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
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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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