Tris [2-(dimethylthiopepaoxysilyloxy) ethyl] isocyanurate compound and preparation method thereof
A technology of tris and dimethyl thioisocyanurate, applied in the field of tris{2-[dimethylsilyloxy]ethyl} isocyanurate compounds and preparation thereof, can solve application limitations, The problem of releasing harmful gases, etc., achieves the effect of large molecular weight, low volatility, and prevention of secondary combustion
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Embodiment 1
[0029] Embodiment 1 In the 250ml four-necked bottle that stirrer, thermometer and condensation tube are equipped with, and drying tube and hydrogen chloride absorption device are equipped with at the top of condensation tube, replace the air in the bottle with nitrogen, add 8.74g (0.0333mol ) Tris (2-hydroxyethyl) isocyanurate, 90ml dioxane and 12.91g (0.1mol) dimethyldichlorosilane, heat up to 70°C, keep warm for 5h; after the HCl gas is released, Cool down to below 30°C, add 19.61g (0.1mol) of SPEPA, heat up to 100°C, keep warm for 6 hours; after the HCl gas is released, add 0.36g of melamine, adjust the pH of the system to 5-6, filter with suction, and depressurize the filtrate Distill off the solvent and a small amount of low-boiling matter, add 100ml of distilled water, stir for 0.5h, filter with suction, and dry in vacuo to obtain tris[2-(dimethylthioPEPAoxysilyloxy)ethyl]isocyanurate , yield 87.8%.
Embodiment 2
[0030] Embodiment 2 In the 250ml four-necked bottle that agitator, thermometer and condensation tube are equipped with, and drying tube and hydrogen chloride absorption device are equipped with on the top of condensation tube, replace the air in the bottle with nitrogen, add 8.74g (0.0333mol ) Tris (2-hydroxyethyl) isocyanurate, 120ml acetonitrile and 12.91g (0.1mol) dimethyldichlorosilane, heat up to 60°C, keep warm for 8h; after the HCl gas is released, cool down to 30 Below ℃, add 20.92g (0.1067mol) SPEPA, raise the temperature to 70℃, and keep it warm for 14h; after the HCl gas is released, add 0.5g melamine, adjust the pH of the system to 5-6, filter with suction, and distill the filtrate to remove the solvent under reduced pressure and a small amount of low boiling point matter, add 100ml of distilled water, stir for 0.5h, filter with suction, and dry in vacuo to obtain tris[2-(dimethylthioPEPAoxysilyloxy)ethyl]isocyanurate, the yield 90.4%.
Embodiment 3
[0031]Embodiment 3 In the 250ml four-necked bottle that stirrer, thermometer and condensation tube are equipped with, and drying tube and hydrogen chloride absorption device are equipped with at the top of condensation tube, replace the air in the bottle with nitrogen, add 8.74g (0.0333mol ) Tris (2-hydroxyethyl) isocyanurate, 150ml acetonitrile and 12.91g (0.1mol) dimethyldichlorosilane, heat up to 70°C, keep warm for 5h; after the HCl gas is released, cool down to 30°C Below ℃, add 22.88g (0.1167mol) SPEPA, raise the temperature to 80℃, keep warm for 10h; after the HCl gas is released, add 0.8g melamine, adjust the pH of the system to 5-6, filter with suction, and distill the filtrate to remove the solvent under reduced pressure and a small amount of low boiling point matter, add 120ml of distilled water, stir for 0.5h, filter with suction, and dry in vacuo to obtain tris[2-(dimethylthioPEPAoxysilyloxy)ethyl]isocyanurate, the yield 93.2%.
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