Flame retardant tris(hydroxyethyl) isocyanurate trisilicate ethyl chloride compound and preparation method thereof

A technology of flame retardant and compound, which is applied in the field of flame retardant chloroethyl trisilicate trisilicate compound and its preparation, can solve problems such as threats to people's life and property safety, fire, etc., and achieve good application and development prospects and production costs Low, low volatility effect

Active Publication Date: 2014-02-05
SHANDONG XINGQIANG CHEM IND TECH RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] With the rapid development of science and technology, the consumption of organic polymer synthetic materials has become an important indicator to measure the development of a country or region, but most polymer materials are flammable and often cause fires, causing serious damage to people's lives and property. Serious threat, thus promoting the development of flame retardant materials and flame retardant technology

Method used

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  • Flame retardant tris(hydroxyethyl) isocyanurate trisilicate ethyl chloride compound and preparation method thereof
  • Flame retardant tris(hydroxyethyl) isocyanurate trisilicate ethyl chloride compound and preparation method thereof
  • Flame retardant tris(hydroxyethyl) isocyanurate trisilicate ethyl chloride compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Example 1 In a 250ml four-neck flask equipped with a stirrer, a thermometer and a high-efficiency reflux condenser, and an extremely expandable sealing sleeve is installed on the upper mouth of the condenser, replace the air in the bottle with nitrogen, and add 20ml of dioxane ring and 8.5g (5.67ml, 0.05mol) of silicon tetrachloride, under stirring, cooled with an ice-water bath, the temperature of the reaction system was reduced to 0°C, and 4.4g (5.05ml, 0.1mol) of epoxy Ethane is introduced into the process to control the reaction temperature not higher than 20°C. After the addition, the temperature is raised to 30°C, and the heat preservation reaction is carried out for 1 hour; then, the upper port of the reflux condenser tube is replaced with a drying tube, and 4.358g (0.0167mol) of Saike The solution dissolved in 50ml of dioxane was dripped into the four-necked flask, and the reaction temperature was controlled by the dropping rate not higher than 65°C. After the dr...

Embodiment 2

[0030]Example 2 In a 250ml four-necked flask equipped with an agitator, a thermometer and a high-efficiency reflux condenser, and an extremely expandable sealing sleeve on the upper mouth of the condenser, replace the air in the bottle with nitrogen, and add 20ml of dichloroethylene Alkanes and 8.5g (5.67ml, 0.05mol) silicon tetrachloride, under stirring, cool with ice-water bath, make the reaction system temperature drop to 0 ℃, pass into 4.4g (5.05ml, 0.1mol) epoxy resin under the liquid surface Ethane is introduced into the process to control the reaction temperature not higher than 20°C. After the addition, the temperature is raised to 30°C, and the heat preservation reaction is carried out for 1 hour; then, the upper port of the reflux condenser tube is replaced with a drying tube, and 4.358g (0.0167mol) of Saike The solution dissolved in 50ml of dichloroethane was dripped into the four-necked flask, and the reaction temperature was controlled by the dropping rate not to b...

Embodiment 3

[0031] Example 3 In a 250ml four-necked flask equipped with a stirrer, a thermometer and a high-efficiency reflux condenser, and an extremely expandable seal sleeve is installed at the upper mouth of the condenser, replace the air in the bottle with nitrogen, add 20ml of acetonitrile and 8.5 g (5.67ml, 0.05mol) of silicon tetrachloride, under stirring, cooled with an ice-water bath, the temperature of the reaction system was reduced to 0°C, and 4.4g (5.05ml, 0.1mol) of ethylene oxide was fed under the liquid surface, Control the reaction temperature not higher than 20°C during the feeding process. After the addition, raise the temperature to 30°C and keep it warm for 1 hour; then replace the upper port of the reflux condenser tube with a drying tube, and dissolve 4.358g (0.0167mol) Cycla in 50ml The acetonitrile solution was dropped into the four-necked flask, and the reaction temperature was controlled by the dropping speed to not be higher than 65°C. After the drop, the tempe...

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Abstract

The invention relates to a flame retardant tris(hydroxyethyl) isocyanurate trisilicate ethyl chloride compound and a preparation method thereof. The compound has a structure shown in the specification. The preparation method comprises the following steps: introducing ethylene oxide into an organic solution of the silicon tetrachloride at a temperature being below 0 DEG C and reacting for 1 hour at 30 DEG C, wherein the molar mass of the ethylene oxide is 2 times that of the silicon tetrachloride; dropwise adding an organic solution of tris(hydroxyethyl) isocyanurate and reacting for 7-10 hours at 70-85 DEG C, wherein the molar mass of the organic solution of tris(hydroxyethyl) isocyanurate is 1 / 3 that of the silicon tetrachloride; cooling to the temperature being below 30 DEG C, introducing the ethylene oxide and reacting for 3-6 hours at 35-50 DEG C, wherein the molar mass of the ethylene oxide is 1-1.5 times that of the silicon tetrachloride; performing purification to obtain the tris(hydroxyethyl) isocyanurate trisilicate ethyl chloride. The compound disclosed by the invention is suitable to be used as flame retardants of the materials such as polyvinyl chloride, polyurethane, epoxy resin and unsaturated resin, is high in synergistic flame retardant performance, simple in preparation process and low in cost, and can be put into industrial production easily.

Description

technical field [0001] The present invention relates to a flame retardant chloroethyl trisilicate compound and a preparation method thereof, in particular to a flame retardant tris[2-tris(chloroethoxy)silyloxyethyl]isocyanurate An ester compound and a preparation method thereof, the compound can be used as a flame retardant for materials such as polyvinyl chloride, unsaturated polyester, polyurethane and epoxy resin. Background technique [0002] With the rapid development of science and technology, the consumption of organic polymer synthetic materials has become an important indicator to measure the development of a country or region, but most polymer materials are flammable and often cause fires, causing serious damage to people's lives and property. Therefore, it promotes the development of flame retardant materials and flame retardant technology. With the continuous enhancement of people's awareness of environmental protection, more stringent requirements have been put...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/04C08K5/5455C08L27/06C08L67/06C08L75/04C08L63/00
Inventor 王彦林董信
Owner SHANDONG XINGQIANG CHEM IND TECH RES INST CO LTD
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