Novel tri(dichloropropyl) bisilicate flame retardant compound containing bromine and preparation method thereof

A technology of dichloropropyl and dichloropropoxy disilicate tri-silicate, which is applied in the field of new-type bromine-containing disilicate triester flame retardant compound and its preparation, can solve problems such as difficulty in finding substitutes, and achieve cheap raw materials , Good compatibility, and easy-to-obtain raw materials

Active Publication Date: 2012-10-17
SUZHOU UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the European Union announced in 1986 that polybrominated diphenyl ether flame retardants produced carcinogen dioxins when burned, the use of halogenated flame retardants has been restricted. However, due to the excellent overall cost performance of halogenated flame retardants, it is difficult to find suitable Therefore, research and development of high-efficiency halogenated flame retardants to reduce the amount of flame retardants and reduce their toxicity has become an important research direction for halogenated flame retardants

Method used

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  • Novel tri(dichloropropyl) bisilicate flame retardant compound containing bromine and preparation method thereof
  • Novel tri(dichloropropyl) bisilicate flame retardant compound containing bromine and preparation method thereof
  • Novel tri(dichloropropyl) bisilicate flame retardant compound containing bromine and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Example 1 In a 100ml four-neck flask equipped with a stirrer, a thermometer, and a high-efficiency reflux condenser, add 10ml of diethylene glycol dimethyl ether, and then add 6.8g of silicon tetrachloride (4.54ml, 0.04mol), at 25 Under the condition of ℃, a solution of 13.12g (0.02mol) tetrabromobisphenol A diglycidyl ether dissolved in 40ml of diethylene glycol dimethyl ether was dropped into silicon tetrachloride within 50min, and During the addition process, use an ice-water bath to control the temperature not higher than 50°C. After the dropwise addition, raise the temperature to 80°C within 30 minutes and keep it warm for 3 hours; then cool down to 25°C and add 16.77g (0.13mol) of 2,3-dichloropropanol dropwise , use a cold water bath and drop rate to control the reaction temperature not higher than 50°C. After the drop is completed, the temperature will be raised to 70°C within 1 hour, and the reaction will be carried out for 6 hours. , N-dimethylaniline acid-bind...

Embodiment 2

[0035] Example 2 In a 100ml four-necked flask equipped with a stirrer, a thermometer, and a high-efficiency reflux condenser, add 10ml of toluene, then add 6.8g of silicon tetrachloride (4.54ml, 0.04mol), and at 25°C, the A solution of 13.12g (0.02mol) tetrabromobisphenol A diglycidyl ether dissolved in 40ml of toluene was dropped into silicon tetrachloride within 50 minutes, and the temperature was controlled not higher than 50°C with an ice-water bath during the dropping process , after the dropwise addition, the temperature was raised to 80°C within 30min, and the temperature was kept for 3h; then the temperature was lowered to 25°C, and 15.48g (0.12mol) of 2,3-dichloropropanol was added dropwise, and the reaction temperature was controlled by a cold water bath and a drop rate. At 50°C, after dripping, raise the temperature to 100°C within 1 hour, and react for 4 hours. After the hydrogen chloride is released, the reaction ends, drop the temperature to 50°C and add about 1ml...

Embodiment 3

[0036] Example 3 In a 100ml four-neck flask equipped with a stirrer, a thermometer, and a high-efficiency reflux condenser, add 10ml of dichloroethane, and then add 6.8g (4.54ml, 0.04mol) of silicon tetrachloride. , a solution of 13.12g (0.02mol) tetrabromobisphenol A diglycidyl ether dissolved in 40ml dichloroethane was dropped into silicon tetrachloride within 50min, and the dropping process was controlled by an ice-water bath The temperature is not higher than 50°C. After the dropwise addition is completed, the temperature is raised to 70°C within 30 minutes and kept for 4 hours; then the temperature is lowered to 25°C, and 16.77g (0.13mol) of 2,3-dichloropropanol is added dropwise. Acceleration controls the reaction temperature not to be higher than 50°C. After dripping, raise the temperature to 80°C within 1 hour, and react for 5 hours. After the hydrogen chloride is released, the reaction ends, and the temperature is lowered to 50°C. Add about 1g of melamine acid-binding ...

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Abstract

The invention relates to a silicon halide three elements synergized flame retarding plasticizer tetrabromo bisphenol A diether dichloropropoxy tri(2,3-dichloropropyl) bisilicate compound and a preparation method thereof. The structure of the compound is shown in the following formula, wherein when m is equal to 0, n is equal to 1; when m is equal to 1, n is equal to 0; x is equal to 0, 1, 2 or 3. The preparation method comprises the following steps: tetrabromo bisphenol A diglycidyl ether is dissolved in organic solvent while being mixed; the obtained solution is dripped in silicon tetrachloride at 25 DEG C, then reacted for 3-4h at 70-80 DEG C in heat preservation, and added with dichloropropanol with a certain mol ratio to react for 4-6h at 70-100 DEG C, at last the solution is purified to obtain the product tetrabromo bisphenol A diether dichloropropoxy tri(2,3-dichloropropyl) bisilicate. The product is an excellent flame retarding plasticizer, and suitable to be used as flame retarding plasticizer additive for epoxy resin, polyvinyl chloride, unsaturated resin, polyurethane, and the like.

Description

technical field [0001] The present invention relates to a novel bromine-containing disilicate tris(dichloropropyl) ester flame retardant compound and a preparation method thereof, in particular to a tetrabromobisphenol A diether dichloropropoxy disilicate tris( Dichloropropyl) ester compound and preparation method thereof, the compound contains three flame retardant elements of silicon, bromine and chlorine in the same molecule, which can exert a synergistic flame retardant synergistic effect and high flame retardant efficiency; its ether ester structure and material It has good compatibility and good plasticity, and is an excellent flame-retardant plasticizer. It is suitable as a flame-retardant plasticizer for epoxy resin, polyvinyl chloride, unsaturated resin, polyurethane, etc. Background technique [0002] With the rapid development of the world economy, the continuous improvement of people's living standards and the enhancement of safety awareness, the flame retardant ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K5/5415C08L27/06
Inventor 王彦林韩志慧顾凤楼
Owner SUZHOU UNIV OF SCI & TECH
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