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

A technology of dibromopropoxysilane and dibromopropoxytrisilane, which is applied in the field of flame retardant dibromopropoxytrisilane compound and its preparation, and can solve the problem of inability to handle by-product silicon tetrachloride, environmental pollution, etc. problems, to achieve the effect of excellent cost performance, stable physical and chemical properties, 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

However, the production of polysilicon, the basic raw material of the photovoltaic industry, will produce a large amount of by-product silicon tetrachloride that cannot be processed, which will cause serious pollution to the environment

Method used

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  • Fire retardant dibromopropyl tri(tribromophenoxy)silane compound and its preparation method
  • Fire retardant dibromopropyl tri(tribromophenoxy)silane compound and its preparation method
  • Fire retardant dibromopropyl tri(tribromophenoxy)silane compound and its preparation method

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 8.50g (0.05mol) 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 10.90g (0.05mol) 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 49.62g (0.15mol) tribromophenol, heat up to 120°C, keep warm for 8 hours, after the hydrogen chloride is released, cool down to 40°C, install an extremely stretchable soft sealing s...

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 toluene and 8.50g (0.05mol) silicon tetrachloride, under stirring, cool with ice-water bath, make reaction system temperature drop to 0 ℃, dropwise add 10.90g (0.05mol) to the organic solution of silicon tetrachloride ) 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 49.62g (0.15mol) Tribromophenol, heat up to 100°C, keep warm for 10 hours, after releasing hydrogen chloride, cool down to 40°C, pass ethylene oxide under the liquid surface to remove trace free acid in the reaction liquid,...

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 xylene and 8.50g (0.05mol) of silicon tetrachloride, under stirring, cool with an ice-water bath, reduce the temperature of the reaction system to 0°C, and drop 10.90g (0.05mol) of silicon tetrachloride into the organic solution mol) 2,3-dibromo-1-propanol, during the dropping process, the temperature is controlled below 8°C. After the drop is completed, the temperature is raised to 35°C for 1 hour, and the temperature is kept for 1 hour. After the hydrogen chloride is released, add 49.62g (0.15mol ) Tribromophenol, heat up to 110°C, heat preservation reaction for 9h, after the hydrogen chloride is released, cool down to 40°C, feed ethylene oxide under the liquid surface to ...

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Abstract

The invention relates to a fire retardant dibromopropyl tri(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 three molar rations of tribromophenol, reacting at 90-120 DEG C for 8-11h, neutralizing free acid by the use of oxirane, and carrying out underpressure distillation to remove a solvent so as to obtain a product dibromopropyl tri(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 present invention relates to a kind of flame retardant dibromopropoxy tris (tribromophenoxy) silane compound and its preparation method, and this compound can be used as polyvinyl chloride, unsaturated polyester, polyurethane and epoxy resin etc. flame retardant. Background technique [0002] With the rapid development of society, a large amount of energy is consumed, and environmental pollution is becoming more and more serious, which promotes the vigorous development of the photovoltaic industry. However, the production of polysilicon, the basic raw material of the photovoltaic industry, will produce a large amount of by-product silicon tetrachloride that cannot be processed, which will cause serious pollution to the environment. Silicon tetrachloride contains silicon flame retardant elements, and silicon-based flame retardants have become the current development of low-smoke, low-toxicity flame-retardant materials due to their excellent thermal...

Claims

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Application Information

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IPC IPC(8): C07F7/06C08L27/06C08K5/5415
Inventor 王彦林孟凡一刘芳贺婧施雯
Owner 张家港市乐余科创园投资发展有限公司
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