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Tribromophenoxychloropropoxytri(dichloropropyl)silicate compound and preparation method thereof

A technology of tribromophenoxychloropropoxysilicate tris and bromophenoxychloropropoxysilicate trisilicate, which is applied in the field of tribromophenoxychloropropoxysilicate triester compounds and their preparation, It can solve the problems of high price and narrow application range, and achieve the effects of low cost, good symmetry and high flame retardant efficiency

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

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-necked 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 at 20° C., add 50ml dropwise within 60min. The solution of 11.6g (0.03mol) tribromophenyl glycidyl ether dissolved in acetonitrile, the temperature of the dropwise addition process is controlled not to exceed 35°C. After dropping, the temperature is raised to 60°C within 1 hour, and the temperature is kept for 6 hours, and then dropwise added within 1 hour. 8.4 g (0.09 mol) of epichlorohydrin was added, and the reaction was kept at 70°C for 10 hours after dropping, and the pH value of the reaction system reached 5-6. The reaction was completed, and then the acetonitrile was distilled off under reduced pressure (recycling) to obtain a pale yellow liquid bromophenoxy Tris(dichloropropyl) chloropropoxysilicate, the product yield is 94.7%. Its flash point (open cup): 228±5℃, decomp...

Embodiment 2

[0028] Embodiment 2 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 at 20° C., dropwise in 60min. A solution of 11.6g (0.03mol) tribromophenylglycidyl ether dissolved in 50ml of dichloroethane was added, and the temperature during the dropwise addition was controlled not to exceed 35°C. Then, 9.16 g (0.099 mol) of epichlorohydrin was added dropwise within 1 h, and the reaction was kept at 80 °C for 9 h after the dropping, and the pH value of the reaction system reached 5-6. The reaction was completed, and then the dichloroethane and excess were removed by distillation under reduced pressure. Epichlorohydrin (recycling) and a small amount of low-boiling substances were used to obtain tris(dichloropropyl) bromphenoxychloropropoxysilicate as a light yellow liquid, and the product yield was 95.8%. Its flash point (open cup): 228±5℃, decomposi...

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 ethylene dichloride, 5.1g (0.03mol, 3.4ml) of silicon tetrachloride, and at 20° C., dropwise within 60min. A solution of 11.6g (0.03mol) tribromophenylglycidyl ether dissolved in 50ml of dichloroethane was added, and the temperature during the dropwise addition was controlled not to exceed 35°C. Then, 9.99g (0.108mol) of epichlorohydrin was added dropwise within 1h, and the reaction was kept at 80°C for 8h after the drop was completed. The pH value of the reaction system reached 5-6, and the reaction was completed. Then, dichloroethane and excess ethylene dichloride were removed by distillation under reduced pressure. Epichlorohydrin (recycling) and a small amount of low-boiling substances were used to obtain light yellow liquid bromophenoxychloropropoxysilicate tris(dichloropropyl) ester, and the product yield was 97.6%. Its flash point (ope...

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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 tris(dichloropropyl) tribromophenoxychloropropoxysilicate compound and a preparation method thereof. Tris(dichloropropyl) tribromophenoxychloropropoxysilicate belongs to the genus Silicon-halogen synergistic flame retardant, suitable for flame retardant of polyvinyl chloride, polyurethane, epoxy resin, unsaturated resin and other materials. Background technique [0002] The application of polymer materials is becoming more and more extensive, but because of its flammable characteristics, it often causes fires, which promotes the rapid development of flame retardant science and technology. Flame retardant plasticizer is a processing aid for polymer materials 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 varieties of excellent flame retardant plasticizers, and people always expect ...

Claims

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Application Information

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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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