A kind of flame retardant bis(dibromopropoxy) bis(tribromophenoxy) silane compound and preparation method thereof

A technology of dibromopropoxy and tribromophenoxy, applied in the direction of silicon organic compounds, can solve the problems of health hazards, difficulty in finding substitutes, etc., to prevent secondary combustion, have excellent cost performance, and overcome the volatile reaction. Effect

Active Publication Date: 2016-04-06
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

The European Union announced in 1986 that the carcinogen dioxin was produced when polybrominated diphenyl ether flame retardants were burned, which would cause harm to the environment and human health. After that, the use of halogenated flame retardants was restricted, but due to the Flame retardants have excellent comprehensive cost performance, high flame retardant performance, little impact on the machinability of materials, and it is difficult to find ideal substitutes. Although the calls for halogen-free environmentally friendly flame retardants are high, halogen-free is still a long process. Therefore, the 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 kind of flame retardant bis(dibromopropoxy) bis(tribromophenoxy) silane compound and preparation method thereof
  • A kind of flame retardant bis(dibromopropoxy) bis(tribromophenoxy) silane compound and preparation method thereof
  • A kind of flame retardant bis(dibromopropoxy) bis(tribromophenoxy) silane compound and preparation method thereof

Examples

Experimental program
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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 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 21.79g (0.1mol) of 2,3-dibromo-1-propanol, and control the temperature below 8°C during the dropwise addition. 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) of tribromophenol, raised the temperature to 90°C, kept the temperature for 4h, after the hydrogen chloride was released, cooled down to 40°C, then added 21.79g (0.1mo...

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 21.79g (0.1mol) 2,3-dibromo-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 70°C, keep warm for 5.5h, after the hydrogen chloride is released, cool down to 40°C, then add 21.79g (0.1mol) 2,3-dibromo-1-propanol dro...

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 21.79g of silicon tetrachloride into the organic solution (0.1mol) 2,3-dibromo-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) tribromophenol, heat up to 80°C, keep warm for 5h, after the hydrogen chloride is released, cool down to 40°C, then add 21.79g (0.1mol) 2,3-dibromo-1-propanol dropwis...

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Abstract

The invention relates to a fire retardant di(dibromo propanolato)di(tribromophenoxy)silane compound and its preparation method. The structure of the compound is as shown in the formula in the specification, wherein R2=CH2Br when R1=H; and R2=H when R1=CH2Br. The preparation method comprises the following steps: dropwisely adding equimolar dibromopropyl alcohol into a silicon tetrachloride organic solution at 8 DEG C, keeping the temperature at 35 DEG C to react for 1h, adding two molar rations of tribromophenol, keeping the temperature at 60-90 DEG C to react for 4-6h, dropwisely adding equimolar dibromopropyl alcohol, keeping the temperature at 70-95 DEG C to react for 5-7h, and carrying out underpressure distillation to remove a solvent so as to obtain a product di(dibromo propanolato)di(tribromophenoxy)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 cost is low. Equipment investment is little. The production technology is simple. The preparation method is easy for large-scale production.

Description

technical field [0001] The invention relates to a flame retardant bis(dibromopropoxy)bis(tribromophenoxy)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 continuous improvement of people's living standards, the awareness of safety and fire prevention has been continuously enhanced, which has promoted the rapid development of the flame retardant industry. The European Union announced in 1986 that the carcinogen dioxin was produced when polybrominated diphenyl ether flame retardants were burned, which would cause harm to the environment and human health. After that, the use of halogenated flame retardants was restricted, but due to the Flame retardants have excellent comprehensive cost performance, high flame retardant performance, little impact on the machinability of materials, and it is difficult to...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/06C08L27/06C08K5/5415
Inventor 王彦林孟凡一施雯刘芳贺婧
Owner 张家港市乐余科创园投资发展有限公司
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