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Flame retardant tetra(tribromophenyl) silicate esterification compound and preparation method thereof

A technology of ester compound and tetrasilicic acid, which is applied in the direction of silicon organic compounds, can solve the problems of difficulty in finding ideal substitutes, high comprehensive cost performance, etc., and achieve excellent plasticizing effect, high decomposition temperature, and good compatibility.

Active Publication Date: 2013-10-09
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

Among them, halogenated flame retardants have a long history of development, and their application technology is very mature. Although halogenated flame retardants emit a large amount of harmful gases such as hydrogen halides and dioxins when burned, their comprehensive cost performance is high, and it is difficult to find an ideal substitute for them. Taste

Method used

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  • Flame retardant tetra(tribromophenyl) silicate esterification compound and preparation method thereof
  • Flame retardant tetra(tribromophenyl) silicate esterification compound and preparation method thereof
  • Flame retardant tetra(tribromophenyl) silicate esterification compound and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Example 1 In a 500ml four-necked flask equipped with a stirrer, a thermometer, a dropping funnel and a high-efficiency reflux condenser and a series hydrogen chloride absorption device and a drying tube at the top of the condenser, nitrogen protection was introduced, and 150ml xylene was added and 8.50g (0.05mol) silicon tetrachloride, start stirring, at 30°C, add 66.16g (0.2mol) tribromophenol, then raise the temperature to 45°C for 1h, keep the temperature for 1h, then raise the temperature to 105°C, keep the temperature for reaction 11 hours, after the hydrogen chloride is released, cool down to 40°C, install an extremely stretchable soft seal on the top of the condenser tube, inject ethylene oxide under the liquid surface to remove traces of free acid in the reaction solution, and test the reaction solution. When the pH=5-6 is the end point, the solvent (recycled) and a small amount of low boiling point substances are distilled off under reduced pressure to obtain th...

Embodiment 2

[0028] Example 2 In a 500ml four-neck flask equipped with a stirrer, a thermometer, a dropping funnel and a high-efficiency reflux condenser and a series hydrogen chloride absorption device and a drying tube on the upper mouth of the condenser, nitrogen protection was introduced, and 150ml of dioxygen was added. Hexacyclic and 8.50g (0.05mol) silicon tetrachloride, start stirring, at 30°C, add 66.16g (0.2mol) tribromophenol, then raise the temperature to 45°C for 1h, keep the temperature for 1h, then raise the temperature to 100°C, Insulate and react for 12 hours. After the hydrogen chloride is released, cool down to 40°C. Install an extremely flexible soft seal on the top of the condenser tube. Put ethylene oxide under the liquid surface to remove traces of free acid in the reaction solution and test the reaction. The pH of the solution is 5-6 as the end point, and the solvent (recycled) and a small amount of low boiling point substances are removed by distillation under reduc...

Embodiment 3

[0029] Example 3 In a 500ml four-neck flask equipped with a stirrer, a thermometer, a dropping funnel and a high-efficiency reflux condenser and a series hydrogen chloride absorption device and a drying tube at the top of the condenser, nitrogen protection was introduced, and 150ml of chlorobenzene was added. and 8.50g (0.05mol) of silicon tetrachloride, start stirring, at 30°C, add 66.16g (0.2mol) of tribromophenol, then raise the temperature to 45°C for 1h, keep the reaction for 1h, then raise the temperature to 115°C, keep the reaction 9h, after the hydrogen chloride is released, lower the temperature to 40°C, install an extremely stretchable soft seal at the top of the condenser tube, inject ethylene oxide under the liquid surface to remove traces of free acid in the reaction solution, and test the reaction solution. When the pH=5-6 is the end point, the solvent (recycled) and a small amount of low boiling point substances are distilled off under reduced pressure to obtain ...

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Abstract

The invention relates to a flame retardant tetra(tribromophenyl) silicate esterification compound and a preparation method thereof. The structure of the compound is shown in the specification. The preparation method comprises the following steps of: adding tribromophenol of quadruple molar weight into an organic solution of silicon tetrachloride at 30 DEG C; heating to 45 DEG C in one hour, and performing a thermal-insulation reaction for one hour; heating to 100-120 DEG C, and performing a thermal-insulation reaction for 8-12 hours; and performing reduced-pressure distillation to remove the solvent to obtain the product tetra(tribromophenyl) silicate. The tetra(tribromophenyl) silicate provided by the invention is an excellent flame-retardant plasticizer with a charring anti-drop effect and good compatibility with a high-molecular material, and can be used as a flame retardant for the materials such as polyvinyl chloride, unsaturated polyester, polyurethane, epoxy resin and the like; and moreover, the flame retardant has the advantages of cheap and easily-available raw materials, low equipment investment and simple production technology, and is easy to produce in a large scale.

Description

technical field [0001] The invention relates to a flame retardant tetrakis (tribromophenyl) 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. Background technique [0002] There are frequent fire accidents in the society, which often pose a serious threat to people's lives and property safety. People's awareness of safety and fire prevention has gradually increased, thus promoting the rapid development of flame retardant science and technology and flame retardant industry. The global flame retardant consumption has been showing a rapid growth trend. Due to the increasingly stringent international flame retardant legislation, the successive introduction of industry directives and the environmental protection requirements for flame retardants, there is an urgent need for new, efficient and environmentally friendly flame retardants. need...

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
Owner 张家港市乐余科创园投资发展有限公司
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