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Polysiloxane low polymer with side epoxy group and preparation method thereof

A kind of technology of phenyltrialkoxysilane and polysiloxane

Inactive Publication Date: 2013-11-13
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Patent CN201010115028.1 adopts the method of hydrolysis and polycondensation of silane monomers containing epoxy groups or hydrolysis and co-condensation with other silane monomers to prepare polysiloxane with epoxy groups, but in this method, silane monomers are under acidic and alkaline conditions. Under hydrolysis and polycondensation, its epoxy group will produce a serious ring-opening reaction

Method used

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  • Polysiloxane low polymer with side epoxy group and preparation method thereof
  • Polysiloxane low polymer with side epoxy group and preparation method thereof
  • Polysiloxane low polymer with side epoxy group and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Step 1. Add 0.08mol γ-chloropropylmethyldimethoxysilane, 0.1mol phenyltriethoxysilane, 116g Toluene, heat the reaction system to 85°C, add 17.5g of dilute hydrochloric acid with a mass fraction of 7% dropwise, after reacting for 5 hours, add 0.0108mol trimethylchlorosilane, continue the reaction for 3 hours, remove the water layer after cooling, and wash with saturated sodium sulfate Wash the toluene layer with an aqueous solution to neutrality to obtain a polychloropropylphenylsiloxane toluene solution, which is completely transferred to a 250ml four-neck flask equipped with a stirrer, a reflux condenser, a thermometer, and a dropping funnel;

[0025] Step 2, in another 250ml four-necked flask equipped with stirrer, reflux condenser, thermometer, feed N 2 , add 0.07mol bisphenol A, 0.14mol sodium hydroxide and 90g deionized water, heat up to 90°C, reflux reaction for 1.5h under stirring, and obtain bisphenol A sodium salt solution after cooling; the prepared bisphenol ...

Embodiment 2

[0031]Step 1. Add 0.02mol γ-chloropropylmethyldiethoxysilane, 0.1mol phenyltrimethoxysilane, and 96g toluene to a 250ml four-neck flask equipped with a stirrer, reflux condenser, thermometer, and dropping funnel , heat the reaction system to 85°C, add 14.4g of dilute hydrochloric acid with a mass fraction of 5% dropwise, and react for 8 hours, add 0.012mol hexamethyldisiloxane, continue the reaction for 3 hours, remove the water layer after cooling, and wash with saturated sulfuric acid Wash the toluene layer with sodium aqueous solution to neutrality to obtain a polychloropropylphenylsiloxane toluene solution, which is all transferred to a 250ml four-necked flask equipped with a stirrer, a reflux condenser, a thermometer, and a dropping funnel;

[0032] Step 2, in another 250ml four-necked flask equipped with stirrer, reflux condenser, thermometer, feed N 2 , add 0.02mol bisphenol A, 0.06mol potassium hydroxide and 81g deionized water, heat up to 80°C, reflux reaction for 1h ...

Embodiment 3

[0037] Step 1. Add 0.05mol γ-chloropropylmethyldiethoxysilane, 0.1mol phenyltrimethoxysilane, and 91g toluene to a 250ml four-neck flask equipped with a stirrer, reflux condenser, thermometer, and dropping funnel , heat the reaction system to 90°C, add 12.1 g of dilute hydrochloric acid with a mass fraction of 7% dropwise, and after reacting for 6 hours, add 0.003 mol of hexamethyldisiloxane, continue the reaction for 4 hours, remove the water layer after cooling, and wash with saturated sulfuric acid Wash the toluene layer with sodium aqueous solution to neutrality to obtain a polychloropropylphenylsiloxane toluene solution, which is all transferred to a 250ml four-necked flask equipped with a stirrer, a reflux condenser, a thermometer, and a dropping funnel;

[0038] Step 2, in another four-necked flask equipped with stirrer, reflux condenser, thermometer, add and feed N 2 , 0.05mol bisphenol A, 0.1mol sodium hydroxide and 108g deionized water, heated up to 100°C, reflux rea...

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Abstract

The invention discloses a polysiloxane low polymer with a side epoxy group and a preparation method thereof. The method comprises the steps of: firstly mixing gamma-chloropropyl methyl dialkoxysilane and phenyl trialkoxysilane with methylbenzene, heating to 85-90 DEG C, dropping diluted hydrochloric acid for reaction for 5-8h, adding end-capping agent for continuous reaction and cooling to obtain polychloropropyl phenylsilane methylbenzene solution; then bisphenol A sodium salt or kali salt solution into the polychloropropyl phenylsilane methylbenzene solution, adding phase transfer catalysts and heating for reaction for 4-6h; and adding epoxy chloropropane for reaction, cooling, separating, removing water layers and methylbenzene and drying in vacuum to obtain the polysiloxane low polymer with the side epoxy group. The polysiloxane low polymer with the side epoxy group has a good thermal and oxidative stability, is flame-retardant, can be used as compatilizer for the blending systems of high-molecular materials, can introduce the high-temperature and low-temperature resistance, the flame retardance and the like of polysiloxane structures and is adaptive to comparatively high processing temperature.

Description

technical field [0001] The invention relates to a polysiloxane oligomer with epoxy groups in side groups and a preparation method thereof. Background technique [0002] The main chain of organopolysiloxane is composed of Si-O-Si bonds, which has good high and low temperature resistance, flame retardancy, weather resistance, biocompatibility, etc., the proportion of silicon and oxygen in the molecular structure, the type of side group, and the molecular weight etc. will greatly affect its performance. Polysiloxanes with epoxy groups in side groups have high reactivity, and can be used as reaction intermediates through the reaction of epoxy groups with amine groups, alcoholic hydroxyl groups, phenolic hydroxyl groups, carboxyl groups, thiol groups, etc. The reactivity of the group is used as a compatibilizer for the blend system of polar polymer materials. General-purpose polymer compatibilizers such as ethylene-butyl acrylate-glycidyl methacrylate copolymer (PTW) and ethyle...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/08C08G77/14C08K5/5435C08L83/06
Inventor 刘述梅杨燕赵建青赵颖
Owner SOUTH CHINA UNIV OF TECH
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