Marine organisms in the pipeline will accelerate the corrosion of the shell, causing serious harm and even blockage of the pipeline. Seaweed, lime worms and other marine organisms attached to the hull and propeller will increase the weight of the hull and the frictional resistance of driving, resulting in reduced speed and increased energy consumption. [0003] According to literature reports, the antifouling paint of a speedboat was used improperly, and the attached organisms reached 17kg / m in the year of launch. 2 , the s...

Claims

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Application Information

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IPC IPC(8): C08F293/00C08F292/00C08F230/08C08F220/22C09D153/00C09D5/16
Inventor 洪杰魏川叶映林
Owner SKSHU PAINT
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