Fluorine-silicon segmented copolymer modified inorganic material and preparation method thereof

A technology of copolymer modification and inorganic materials, which is applied in the field of technical materials to achieve the effects of reducing dead polymerization, mild reaction conditions and reducing costs

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

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Problems solved by technology

Such a large amount of transition metals...

Method used

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  • Fluorine-silicon segmented copolymer modified inorganic material and preparation method thereof
  • Fluorine-silicon segmented copolymer modified inorganic material and preparation method thereof
  • Fluorine-silicon segmented copolymer modified inorganic material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Step 1: Preparation of Silane Coupling Agent Modified Silica

[0041] Add 1 mol of silica, 5 mol of silane coupling agent and 100 mol of toluene into the container, reflux for 1 hour, centrifuge to separate silica, and wash with toluene several times to obtain silica modified by silane coupling agent;

[0042] Step 2: Preparation of silica with initiator on its surface

[0043] Add 1 mol of silane coupling agent modified silica on the surface and 1.1 mol of pyridine to 1 mol of toluene and stir at low temperature, then slowly drop 1.1 mol of 2-bromoisobutyryl bromide diluted with 1 mol of toluene. After 1 hour, return the system to room temperature, continue to stir for 1 hour, centrifuge, and wash with a solvent several times, and dry to obtain silica with initiator sites on the surface; the solvent is tetrahydrofuran, dichloromethane, tris Any one of methyl chloride, benzene, toluene, and xylene inert solvents;

[0044] Step 3: Preparation of poly-3-methacryloxyprop...

Embodiment 2

[0049] Step 1: Preparation of Silane Coupling Agent Modified Silica

[0050] Add 1 mol of silica, 10 mol of silane coupling agent and 500 mol of toluene into the container, reflux for 24 hours, centrifuge to separate silica, and wash with toluene several times to obtain silica modified by silane coupling agent;

[0051] Step 2: Preparation of silica with initiator sites on the surface

[0052] Add 1 mol of silane coupling agent on the surface of modified silica and 10 mol of pyridine to 100 mol of toluene and stir at low temperature, then slowly drop 10 mol of 2-bromoisobutyryl bromide diluted with 100 mol of toluene. After 3 hours, the system was returned to room temperature, continued to stir for 24 hours, centrifuged, and washed with a solvent for several times, and dried to obtain silica with initiator sites on the surface; the solvents were tetrahydrofuran, dichloromethane, tris Any one of methyl chloride, benzene, toluene, and xylene inert solvents;

[0053] Step 3: Pr...

Embodiment 3

[0058] Step 1: Preparation of Silane Coupling Agent Modified Silica

[0059] Add 1 mol of silica, 8 mol of silane coupling agent and 300 mol of toluene into the container, reflux for 12 hours, centrifuge to separate the silica, and wash with toluene several times to obtain silica modified by silane coupling agent;

[0060] Step 2: Preparation of silica with initiator sites on the surface

[0061] Add 1 mol of silane coupling agent modified silica on the surface and 1.1 mol of pyridine to 1 mol of toluene and stir at low temperature, then slowly drop 1.1 mol of 2-bromoisobutyryl bromide diluted with 1 mol of toluene. After 1 hour, return the system to room temperature, continue to stir for 1 hour, centrifuge, and wash with a solvent several times, and dry to obtain silica with initiator sites on the surface; the solvent is tetrahydrofuran, dichloromethane, tris Any one of methyl chloride, benzene, toluene, and xylene inert solvents;

[0062] Step 3: Preparation of poly-3-meth...

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Abstract

The invention specifically relates to a method for preparing a fluorine-silicon segmented copolymer modified inorganic material through surface-initiated activators regenerated by electron transfer-atom transfer radical polymerization under the condition of a low catalyst concentration, belonging to the field of technical materials. According to the invention, a silane coupling agent and a chemical reagent containing an initiator site are respectively used to treat an inorganic material, and an initiator is modified on the surface of the material; then surface-initiated activators regenerated by electron transfer-atom transfer radical polymerization is employed for successive initiation of polymerization the two monomers consisting of 3-methacryloxypropyltrimethoxylsilane and heptafluorobutyl methacrylate so as to prepare the fluorine-silicon segmented copolymer modified inorganic material. The method uses a weak reducing agent to continuously reduce a passivating agent in a system, generates an activator, catalyzes atom transfer radical polymerization of the monomers, consumes a small amount of oxygen hard to thoroughly remove in the system in situ, substantially reduces the amount of a catalyst used in a polymerization system and shortens time needed for subsequent purification operation.

Description

technical field [0001] The invention belongs to the field of technical materials, and in particular relates to the preparation of fluorine by surface initiated activators regenerated by electron transfer atom transfer radical polymerization (SI-ARGET ATRP) at a low catalyst concentration. Method for modifying inorganic materials with silicon block polymers. Background technique [0002] Fluorosilicone coatings have excellent hydrophobic properties, corrosion resistance, and aging resistance, and have broad application prospects in industry. Poly-3-methacryloxypropyltrimethoxysilane-b-polyheptafluorobutyl methacrylate (PMPTS-b-PHFBMA) is a recently studied fluorosilicone block polymer with fluorine coating and the advantages of silicon coatings. (YuH.; LuoZ.; J.Polym.Sci., PartA: Polym.Chem., 2010, 48, 5570-5580; Luo Zhenghong, Yu Haijiang, Zhou Yinning; Chinese Patent Publication No.: CN101805434A). PMPTS has the heat-resistant and cold-resistant characteristics of silico...

Claims

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Application Information

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IPC IPC(8): C08F293/00C08F292/00C08F230/08C08F220/24C09D153/00
Inventor 洪杰魏川叶映林
Owner SKSHU PAINT
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