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Flame retardant silicic acid di-(tribromophenyl) dichlorohydrin compound and preparation method thereof

A technology of tribromophenyl and dichloropropyl ester, applied in the direction of silicon organic compounds, etc., can solve the problems of high price and application limitation of silicon-based flame retardants, and achieves overcoming volatile reaction, low production cost, and difficulty in dispersion. Effect

Active Publication Date: 2015-06-10
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 excellent properties of suppressing smoke and promoting char formation, people pay attention to them. However, the price of general silicon-based flame retardants is high, and its application is limited. The development of the photovoltaic industry requires a large amount of polysilicon. A large amount of by-products of silicon tetrachloride are produced in the production of polysilicon. The utilization of silicon tetrachloride provides cheap raw materials for the production of silicon-based flame retardants, and can also solve the problem of comprehensive utilization of by-products in the polysilicon industry.

Method used

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  • Flame retardant silicic acid di-(tribromophenyl) dichlorohydrin compound and preparation method thereof
  • Flame retardant silicic acid di-(tribromophenyl) dichlorohydrin compound and preparation method thereof
  • Flame retardant silicic acid di-(tribromophenyl) dichlorohydrin compound and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Embodiment 1 In the 150ml four-neck flask that stirrer, thermometer, dropping funnel and high-efficiency reflux condenser are equipped with and an extremely stretchable and expandable soft sealing sleeve is housed on the condenser upper mouth, replace the nitrogen in the bottle with nitrogen. After the air, add 70ml of dioxane and 8.50g (0.05mol) of silicon tetrachloride, start stirring, and under cooling in an ice-water bath, add 2.90g (0.05mol) of propylene oxide dropwise, and control the temperature at 30°C with the dropping rate Below, after dropping, keep warm at 30°C for 30 minutes, refit the hydrogen chloride absorption device at the top of the condenser, add 33.08g (0.1mol) tribromophenol, raise the temperature to 85°C, keep warm for 4 hours, and cool down after the hydrogen chloride is released. To 40°C, restore the soft sealing sleeve device on the upper port of the condenser tube, then add 4.07g (0.07mol) propylene oxide dropwise, and control the temperature b...

Embodiment 2

[0030]Example 2 In a 150ml four-necked flask equipped with a stirrer, a thermometer, a dropping funnel and a high-efficiency reflux condenser and an extremely flexible and expandable soft seal at the top of the condenser, replace the nitrogen in the bottle with nitrogen. After the air, add 70ml toluene and 8.50g (0.05mol) silicon tetrachloride, start stirring, under ice-water bath cooling, add 2.90g (0.05mol) propylene oxide dropwise, control the temperature below 30°C with the dropping speed, drop After completion, keep the reaction at 30°C for 30 minutes, refit the hydrogen chloride absorption device at the top of the condenser, add 33.08g (0.1mol) tribromophenol, raise the temperature to 90°C, and keep the reaction for 3.5h. After the hydrogen chloride is released, cool down to 40 ℃, restore the soft sealing sleeve device on the upper port of the condenser tube, then add 5.81g (0.1mol) propylene oxide dropwise, and control the temperature below 50°C with the dropping speed. ...

Embodiment 3

[0031] Example 3 In a 150ml four-necked flask equipped with a stirrer, a thermometer, a dropping funnel and a high-efficiency reflux condenser and an extremely flexible and expandable soft seal at the top of the condenser, replace the nitrogen in the bottle with nitrogen. After air, add 70ml of carbon tetrachloride and 8.50g (0.05mol) of silicon tetrachloride, start stirring, and under cooling in an ice-water bath, add 2.90g (0.05mol) of propylene oxide dropwise, and control the temperature at 30°C with the dropping rate Below, after dropping, keep warm at 30°C for 30 minutes, refit the hydrogen chloride absorption device at the top of the condenser, add 33.08g (0.1mol) tribromophenol, raise the temperature to 70°C, keep warm for 6 hours, and cool down after the hydrogen chloride is released. To 40°C, restore the soft sealing sleeve device on the upper port of the condenser tube, then add 4.65g (0.08mol) propylene oxide dropwise, and control the temperature below 50°C with the ...

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Abstract

The invention relates to a flame retardant silicic acid di-(tribromophenyl) dichlorohydrin compound and a preparation method thereof. A structural formula of the compound is as follows as shown in the specification, wherein n is an integer between 0 and 2. The preparation method comprises the steps that equimolar epoxy propane is dropwise added to an organic solution of silicon tetrachloride, and reacts at 30 DEG C for 30min; twice mole of tribromophenol is added, and reacts at 70-100 DEG C for 3-6h; epoxy propane at a certain mole ratio is dropwise added, and reacts at 60-85 DEG C for 4-6h; a solvent and a low-boiling-point object are removed by reduced pressure distillation; and silicic acid di-(tribromophenyl) dichlorohydrin is obtained. Silicic acid di-(tribromophenyl) dichlorohydrin is an excellent antiflaming plasticizer, has charring and dripping prevention functions, has good compatibility with a high polymer material, and can serve as a flame retardant of polyvinyl chloride, unsaturated polyester, polyurethane, epoxy resin and the like, raw materials of silicic acid di-(tribromophenyl) dichlorohydrin are low in cost and 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 bis(tribromophenyl)dichloropropyl silicate 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] Due to the wide application of polymer materials such as flammable plastics, rubber and fibers, the research on flame retardant technology and the rapid development of flame retardant plasticizer industry have been promoted. 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-retardant plasticizers. For this reason, the development of flame-retardant plasticizers, especially multi-e...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/06C08K5/5425
Inventor 王彦林孟凡一
Owner 张家港市乐余科创园投资发展有限公司
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