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
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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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