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Reactive organosilicon flame retardant allyl trisilyl silicate compound and preparation method thereof

A technology of allyl trisilacol silicate and allyl silicate trisilacol, which is applied in the field of reaction type organosilicon flame retardant allyl silicate trisilacol ester compound and its preparation field, It can solve the problems of escaping, decomposition and affecting material properties, and achieve the effects of good carbon formation, anti-melting and dripping, high silicon content and high flame retardant efficiency.

Active Publication Date: 2020-11-20
SUZHOU UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the more or less incompatibility between the additive flame retardant and the polymer matrix, it will be accompanied by escape and decomposition during processing, which will affect the performance of the material

Method used

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  • Reactive organosilicon flame retardant allyl trisilyl silicate compound and preparation method thereof
  • Reactive organosilicon flame retardant allyl trisilyl silicate compound and preparation method thereof
  • Reactive organosilicon flame retardant allyl trisilyl silicate compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Example 1 In a 250ml three-necked flask equipped with a stirrer, a thermometer, a reflux condenser and a drying tube and a hydrogen chloride absorption device connected to the upper mouth, 0.15mol (26.40g) pentaerythritol methylsilicate and 130ml ethylene glycol were added Diethyl ether, under the protection of nitrogen, heat up to 60℃, start to add 0.05mol (8.78g) allyltrichlorosilane dropwise, after dripping, reflux and gradually heat up to 120℃, keep the temperature for 11h, and bind acid with triethylamine The agent is adjusted to pH=6.5-8, cooled to 25°C, filtered, washed with 70ml of cold water, and dried to obtain a white solid allyl trisilicate, and its decomposition temperature: 350±5°C, density (25 ℃): 1.384g / cm 3 The yield was 85.3%.

Embodiment 2

[0031] Example 2 In a 250ml three-necked flask equipped with a stirrer, thermometer, reflux condenser and connected to the upper mouth with a drying tube and hydrogen chloride absorption device, 0.155mol (27.28g) pentaerythritol methylsilicate and 100ml tetrachloroethane were added Alkane, under the protection of nitrogen, the temperature is raised to 60℃, and 0.05mol (8.78g) allyltrichlorosilane is added dropwise. After the dripping, the reflux is gradually heated to 130℃, the temperature is kept for 12h, and the acid binding agent is adjusted to pH=6.5-8, cooling to 25°C, filtering, washing with 70ml cold water, and drying to obtain white solid trisilicosan allylsilicate. Its decomposition temperature: 350±5°C, density (25°C): 1.384g / cm 3 The yield was 89.2%.

Embodiment 3

[0032] Example 3 In a 250ml three-necked flask equipped with a stirrer, a thermometer, a reflux condenser and a drying tube and a hydrogen chloride absorption device connected to the upper mouth, 0.16mol (28.40g) pentaerythritol methylsilicate and 100ml diethylene were added Dimethyl ethoxylate, under the protection of nitrogen, heat up to 60℃, start adding 0.05mol (8.78g) allyl trichlorosilane dropwise, after dripping, reflux and gradually heat up to 140℃, keep the temperature for 13h, use triethylamine The acid binding agent is adjusted to pH=6.5-8, cooled to 25℃, filtered, washed with 70ml cold water, and dried to obtain white solid trisilicone allylsilicate. Its decomposition temperature: 350±5℃, density (25℃): 1.384g / cm 3 The yield was 92.2%.

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Abstract

The invention relates to a reactive organosilicone flame retardant allyl trisilanol silicate ester compound and a preparation method thereof. The structure of the compound is as shown in a formula. The preparation method comprises the following steps: in an organic solvent, carrying out a reaction on allyltrichlorosilane or allyltrimethoxysilane and pentaerythritol methyl silicate ester of three times in molar ratio; and carrying out purification treatment to obtain the allyl trisilanol silicate ester. The compound is high in silicon content, excellent in flame retardance, good in charcoal forming property and suitable for being used as a flame retardant charcoal forming agent made from materials such as saturated resin, styrene, acrylate, polyester, polyamide, polyurethane, epoxy resin and polyolefin. The preparation method is a one-step reaction, so that the preparation method is simple in process, less in equipment investment and easy to implement industrial production.

Description

Technical field [0001] The invention relates to a reactive organosilicon flame retardant allyl trisilicate compound and a preparation method thereof, in particular to a reactive organosilicon flame retardant allyl tris{1-methyl-1 -Sila-2,6,7-trioxabicyclo[2,2,2]octyl-(4)-methyleneoxy}silane compound and its preparation method, the compound is suitable for use as unsaturated resin, Flame retardant for styrene, acrylate, polyester, polyamide, polyurethane, epoxy resin, polyolefin and other materials. Background technique [0002] The wide application of flammable synthetic polymer materials has led to the rapid development of the flame retardant industry; with the continuous improvement of people’s living standards and the increasing awareness of safety and environmental protection, there are higher requirements for flame retardants. At the same time, more attention is paid to its safety, non-toxicity and environmental protection. The research and application of silicone flame ret...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/18C08K5/549
CPCC07F7/188C08K5/549
Inventor 刘垚曹东东王彦林
Owner SUZHOU UNIV OF SCI & TECH
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