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Fire retardant tribromophenoxy tri(dichloro propanolato)silane compound and its preparation method

A technology of tribromophenoxy tri, dichloropropoxy, applied in the direction of silicon organic compounds, etc., can solve problems such as difficulty in finding substitutes, and achieve the effects of easy purification and separation, easy availability of raw materials, and good compatibility

Active Publication Date: 2013-09-25
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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  • Fire retardant tribromophenoxy tri(dichloro propanolato)silane compound and its preparation method
  • Fire retardant tribromophenoxy tri(dichloro propanolato)silane compound and its preparation method
  • Fire retardant tribromophenoxy tri(dichloro propanolato)silane compound and its preparation method

Examples

Experimental program
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Embodiment 1

[0031] Example 1 In the 250ml four-neck 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 80ml 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 33.08g ( 0.1mol) tribromophenol, heat up to 80°C, keep warm for 2 hours, after the hydrogen chloride is released, cool down to below 25°C, then add 25.80g (0.2mol) 2,3-dichloro-1-propanol ...

Embodiment 2

[0032]Example 2 In a 250ml four-necked flask equipped with a stirrer, a thermometer, a dropping funnel and a high-efficiency reflux condenser and a hydrogen chloride absorption device connected in series with a drying tube at the top of the condenser, replace the air in the bottle with nitrogen , add 80ml 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 33.08 g (0.1mol) tribromophenol, heat up to 60°C, keep warm for 4 hours, after the hydrogen chloride is released, cool down to below 25°C, then add 25.80g (0.2mol) 2,3-dichloro-1-pr...

Embodiment 3

[0033] Example 3 In a 250ml 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 80ml acetonitrile and 16.99g (0.1mol) silicon tetrachloride, under stirring, cool with ice-water bath, make reaction system temperature drop to 0 ℃, in the organic solution of silicon tetrachloride, add dropwise 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 33.08g (0.1mol) Tribromophenol, heat up to 70°C, keep warm for 3 hours, after the hydrogen chloride is released, cool down to below 25°C, then add 25.80g (0.2mol) 2,3-dichloro-1-propanol dropwise, and control the temp...

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Abstract

The invention relates to a fire retardant tribromophenoxy tri(dichloro propanolato)silane compound and its preparation method. The structure of the compound is as shown in the formula in the specification, wherein R2=CH2Cl when R1=H; and R2=H when R1=CH2Cl. The preparation method comprises the following steps: dropwisely adding equimolar dichlorohydrin into a silicon tetrachloride organic solution to react at 35 DEG C for 1h, adding equimolar tribromophenol to react at 50-80 DEG C for 2-5h, dropwisely adding double mole times of dichlorohydrin to react at 50-70 DEG C for 3-6h, and carrying out underpressure distillation to remove a solvent so as to obtain a product tribromophenoxy tri(dichloro propanolato)silane. The product is an excellent flame retardation plasticizer, has charcoal-forming and antidrip effects, and can be used as a fire retardant of materials such as polyvinyl chloride, nonsaturated polyester, polyurethane and epoxy resin, etc. Raw materials of the product are cheap and easily available. Production costs are low. Equipment investment is little. The production technology is simple. The preparation method is easy for large-scale production.

Description

technical field [0001] The present invention relates to a kind of flame retardant tribromophenoxy tris (dichloropropoxy) silane compound and preparation method thereof, and this compound can be used as material such as polyvinyl chloride, unsaturated polyester, polyurethane and epoxy resin flame retardant. Background technique [0002] Due to the rapid development of science, technology and economy, people's safety awareness has been continuously enhanced, which has promoted 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. Among them, improving the flame reta...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/06C08K5/5415C08L27/06
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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