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Silicic acid-3-(3-bromophenyl)-chloropropyl ethyl ester compound used as fire retardant and preparation method thereof

A technology of tribromophenyl and trisilicate, which is applied in the direction of silicon organic compounds, can solve the problems of restrictions, high price, and narrow application range, and achieve the effects of low production cost, convenient operation, and low equipment investment

Active Publication Date: 2013-10-02
张家港市乐余科创园投资发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Silicon-based flame retardant plasticizers have attracted people's attention due to their excellent properties of suppressing smoke and promoting carbon formation. However, general silicon-based flame retardants are limited by their high price and narrow application range.

Method used

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  • Silicic acid-3-(3-bromophenyl)-chloropropyl ethyl ester compound used as fire retardant and preparation method thereof
  • Silicic acid-3-(3-bromophenyl)-chloropropyl ethyl ester compound used as fire retardant and preparation method thereof
  • Silicic acid-3-(3-bromophenyl)-chloropropyl ethyl ester compound used as fire retardant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Embodiment 1 In the 500ml four-neck flask that stirrer, thermometer, dropping funnel and high-efficiency reflux condenser are equipped with and an extremely stretchable and expandable soft sealing sleeve is housed on the condenser upper mouth, replace the nitrogen in the bottle with nitrogen. After the air, add 100ml toluene and 8.50g (0.05mol) silicon tetrachloride, start stirring, under the cooling of ice-water bath, feed 2.20g (0.05mol) ethylene oxide under the liquid surface, control the temperature at the speed of feeding. Below 20°C, after passing through, add 49.62g (0.15mol) of tribromophenol, raise the temperature to 100°C, keep the temperature for 10 hours, after the hydrogen chloride is released, cool down to 40°C, and then add ethylene oxide under the liquid surface to remove A small amount of free acid in the reaction solution, check the pH of the reaction solution = 5 to 6 as the end point, and distill off the solvent (recycled for use) and a small amount o...

Embodiment 2

[0029] Example 2 In a 500ml four-necked flask equipped with a stirrer, a thermometer, a dropping funnel and a high-efficiency reflux condenser and an extremely flexible and expandable soft seal at the top of the condenser, replace the nitrogen in the bottle with nitrogen. After the air, add 100ml of xylene and 8.50g (0.05mol) of silicon tetrachloride, start stirring, under the cooling of ice-water bath, pass 2.20g (0.05mol) of ethylene oxide under the liquid surface, and control the temperature with the speed of entry Below 20°C, after passing through, add 49.62g (0.15mol) of tribromophenol, raise the temperature to 110°C, keep the temperature for 8 hours, after the hydrogen chloride is released, cool down to 40°C, and then pass in ethylene oxide under the liquid surface Remove a small amount of free acid in the reaction solution, check the pH of the reaction solution = 5 to 6 as the end point, and distill off the solvent (recycled for use) and a small amount of low boiling poi...

Embodiment 3

[0030] Example 3 In a 500ml four-necked flask equipped with a stirrer, a thermometer, a dropping funnel and a high-efficiency reflux condenser and an extremely flexible and expandable soft seal at the top of the condenser, replace the nitrogen in the bottle with nitrogen. After air, add 100ml of chlorobenzene and 8.50g (0.05mol) of silicon tetrachloride, start stirring, under the cooling of ice-water bath, pass 2.20g (0.05mol) of ethylene oxide under the liquid surface, and control the temperature with the speed of introduction Below 20°C, after passing through, add 49.62g (0.15mol) of tribromophenol, raise the temperature to 105°C, keep the temperature for 9 hours, after the hydrogen chloride is released, cool down to 40°C, and then add ethylene oxide under the liquid surface Remove a small amount of free acid in the reaction solution, check the pH of the reaction solution = 5 to 6 as the end point, and distill off the solvent (recycled for use) and a small amount of low boili...

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Abstract

The invention relates to a silicic acid-3-(3-bromophenyl)-chloropropyl ethyl ester compound used as a fire retardant and the preparation method thereof. The structural formula of the compound is shown in the specification. The preparation method comprises the following steps: filling ethylene oxide of which the mole is same as that of silicon tetrachloride in silicon tetrachloride organic solution at the temperature of below 20 DEG C, adding tribromophenol of which is three times the mole of silicon tetrachloride, carrying out the thermal reaction for 6-10 hours at the temperature of 100-120 DEG C, and reducing pressure and distilling to remove solvent and a small amount of low boiling point substances to obtain the silicic acid-3-(3-bromophenyl)-chloropropyl ethyl ester compound. The silicic acid-3-(3-bromophenyl)-chloropropyl ethyl ester compound is an excellent fire retardant plasticizer, has carbon-forming and anti-dripping functions and good compatibility with high polymer material, can be used as fire retardants made of polyvinyl chloride, unsaturated polyester, polyurethane, epoxy resin and the like, and is easy to access in raw material, low in production cost, small in equipment investment, simple in production technology, and easy for large-scale production.

Description

technical field [0001] The invention relates to a flame retardant tris(tribromophenyl)chloroethyl silicate 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. agent. Background technique [0002] With the development of science and technology and the improvement of people's living standards, the three major synthetic polymer materials have been widely used. Because most of them are flammable, they often cause fires and pose a serious threat to people's lives and property, thereby promoting The research of flame retardant technology and the rapid development of flame retardant plasticizer industry. Flame retardant plasticizer is a plastic processing aid with flame retardant function and plasticizing effect. It can overcome the problem of making polymer materials more flammable due to the addition of plasticizers. Phosphate ester flame retardant...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/06C08K5/5425
Inventor 王彦林孟凡一侯宁
Owner 张家港市乐余科创园投资发展有限公司
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