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A flame retardant tris(tribromophenoxy)dichloropropoxysilane compound and its preparation method

A technology of dichloropropoxysilane and tribromophenoxy, which is applied in the field of flame retardant tridichloropropoxysilane compound and its preparation, can solve the problems such as difficulty in finding substitutes, and achieve easy purification and separation, phase Good capacity and simple operation

Active Publication Date: 2015-12-23
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

Since the European Union announced in 1986 that polybrominated diphenyl ether flame retardants produced carcinogen dioxin when burned, the use of halogenated flame retardants has been restricted. 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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  • A flame retardant tris(tribromophenoxy)dichloropropoxysilane compound and its preparation method
  • A flame retardant tris(tribromophenoxy)dichloropropoxysilane compound and its preparation method
  • A flame retardant tris(tribromophenoxy)dichloropropoxysilane compound and its preparation method

Examples

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Effect test

Embodiment 1

[0032] Example 1 In the 500ml four-necked flask equipped with agitator, thermometer, dropping funnel and high-efficiency reflux condenser and a hydrogen chloride absorbing device connected in series with a drying tube at the top of the condenser, replace the air in the bottle with nitrogen , add 180ml of diethylene glycol dimethyl ether and 16.99g (0.1mol) of silicon tetrachloride, under stirring, cool with an ice-water bath, reduce the temperature of the reaction system to 0 ° C, drop into the organic solution of silicon tetrachloride Add 12.90g (0.1mol) of 2,3-dichloro-1-propanol, and control the temperature below 8°C during the dropwise addition process. After the dropwise addition, raise the temperature to 35°C for 1 hour, and keep the temperature for 1 hour. After the hydrogen chloride is released, add 99.24g (0.3mol) tribromophenol, heat up to 110°C, keep warm for 7 hours, after the hydrogen chloride is released, cool down to below 40°C, install an extremely stretchable s...

Embodiment 2

[0033]Example 2 In a 500ml four-necked flask equipped with a stirrer, a thermometer, a dropping funnel and a high-efficiency reflux condenser and a hydrogen chloride absorbing device connected in series with a drying tube at the top of the condenser, replace the air in the bottle with nitrogen , add 180ml of ethylene glycol dimethyl ether and 16.99g (0.1mol) of silicon tetrachloride, under stirring, cool with an ice-water bath, reduce the temperature of the reaction system to 0°C, and add dropwise to the organic solution of silicon tetrachloride 12.90g (0.1mol) 2,3-dichloro-1-propanol, the dropwise addition process controls the temperature below 8°C, after the drop is completed, the temperature is raised to 35°C for 1h, and the temperature is kept for 1h. After the hydrogen chloride is released, add 99.24 g (0.3mol) of tribromophenol, heat up to 80°C, keep warm for 9 hours, after the hydrogen chloride is released, cool down to below 40°C, install an extremely stretchable soft s...

Embodiment 3

[0034] 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 hydrogen chloride absorbing device connected in series with a drying tube at the top of the condenser, replace the air in the bottle with nitrogen , add 180ml of dioxane and 16.99g (0.1mol) of silicon tetrachloride, under stirring, cool with an ice-water bath, reduce the temperature of the reaction system to 0°C, and drop 12.90g of silicon tetrachloride into the organic solution (0.1mol) 2,3-dichloro-1-propanol, the temperature of the dropwise addition process is controlled below 8°C, after the drop is completed, the temperature is raised to 35°C in 1h, and the heat preservation reaction is carried out for 1h. After the hydrogen chloride is released, add 99.24g ( 0.3mol) tribromophenol, heat up to 90°C, keep warm for 8 hours, after the hydrogen chloride is released, cool down to below 40°C, install an extremely stretchable soft seali...

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Abstract

The invention relates to a flame retardant tri-(tribromophenoxy) dichloro propoxy silane compound and a preparation method thereof. A structural formula of the compound is as follows as shown in the specification, wherein when R1 is H, R2 is CH2Cl, and when R1 is CH2Cl, R2 is H. The preparation method comprises the steps that equimolar dichloropropanol is dropwise added to an organic solution of silicon tetrachloride, and reacts at 35 DEG C for 1h; three times of mole of tribromphenol is added, and reacts at 80-110 DEG C for 7-9h; a solvent is removed by reduced pressure distillation; and tri-(tribromophenoxy) dichloro propoxy silane is obtained. Tri-(tribromophenoxy) dichloro propoxy silane is an excellent antiflaming plasticizer, has charring and dripping prevention functions, has good compatibility with a high polymer material, and can serve as a flame retardant of polyvinyl chloride, unsaturated polyester, polyurethane, epoxy resin and the like, raw materials of tri-(tribromophenoxy) dichloro propoxy silane are low in cost and easy to obtain, the production cost is low, the equipment investment is low, a production technology is simple, and the scale production is facilitated.

Description

technical field [0001] The invention relates to a flame retardant tris(tribromophenoxy)dichloropropoxysilane compound and a preparation method thereof. The compound can be used as a compound for materials such as polyvinyl chloride, unsaturated polyester, polyurethane and epoxy resin flame retardant. Background technique [0002] With the advancement of science and technology, people's living standards continue to improve, and the awareness of safety and fire prevention continues to increase, which promotes the rapid development of the flame retardant industry. Since the European Union announced in 1986 that polybrominated diphenyl ether flame retardants produced carcinogen dioxin when burned, the use of halogenated flame retardants has been restricted. The 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 of halogenated flame retardants. Amo...

Claims

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Application Information

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