A kind of preparation method of silicon, nitrogen, halogen multi-element synergistic flame retardant compound
A synergistic flame-retardant, dimethyl dihalopropoxysilyloxyhalopropyl technology, which is applied in the field of isocyanurate triester preparation, can solve the problem of lower mechanical properties of substrates, moisture-absorbing processing properties, Low flame retardant efficiency and other issues, to achieve excellent flame retardant effect, strong water resistance, and good compatibility
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Embodiment 1
[0030]Example 1 In a 250ml four-necked bottle equipped with a stirrer, a thermometer and a condenser tube, and a drying tube on the top of the condenser tube, replace the air in the bottle with nitrogen, and add 9.91g (0.0333mol) of isocyanurate Acetate triglycidyl ester, 70ml dioxane and 12.91g (0.1mol) dimethyldichlorosilane, heat up to 90°C for 1h, keep warm for 6h; cool down to below 40°C, connect a hydrogen chloride absorption device to the drying tube, Add 21.79g (0.1mol) of 1,3-dibromo-2-propanol dropwise, and control the reaction temperature not higher than 60°C at the rate of addition, raise the temperature to 100°C after dropping, and keep the reaction for 6 hours; after the HCl gas is released , add 0.4g melamine, adjust the pH of the system to 5-6, filter with suction, distill the filtrate under reduced pressure to remove the solvent and a small amount of low boiling point substances, then add 30ml of petroleum ether, stir for 0.5h, let stand, separate the lower lay...
Embodiment 2
[0031] Example 2 In a 250ml four-necked bottle equipped with a stirrer, a thermometer and a condenser tube, and a drying tube on the top of the condenser tube, replace the air in the bottle with nitrogen, and add 9.91g (0.0333mol) of isocyanurate Acetate triglycidyl ester, 100ml acetonitrile and 21.8g (0.1mol) dimethyldibromosilane, heat up to 80°C, keep warm for 7 hours; cool down to below 40°C, connect the hydrogen bromide absorption device to the drying tube, drop 23.25g (0.1067mol) 1,3-dibromo-2-propanol, control the reaction temperature not higher than 60°C at the rate of addition, raise the temperature to 80°C after the drop, keep the temperature for 7 hours; after the HBr gas is released, add 1g of melamine, adjust the pH of the system to 5-6, filter with suction, distill the filtrate under reduced pressure to remove the solvent, excess 1,3-dibromo-2-propanol (recycled) and a small amount of low boiling point matter, then add 50ml petroleum ether, Stir for 0.5h, let it ...
Embodiment 3
[0032] Example 3 In a 250ml four-necked bottle equipped with a stirrer, a thermometer and a condenser tube, and a drying tube on the top of the condenser tube, replace the air in the bottle with nitrogen, and add 9.91g (0.0333mol) of isocyanurate Acid triglycidyl ester, 50ml diethylene glycol dimethyl ether and 12.91g (0.1mol) dimethyl dichlorosilane, heat up to 100°C for 1h, keep the temperature for 5h; cool down to below 40°C, connect hydrogen chloride to the drying tube Absorption device, add 25.43g (0.1167mol) 1,3-dibromo-2-propanol dropwise, control the reaction temperature not higher than 60°C at the rate of addition, raise the temperature to 110°C after dropping, keep warm for 5 hours; wait for HCl gas After the release, add 1.2g of melamine, adjust the pH of the system to 5-6, filter with suction, and distill off the filtrate under reduced pressure to remove the solvent, excess 1,3-dibromo-2-propanol (recycled for use) and a small amount of low boiling point matter, Th...
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