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A kind of flame retardant tris(chloropropyl)tribromophenyl silicate compound and preparation method thereof

A technology of tribromophenyl ester and trisilicate, which is applied in the direction of silicon organic compounds, can solve problems such as the difficulty of finding substitutes for halogenated flame retardants, and overcome the volatile nature of the reaction, good compatibility, and cheap raw materials. The effect

Active Publication Date: 2015-09-16
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

Although halogenated flame retardants have the disadvantage of releasing hydrogen halide when they burn, it is still difficult to find ideal substitutes for halogenated flame retardants in many fields, so the development of high-efficiency halogenated flame retardants has become an important research topic. topic

Method used

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  • A kind of flame retardant tris(chloropropyl)tribromophenyl silicate compound and preparation method thereof
  • A kind of flame retardant tris(chloropropyl)tribromophenyl silicate compound and preparation method thereof
  • A kind of flame retardant tris(chloropropyl)tribromophenyl silicate compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Embodiment 1 In the 150ml 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 air, add 70ml of dioxane and 16.99g (0.1mol) of silicon tetrachloride, start stirring, and under cooling in an ice-water bath, add 5.81g (0.1mol) of propylene oxide dropwise, and control the temperature at 30°C with the dropping rate Below, after dripping, keep warm at 30°C for 30 minutes, refit the hydrogen chloride absorption device at the top of the condenser, add 33.08g (0.1mol) tribromophenol, raise the temperature to 65°C, keep warm for 3 hours, and cool down after the hydrogen chloride is released. To 30°C, restore the soft sealing sleeve device on the upper port of the condenser, then add 13.94g (0.24mol) propylene oxide dropwise, and control the temperature below 40°C...

Embodiment 2

[0030]Example 2 In a 150ml 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 70ml of acetonitrile and 16.99g (0.1mol) of silicon tetrachloride, start stirring, and drop 5.81g (0.1mol) of propylene oxide under cooling in an ice-water bath. After completion, keep the reaction at 30°C for 30 minutes, refit the hydrogen chloride absorption device at the top of the condenser, add 33.08g (0.1mol) of tribromophenol, raise the temperature to 50°C, and keep the reaction for 3.5h. After the hydrogen chloride is released, cool down to 30 ℃, restore the soft sealing sleeve device on the upper mouth of the condenser tube, then add 12.78g (0.22mol) propylene oxide dropwise, and control the temperature below 40°C with the dropping speed. Make the pH value of the reaction solution reach...

Embodiment 3

[0031] Example 3 In a 150ml 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 70ml of carbon tetrachloride and 16.99g (0.1mol) of silicon tetrachloride, start stirring, under cooling in an ice-water bath, add 5.81g (0.1mol) of propylene oxide dropwise, and control the temperature at 30°C with the dropping rate Below, after dropping, keep warm at 30°C for 30 minutes, refit the hydrogen chloride absorption device on the top of the condenser, add 33.08g (0.1mol) tribromophenol, raise the temperature to 70°C, keep warm for 2 hours, and cool down after the hydrogen chloride is released. To 30°C, restore the soft sealing sleeve device on the upper port of the condenser, then add 11.62g (0.2mol) propylene oxide dropwise, and control the temperature below 40°C with the dropping s...

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Abstract

The invention relates to a flame retardant tri(chloropropyl)tribromophenyl silicate esterification compound and a preparation method thereof. The structure of the compound is shown in the specification, wherein n is an integer from 0 to 3. The preparation method comprises the following steps of: controlling the temperature below 30 DEG C; dropwise adding equimolar epoxypropane into an organic solution of silicon tetrachloride, and adding equimolar tribromophenol; performing a thermal-insulation reaction at 50-70 DEG C for 2-4 hours; cooling to 40 DEG C; dropwise adding epoxypropane of a certain molar ratio, and performing a thermal-insulation reaction at 45-70 DEG C for 3-6 hours; distilling out excessive epoxypropane; and performing reduced-pressure distillation to remove the solvent and a few low-boiling point substances to obtain the product tri(chloropropyl)tribromophenyl silicate. The tri(chloropropyl)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 production cost, 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 tris(chloropropyl)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. agent. Background technique [0002] With the rapid development of my country's economy and the continuous improvement of people's living standards, people's safety awareness has gradually increased. Because most of the widely used polymer materials are flammable, they often cause fires and pose a serious threat to people's lives and properties. In order to prevent or reduce the damage caused by fire, people are constantly looking for various new high-efficiency flame retardants. Among them, halogenated flame retardants have a long history of development, mature application technology, high comprehensive cost performance, and have been widely used. Although halogenated flame retardants...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/06C08K5/5415C08L27/06C08L67/06C08L75/04C08L63/00
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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