Fire retardant dimethyl silicate di-thio-phosphonia trioxide hybrid cage ring octyl methyl ester compound and preparation method thereof
The technology of dimethylsilicic acid and thiophosphati is applied in the field of flame retardant dimethylsilicic acid bisthiophosphatrioxane octyl methyl ester compound and its preparation, and can solve the problem of low decomposition temperature. , can not adapt to the high temperature processing of polymer materials and other problems, to achieve the effect of high decomposition temperature, good application development prospects, high flame retardant efficiency
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Embodiment 1
[0027] Example 1 In a 250ml four-necked reaction flask equipped with a stirrer, a thermometer and a fractionation device, replace the air with nitrogen, and at a temperature of 25°C, add 21.56g (0.11mol) of 1-thiophospha-4-hydroxymethyl Base-2,6,7-trioxabicyclo[2.2.2]octane, 6.01g (0.05mol) dimethyldimethoxysilane and 50mL dioxane are heated to reflux, and the temperature of system reflux varies with The temperature rises as the reaction progresses, and finally keeps at 95°C for fractional distillation reaction for 7 hours. The cake was washed with 25 mL of absolute ethanol, filtered with suction, and dried to obtain a white solid powder of bis-1-thiophospha-2,6,7-trioxabicyclo[2.2.2]octyl- 4-Methyl ester, yield 90.1%.
Embodiment 2
[0028] Example 2 In a 250ml four-necked reaction flask equipped with a stirrer, a thermometer and a fractionation device, replace the air with nitrogen, and at a temperature of 25°C, add 39.23g (0.20mol) of 1-thiophospha-4-hydroxymethyl Base-2,6,7-trioxabicyclo[2.2.2]octane, 6.01g (0.05mol) dimethyldimethoxysilane and 100mL ethylene glycol dimethyl ether, warming up to reflux, system reflux The temperature rises with the progress of the reaction, and finally keeps at 80°C for 9 hours of fractionation reaction, and the temperature of the top of the fractionation column is controlled not to be higher than 65°C. After the methanol generated by fractionation reaches the theoretical amount, the reaction is completed, and the temperature is lowered to 25°C. Suction filtration , the filter cake was washed with 40 mL of methanol, suction filtered, and dried to obtain a white solid powder of bis-1-thiophospha-2,6,7-trioxabicyclo[2.2.2]octyl- 4-Methyl ester, yield 89.6%.
Embodiment 3
[0029]Example 3 In a 250ml four-necked reaction flask equipped with a stirrer, a thermometer and a fractionation device, replace the air with nitrogen, and at a temperature of 25°C, add 19.62g (0.10mol) of 1-thiophospha-4-hydroxymethyl Base-2,6,7-trioxabicyclo[2.2.2]octane, 6.01g (0.05mol) dimethyldimethoxysilane and 30mL dioxane are heated to reflux, and the temperature of system reflux varies with As the reaction proceeds, the fractional distillation reaction is finally maintained at 100°C for 5 hours, and the temperature at the top of the fractionation column is controlled not to be higher than 65°C. After the methanol generated by fractional distillation reaches the theoretical amount, the reaction is completed, and the temperature is lowered to 25°C. The cake was washed with 35 mL of absolute ethanol, filtered with suction, and dried to obtain a white solid powder of bis-1-thiophospha-2,6,7-trioxabicyclo[2.2.2]octyl-dimethylsilicate 4-Methyl ester, yield 87.3%.
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