Fire retardant di(tribromophenoxy)dihalidepropoxysilane compound and its preparation method

A technology of dihalopropoxysilane and tribromophenoxy, which is applied in the field of flame retardant dihalopropoxysilane compounds and their preparation, can solve the problems of high price and application restrictions of silicon-based flame retardants, Achieve the effect of good compatibility, high flame retardant efficiency, and reduce the amount of addition

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

Because silicon-based flame retardant plasticizers have the excellent performance of suppressing smoke and promoting carbon formation, people pay attention to them. However, the high price of silicon-based flame retardants generally limits their application.

Method used

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  • Fire retardant di(tribromophenoxy)dihalidepropoxysilane compound and its preparation method
  • Fire retardant di(tribromophenoxy)dihalidepropoxysilane compound and its preparation method
  • Fire retardant di(tribromophenoxy)dihalidepropoxysilane compound and its preparation method

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 carbon tetrachloride and 16.99g (0.1mol) of silicon tetrachloride, under stirring, cool with ice-water bath, make the reaction system temperature drop to 0 ℃, dropwise add 9.45g in the organic solution of silicon tetrachloride (0.1mol) 2-chloro-1-propanol, the dropwise addition process controls the temperature below 5°C, after the drop is completed, the temperature is raised to 30°C for 1h, and the temperature is kept for 1h. After the hydrogen chloride is released, add 66.16g (0.2mol) Tribromophenol, heat up to 80°C, heat preservation reaction for 5h, after the hydrogen chloride is released, cool down to below 30°C, then add 9.45g (0.1mol) 2-chloro-1-propanol dropwise, and con...

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 acetonitrile and 16.99g (0.1mol) silicon tetrachloride, under stirring, cool with ice-water bath, make the temperature of reaction system drop to 0 ℃, dropwise add 9.45g (0.1mol) in the organic solution of silicon tetrachloride ) 1-chloro-2-propanol, the dropping process controls the temperature below 5°C, after the drop is completed, the temperature is raised to 30°C for 1h, and the heat preservation reaction is carried out for 1h, after the hydrogen chloride is released, add 66.16g (0.2mol) of tribromophenol , heat up to 60°C, heat preservation reaction for 6h, after the hydrogen chloride is released, cool down to below 30°C, then add 9.45g (0.1mol) 1-chloro-2-propanol drop...

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 dioxane and 16.99g (0.1mol) silicon tetrachloride, under stirring, cool with ice-water bath, make the reaction system temperature drop to 0 ℃, dropwise add 9.45g in the organic solution of silicon tetrachloride (0.1mol) 3-chloro-1-propanol, the dropwise addition process controls the temperature below 5°C, after the drop is completed, the temperature is raised to 30°C for 1h, and the temperature is kept for 1h. After the hydrogen chloride is released, add 66.16g (0.2mol) Tribromophenol, heat up to 90°C, keep warm for 4 hours, after the hydrogen chloride is released, cool down to below 30°C, then add 9.45g (0.1mol) 3-chloro-1-propanol dropwise, and control the temperature not to ...

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Abstract

The invention relates to a fire retardant di(tribromophenoxy)dihalidepropoxysilane compound and its preparation method. The structure of the compound is as shown in the formula in the specification, wherein R is 2-chloro-1-propyl, 1-chloro-2-propyl, 3-chloro-1-propyl, 2-bromine-1-propyl, 1-bromine-2-propyl or 3-bromine-1-propyl. The preparation method comprises the following steps: dropwisely adding equimolar halogenated propanol into a silicon tetrachloride organic solution to react at 30 DEG C for 1h, adding tribromophenol which accounts for two times larger than equimolar halogenated propanol to react at 60-90 DEG C for 4-6h, dropwisely adding equimolar halogenated propanol to react at 40-60 DEG C for 3-5h, and carrying out underpressure distillation to remove a solvent so as to obtain di(tribromophenoxy)dihalidepropoxysilane. The product has good flame retardation and plastification properties, has charcoal-forming and antidrip effects, and can be used as a fire retardant of materials such as polyvinyl chloride, nonsaturated polyester, polyurethane, epoxy resin and the like. Raw materials of the fire retardant are easily available; production costs are low; equipment investment is little; the technology is simple; and the preparation method is easy for large-scale production.

Description

technical field [0001] The invention relates to a flame retardant bis(tribromophenoxy)dihalopropoxysilane 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] Since the 1970s, polymer materials such as plastics, rubber, and fibers have gradually been widely used. Because of their flammability, they often cause fires, which pose a serious threat to people's lives and property, thus promoting flame-retardant science and technology. With the rapid development of flame retardant industry. Flame retardant plasticizer is a plastic processing aid with flame retardant function and plasticizing effect. It can overcome the problem of making polymer materials more flammable due to the addition of plasticizers. At present, there is a strong urgency in the market for new high-efficiency, low-toxicity, and cheap flame-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/06C08K5/5415C08L27/06
Inventor 王彦林孟凡一龚菁
Owner 张家港市乐余科创园投资发展有限公司
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