Flame retardant tribromophenoxychloropropoxytri(chloropropyl) silicate compound and preparation method thereof

A technology of tribromophenoxy chloropropoxysilicate tris and bromophenoxy chloropropoxysilicate tris, which is applied in flame retardant tribromophenoxy chloropropoxysilicate triester compound and its In the field of preparation, it can solve the problems of high price, few varieties and limitations of flame retardant plasticizers, and achieve the effects of low cost, good plasticization and good processing performance

Active Publication Date: 2012-10-17
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

At present, there are few varieties of flame retardant plasticizers, and the market for new high-efficiency, low-toxicity, and low-cost flame retardant plasticizers is urgently needed
Especially after the European Union proposed a ban on halogenated flame retardants, it is difficult to find suitable substitutes for halogenated flame retardants, and how to reduce the amount of halogenated flame retardants added to reduce the toxicity of combustion, that is, to develop high-efficiency halogenated flame retardants Flame retardants have become an important subject of research; silicon-based flame retardants have attracted people's attention due to their excellent performance in suppressing smoke and promoting carbon formation, but they are limited by their high price.

Method used

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  • Flame retardant tribromophenoxychloropropoxytri(chloropropyl) silicate compound and preparation method thereof
  • Flame retardant tribromophenoxychloropropoxytri(chloropropyl) silicate compound and preparation method thereof
  • Flame retardant tribromophenoxychloropropoxytri(chloropropyl) silicate compound and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Example 1 In a 100ml three-necked flask equipped with a stirrer, a thermometer, and a high-efficiency reflux condenser, 10ml of tetrahydrofuran and 0.03mol (5.1g) of silicon tetrachloride were added, and at 20°C, 0.03 mol (11.6g) solution of tribromophenylglycidyl ether, the dropwise addition process controls the temperature not to exceed 35°C, after the drop is completed, the temperature rises to 60°C within 1 hour, keeps the temperature for 6 hours, and then cools down to 35°C, The upper port is equipped with an extremely stretchable and inflatable soft sealing sleeve. Under cooling conditions, add 0.09mol (5.22g) propylene oxide dropwise under the liquid surface within 1 hour, and control the temperature at a rate not exceeding 45°C, and react at 45°C after dropping. After 1 hour, the temperature was raised to 50°C for 5 hours, and the pH reached 5-6. After the reaction was completed, tetrahydrofuran (recycled) was removed by distillation at atmospheric pressure, and ...

Embodiment 2

[0027] Example 2 In a 100ml three-necked flask equipped with a stirrer, a thermometer, and a high-efficiency reflux condenser, 10ml of chloroform and 0.03mol (5.1g) of silicon tetrachloride were added, and at 20°C, 0.03 mol (11.6g) solution of tribromophenylglycidyl ether, the dropwise addition process controls the temperature not to exceed 35°C, after the drop is completed, the temperature rises to 60°C within 1 hour, keeps the temperature for 5 hours, and then cools down to 35°C. The upper port is equipped with an extremely stretchable and inflatable soft sealing sleeve. Under cooling conditions, add 0.099mol (5.75g) propylene oxide dropwise under the liquid surface within 1 hour, and control the temperature at a rate not exceeding 45°C, and react at 45°C after dropping. After 1 hour, the temperature was raised to 55°C for 4 hours, and the pH reached 5-6. After the reaction was completed, the excess propylene oxide and chloroform (recycled) were removed by normal pressure dis...

Embodiment 3

[0028]Example 3 In a 100ml three-necked flask equipped with a stirrer, a thermometer, and a high-efficiency reflux condenser, add 10ml of acetonitrile, 0.03mol (5.1g) of silicon tetrachloride, and dropwise add 0.03mol (5.1g) of silicon tetrachloride dissolved in 50ml of acetonitrile at 20°C within 50min. mol (11.6g) solution of tribromophenylglycidyl ether, the dropwise addition process controls the temperature not to exceed 35°C, after the drop is completed, the temperature rises to 70°C within 1 hour, keeps the temperature for 4 hours, and then cools down to 35°C. The upper port is equipped with an extremely stretchable and inflatable soft sealing sleeve. Under cooling conditions, 0.108mol (6.26g) of propylene oxide is added dropwise under the liquid surface within 1 hour, and the temperature is controlled by the dropping speed to not exceed 45°C. After the drop is completed, it will react at 45°C. After 1 hour, the temperature was raised to 60°C for 3 hours, and the pH reach...

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Abstract

The invention relates to a flame-retardant plasticizer tribromophenoxychloropropoxytri(chloropropyl) silicate compound with synergic flame retardance of silicon, chlorine and bromine and a preparation method thereof. The compound has the structural formula shown in the specification. The preparation method comprises the following steps of: at 20 DEG C, dropwise adding the organic solvent solution of tribromophenylepoxypropyl ester into silicon tetrachloride with an equal molar ratio; keeping the temperature at 60-80 DEG C and reacting for 4-6 hours; cooling to 35 DEG C; dropwise adding epoxypropane with a certain molar ratio; keeping the temperature at 50-70 DEG C and reacting for 3-5 hours; and purifying to obtain light yellow liquid tribromophenoxychloropropoxytri(chloropropyl) silicate. The compound is suitable to be used as a flame-retardant plasticizer of polyvinyl chloride, polyurethane, epoxy resin, unsaturated resin and the like; and the production technology is simple, the equipment investment is low, the cost is low, and the industrial production is easy to realize.

Description

technical field [0001] The invention relates to a flame retardant tribromophenoxy chloropropoxy tris(chloropropyl)silicate compound and a preparation method thereof, tribromophenoxy chloropropoxysilicate tris(chloropropyl)silicate It is a high-efficiency flame retardant that is synergistically flame-retardant by the three elements of silicon, chlorine, and bromine. It is suitable for flame-retardant plasticizers such as polyvinyl chloride, polyurethane, epoxy resin, and unsaturated resin. Background technique [0002] With the wide application of polymer materials, because of its flammability, it often causes fires and poses a serious threat to people's lives and property, thus promoting the research of flame retardant technology and the rapid development of flame retardant plasticizer 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 ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/06C08K5/5415C08K13/02C08L27/06
Inventor 王彦林范腊梅俞春雷刘颖棋
Owner 张家港市乐余科创园投资发展有限公司
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