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Tribromophenoxychloropropoxytri(dichloropropyl)silicate compound and preparation method thereof

A technology of tribromophenoxychloropropoxysilicate tris and bromophenoxychloropropoxysilicate tris, which is applied in the field of tribromophenoxychloropropoxysilicate triester compounds and their preparation, It can solve the problems of narrow application range and high price, and achieve the effect of low cost, cheap raw materials and stable physical and chemical properties

Active Publication Date: 2015-02-25
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, silicone-based products are expensive and limited in scope of use.

Method used

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  • Tribromophenoxychloropropoxytri(dichloropropyl)silicate compound and preparation method thereof
  • Tribromophenoxychloropropoxytri(dichloropropyl)silicate compound and preparation method thereof
  • Tribromophenoxychloropropoxytri(dichloropropyl)silicate compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Example 1 In a 100ml four-neck flask equipped with a stirrer, a thermometer, and a high-efficiency reflux condenser, add 10ml of acetonitrile, 5.1g (0.03mol, 3.4ml) of silicon tetrachloride, and drop 50ml of it within 60min at 20°C. A solution of 11.6g (0.03mol) tribromophenylglycidyl ether dissolved in acetonitrile, the dropwise addition process controls the temperature not to exceed 35°C, after the dropwise addition, the temperature is raised to 60°C within 1h, kept for 6h, and then added dropwise within 1h Epichlorohydrin 8.4g (0.09mol), after dripping, keep warm at 70°C for 10h, the pH value of the reaction system reaches 5-6, after the reaction is completed, acetonitrile is removed by distillation under reduced pressure (recycled), and bromophenoxy is obtained as a light yellow liquid Chloropropoxy tris(dichloropropyl)silicate, product yield 94.7%. Its flash point (open cup): 228±5°C, decomposition temperature: 302±5°C, density (25°C): 1.857g / cm 3 , Refractive ind...

Embodiment 2

[0028] Example 2 In a 100ml four-neck flask equipped with a stirrer, a thermometer, and a high-efficiency reflux condenser, add 10ml of dichloroethane, 5.1g (0.03mol, 3.4ml) of silicon tetrachloride, and drop it in 60min at 20°C Add a solution of 11.6g (0.03mol) tribromophenylglycidyl ether dissolved in 50ml dichloroethane, and control the temperature during the dropwise addition to not exceed 35°C. After the dropwise addition, raise the temperature to 60°C within 1h and keep it warm for 5h , then 9.16g (0.099mol) of epichlorohydrin was added dropwise within 1 hour, and after the drop was completed, the temperature was kept at 80°C for 9 hours, and the pH value of the reaction system reached 5-6. Epichlorohydrin (recycled for use) and a small amount of low-boilers were used to obtain tris(dichloropropyl)bromophenoxychloropropoxysilicate as a pale yellow liquid, and the product yield was 95.8%. Its flash point (open cup): 228±5°C, decomposition temperature: 302±5°C, density (25...

Embodiment 3

[0029] Example 3 In a 100ml four-necked flask equipped with a stirrer, a thermometer, and a high-efficiency reflux condenser, add 10ml of dichloroethane, 5.1g (0.03mol, 3.4ml) of silicon tetrachloride, and drop it in 60min at 20°C Add a solution of 11.6g (0.03mol) tribromophenylglycidyl ether dissolved in 50ml of dichloroethane, and control the temperature during the dropwise addition to not exceed 35°C. After the dropwise addition, the temperature will be raised to 70°C within 1h and kept for 4h , then 9.99 g (0.108 mol) of epichlorohydrin was added dropwise within 1 h, and after the drop was completed, 80 ° C was incubated for 8 h, and the pH value of the reaction system reached 5-6. After the reaction was completed, dichloroethane and excess Epichlorohydrin (recycled for use) and a small amount of low-boilers were used to obtain tris(dichloropropyl)bromophenoxychloropropoxysilicate, a light yellow liquid, with a yield of 97.6%. Its flash point (open cup): 228±5°C, decomposi...

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Abstract

The invention relates to a silicon-halogen synergic flame retardant tribromophenoxychloropropoxytri(dichloropropyl)silicate compound. The compound has the structural formula shown in the specification, wherein n is an integer from 0 to 3. The preparation method comprises the following steps of: enabling the tribromophenylepoxypropyl ester and silicon tetrachloride with an equal molar ratio to react in an organic solvent at 60-80 DEG C for 4-6 hours; dropwise adding epoxy chloropropane with a certain molar ratio, and reacting at 70-100 DEG C for 6-10 hours; and performing reduced-pressure distillation to remove the solvent and excessive epoxy chloropropane to obtain light yellow liquid tribromophenoxychloropropoxytri(dichloropropyl)silicate. The product provided by the invention is suitable to be used as a flame retardant 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 tribromophenoxy chloropropoxy tris(dichloropropyl)silicate compound and a preparation method thereof. Tribromophenoxy chloropropoxysilicate tris(dichloropropyl) Silicon-halogen synergistic flame retardant, suitable for flame retardants of polyvinyl chloride, polyurethane, epoxy resin, unsaturated resin and other materials. Background technique [0002] Polymer materials are used more and more widely, but because of their flammable characteristics, they often cause fires, thus promoting the rapid development of flame retardant science and technology. Flame retardant plasticizer is a polymer material processing aid with both 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 are few excellent flame-retardant plasticizers, and people always expect to develop new flame-retardant plasticizers with high effi...

Claims

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Application Information

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