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Flame retardant tri-(tribromophenoxy) halogen propoxy silane compound and preparation method thereof

A technology of halopropoxysilane and tribromophenoxy, which is applied in the field of flame retardant trihalopropoxysilane compound and its preparation, can solve the problems of application limitation and high price of silicon-based flame retardants, and achieve production cost Low, overcome the effect of volatile reaction and high flame retardant efficiency

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

Among them, silicon-based flame retardants have excellent properties of suppressing smoke and promoting carbon formation, and have attracted people's attention. However, the high price of silicon-based flame retardants generally limits their application.

Method used

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  • Flame retardant tri-(tribromophenoxy) halogen propoxy silane compound and preparation method thereof
  • Flame retardant tri-(tribromophenoxy) halogen propoxy silane compound and preparation method thereof
  • Flame retardant tri-(tribromophenoxy) halogen propoxy silane compound 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 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 9.45g of silicon tetrachloride into the organic solution (0.1mol) 2-chloro-1-propanol, during the dropping process, the temperature is controlled 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 99.24g (0.3mol) Tribromophenol, heat up to 90°C, keep warm for 7 hours, after the hydrogen chloride is released, cool down to below 40°C, install an extremely stretchable soft seal on the top of the condenser tube, ...

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 acetonitrile 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 (0.1mol) in the organic solution of silicon tetrachloride ) 1-chloro-2-propanol, the dropping process controls the temperature below 5°C, after the dropping, 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 99.24g (0.3mol) of tribromophenol , heat up to 70°C, keep warm for 9 hours, after the hydrogen chloride is released, cool down to below 40°C, add propylene oxide dropwise under the liquid surface to remove a small a...

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 tetrachloroethane and 16.99g (0.1mol) silicon tetrachloride, under stirring, cool with ice-water bath, make 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 99.24g (0.3mol) Tribromophenol, heat up to 100°C, keep warm for 6 hours, after the hydrogen chloride is released, cool down to below 40°C, add propylene oxide dropwise under the liquid surface to remove a small amount of ...

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Abstract

The invention relates to a flame retardant tri-(tribromophenoxy) halogen propoxy silane compound and a preparation method thereof. A structural formula of the compound is as follows as shown in the specification, wherein R is 2-chlorine-1-propyl, 1-chlorine-2-propyl, 3-chlorine-1-propyl, 2-bromine-1-propyl, 1-bromine-2-propyl or 3-bromine-1-propyl. The preparation method comprises the steps that equimolar halogenated propyl alcohol is dropwise added to an organic solution of silicon tetrachloride, and reacts at 30 DEG C for 1h; three times of mole of tribromphenol is added, and reacts at 70-100 DEG C for 6-9h; a solvent is removed by reduced pressure distillation; and tri-(tribromophenoxy) halogen propoxy silane is obtained. Tri-(tribromophenoxy) halogen propoxy silane is good in flame retardancy and plasticity, has charring and dripping prevention functions, has good compatibility with a high polymer material, can serve as a flame retardant of polyvinyl chloride, unsaturated polyester, polyurethane, epoxy resin and the like, raw materials of tri-(tribromophenoxy) halogen propoxy silane are 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)halopropoxysilane compound and a preparation method thereof. The compound can be used as a flame retardant for materials such as polyvinyl chloride, unsaturated polyester, polyurethane and epoxy resin. Fuel. Background technique [0002] With the development of the polymer industry, 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 the development of anti-corrosion The rapid development of flame retardant science and technology and flame retardant industry. Among them, silicon-based flame retardants have excellent properties of suppressing smoke and promoting carbon formation, and have attracted people's attention. However, the high price of silicon-based flame retardants generally limits their application. The development ...

Claims

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Application Information

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IPC IPC(8): C07F7/06C08K5/5415C08L27/06
Inventor 王彦林徐玫孟凡一
Owner 张家港市乐余科创园投资发展有限公司
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