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2-(3-broMopropoxy)-2(2-dicholoropropoxy) silane compound used as fire retardant and preparation method thereof

A technology of tribromophenoxy and dichloropropoxy, which is applied in the direction of silicon organic compounds, can solve problems such as difficulty in finding substitutes, and achieve the effects of easy purification and separation, low production cost, and stable physical and chemical properties

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

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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  • 2-(3-broMopropoxy)-2(2-dicholoropropoxy) silane compound used as fire retardant and preparation method thereof
  • 2-(3-broMopropoxy)-2(2-dicholoropropoxy) silane compound used as fire retardant and preparation method thereof
  • 2-(3-broMopropoxy)-2(2-dicholoropropoxy) silane compound used as fire retardant and preparation method thereof

Examples

Experimental program
Comparison scheme
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 150ml 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 66.16g (0.2mol) tribromophenol, heat up to 90°C, keep warm for 4 hours, after hydrogen chloride is released, cool down to below 40°C, then add 12.90g (0.1mol) 2,3-dichloro-1...

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 150ml 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 66.16 g (0.2mol) tribromophenol, heat up to 75°C, keep warm for 5.5h, after the hydrogen chloride is released, cool down to below 40°C, then add 12.90g (0.1mol) 2,3-dichloro-1-propa...

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 150ml 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 66.16g ( 0.2mol) of tribromophenol, raised the temperature to 80°C, and kept the temperature for 5 hours. Acceleration control temperature does not exceed 50°C. After dripping, rais...

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Abstract

The invention relates to a 2-(3-broMopropoxy)-2(2-dicholoropropoxy) silane compound used as a fire retardant and the preparation method thereof. The structural formula of the compound is shown in the specification, wherein when R1equals to H, R2 equals to CH2C1; when R1 equals to CH2C1, R2 equals to H. The preparation method comprises the following steps: dripping dichloropropanol of which the mole is the same as that of silicon tetrachloride into silicon tetrachloride organic solution, reacting for 1 hour at the temperature of 35 DEG C, then adding tribromophenol of which the mole doubles that of silicon tetrachloride, reacting for 4-6 hours at the temperature of 65-90 DEG C, dripping dichloropropanol of which the mole is equal to that of silicon tetrachloride, reacting for 5-7 hours at the temperature of 70-95 DEG C, and reducing pressure and distilling to remove solvent to obtain the 2-(3-broMopropoxy)-2(2-dicholoropropoxy) silane compound. The silane compound is an excellent fire retardant plasticizer, has carbon-forming and anti-dripping functions, can be used as fire retardant 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 bis(tribromophenoxy)bis(dichloropropoxy)silane compound and a preparation method thereof, the compound can be used as polyvinyl chloride, unsaturated polyester, polyurethane and epoxy resin Flame retardant for other materials. 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. Among them, ...

Claims

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Application Information

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IPC IPC(8): C07F7/04C08K5/5415C08L27/06C08L67/06C08L63/00C08L75/04
Inventor 王彦林韩志慧孟凡一
Owner 张家港市乐余科创园投资发展有限公司
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