Method for preparing flame retardant tris[2-tri(chloroethoxy)silicon-acyloxy-ethyl]isocyanurate

A technology of silyloxyethyl and isocyanurate, which is applied in the direction of silicon organic compounds, can solve problems such as threats to people's life and property safety, fire, etc., to overcome the volatile reaction, low production cost, and flame-retardant performance high 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] The consumption of organic polymer synthetic materials has become one of the important indicators to measure whether a country or region is developed; however, most polymer materials are flammable and often cause fires, which pose a serious threat to people's lives and property. There is a strong social urgency for flame retardant materials, thus promoting the development of flame retardant materials and flame retardant technology

Method used

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  • Method for preparing flame retardant tris[2-tri(chloroethoxy)silicon-acyloxy-ethyl]isocyanurate
  • Method for preparing flame retardant tris[2-tri(chloroethoxy)silicon-acyloxy-ethyl]isocyanurate
  • Method for preparing flame retardant tris[2-tri(chloroethoxy)silicon-acyloxy-ethyl]isocyanurate

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 a drying tube on the upper mouth of the condenser, replace the air in the bottle with nitrogen, add 20ml of dichloroethane and 8.5 g (5.67ml, 0.05mol) of silicon tetrachloride, under stirring, cooled with a cold water bath to reduce the temperature of the reaction system to below 20°C, add 4.025g (3.35ml, 0.05mol) of chloroethanol dropwise, and the dropwise addition process is controlled The reaction temperature is not higher than 30°C. After dropping, raise the temperature to 35°C, and keep it warm for 1 hour; after the HCl gas is released, dissolve 4.358g (0.0167mol) Cycla in 50ml dichloroethane dropwise into the tetrachloride In the flask, the reaction temperature was controlled at a rate of addition not higher than 60°C. After the drop, the temperature was raised to 80°C, and the reaction was carried out for 9 hours; , 0.105mol) chloroethanol, the ...

Embodiment 2

[0030]Example 2 In a 250ml four-necked flask equipped with a stirrer, a thermometer and a high-efficiency reflux condensing tube, and a drying tube on the condensing tube, replace the air in the bottle with nitrogen, and add 20ml of dioxane and 8.5 g (5.67ml, 0.05mol) of silicon tetrachloride, under stirring, cooled with a cold water bath to reduce the temperature of the reaction system to below 20°C, add 4.025g (3.35ml, 0.05mol) of chloroethanol dropwise, and the dropwise addition process is controlled The reaction temperature is not higher than 30°C. After dripping, raise the temperature to 35°C, and keep it warm for 1 hour; after the HCl gas is released, dissolve 4.358g (0.0167mol) Cycla in 50ml of dioxane dropwise into the four In the flask, the reaction temperature was controlled by the dropping rate to not be higher than 60°C. After the drop, the temperature was raised to 85°C, and the reaction was carried out for 7 hours; , 0.11mol) chloroethanol, the reaction temperatu...

Embodiment 3

[0031] Embodiment 3 In the 250ml four-necked flask that stirrer, thermometer and high-efficiency reflux condenser are equipped with, and drying tube is housed on the condenser upper mouth, replace the air in the bottle with nitrogen, add 20ml acetonitrile and 8.5g (5.67 ml, 0.05mol) of silicon tetrachloride, under stirring, cooled with a cold water bath, the temperature of the reaction system was reduced to below 20°C, and 4.025g (3.35ml, 0.05mol) of chloroethanol was added dropwise, and the reaction temperature was controlled during the dropwise addition process. If the temperature is higher than 30°C, after dropping, raise the temperature to 35°C, and keep it warm for 1 hour; after the HCl gas is released, drop 4.358g (0.0167mol) of Cycla in 50ml of acetonitrile into the four-necked flask to drip Acceleration controls the reaction temperature not to be higher than 60°C. After dropping, raise the temperature to 80°C and react for 8 hours; after the HCl gas is released, cool th...

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Abstract

The invention relates to a method for preparing a flame retardant tris[2-tri(chloroethoxy)silicon-acyloxy-ethyl]isocyanurate. The structure of the compound is represented by a formula shown in a drawing. The preparation method comprises the steps of reacting silicon tetrachloride with chloroethanol of a mole which is equal to that of silicon tetrachloride in an organic solvent at the temperature below 20 DEG C, then, dropwise adding an organic solution of trishydroxyethyl isocyanurate of a mole which is 1/3 that of silicon tetrachloride, heating to the temperature of 75-85 DEG C after completing dripping, and reacting for 7-10 hours; then, dropwise adding chloroethanol of a mole which is 2-3 times that of silicon tetrachloride, and carrying out heat-preservation reaction for 6-8 hours at the temperature of 75-85 DEG C; then, adding an acid binding agent, and carrying out heat preservation for 1 hour while stirring; purifying, thereby obtaining the flame retardant tris[2-tri(chloroethoxy)silicon-acyloxy-ethyl]isocyanurate. The compound disclosed by the invention has high flame retarding efficacy and is suitable for serving as a flame retardant for materials, such as polyvinyl chloride, polyurethane, epoxy resin, unsaturated resin and the like, and the preparation method is simple and is low in cost, so that the industrial production is easy to realize.

Description

technical field [0001] The invention relates to a method for preparing a flame retardant tris[2-tris(chloroethoxy)silyloxyethyl]isocyanurate, which can be used as polyvinyl chloride, unsaturated polyester, polyurethane and Flame retardant for materials such as epoxy resins. Background technique [0002] The consumption of organic polymer synthetic materials has become one of the important indicators to measure whether a country or region is developed; however, most polymer materials are flammable and often cause fires, which pose a serious threat to people's lives and property. There is a strong social urgency for flame retardant materials, thus promoting 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 forward for halogenated flame retardants in recent years, that is, they are developing in the direction of high efficiency...

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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