A polyhydroxy silicon nitrogen type flame retardant and its preparation method and application in flame retardant polyurethane rigid foam material
A polyurethane rigid foam and flame retardant technology, which is applied in the field of silicon nitrogen flame retardant and full water foamed rigid polyurethane foam, can solve the problems of low strength, brittle foam, poor dimensional stability, etc., and achieve high resistance Flammability, enhanced thermal stability and flame retardancy, high mechanical properties
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Embodiment 1
[0032]Preparation of flame retardant:
[0033] 1. Under the condition of stirring at room temperature, 5.0g (0.041mol) p-hydroxybenzaldehyde was dissolved in 75g (95ml) ethanol solution to form A solution, and 3.0g (0.0164mol) 4,4'-diaminobiphenyl was dissolved in 30g (38ml) ) in ethanol solution to form B solution. Add B solution dropwise to A solution at 30°C. The time for dropping is controlled at 2h. Polyols;
[0034] 2. Under the protection of nitrogen, add the silicon hydride trimethoxyhydrosilane to the mixing system in the above 1, and at the same time add 0.25 g of catalyst zinc chloride, raise the temperature of the reaction mixture to 85 ° C, react for 16 hours, and cool to room temperature It was poured into 250g (386ml) of petroleum ether and stirred for 1.5h, filtered to obtain a solid product, washed 5 times with cold ethanol solution, and vacuum-dried at 75°C for 24h to obtain a polyhydroxyphenylcyclosilane nitrogen-type flame retardant.
[0035] The structur...
Embodiment 2
[0052] Preparation of flame retardant:
[0053] 1. Under the condition of stirring at room temperature, 5.0g (0.041mol) p-hydroxybenzaldehyde was dissolved in 40g ethanol solution to form A solution, and 0.0205mol3,3'-dimethoxy 4,4'-diaminobiphenyl was dissolved in 25g ethanol Solution B is formed in the solution, and solution B is added dropwise to solution A at 25°C. The dropping time is controlled at 1h. After the addition, the temperature is raised to 40°C and reacted for 2h to obtain a polyhydroxyl compound containing a carbon-nitrogen double bond. compound;
[0054] 2. Under the protection of nitrogen, add the silicon hydride compound trimethoxyhydrosilane to the mixing system in the above 1, and at the same time add 0.1 g of catalyst zinc chloride, raise the temperature of the reaction mixture to 70 ° C, react for 8 hours, and cool to room temperature It was poured into 175g of petroleum ether and stirred for 0.5h, filtered to obtain a solid product, washed 5 times wit...
Embodiment 3
[0072] Preparation of flame retardant:
[0073] 1. Under the condition of stirring at room temperature, 5.0g (0.041mol) p-hydroxybenzaldehyde is dissolved in 75g (95ml) ethanol solution to form A solution, and 0.0164mol3,3'-diaminophenyl sulfone is dissolved in 30g (38ml) ethanol solution to form B solution, add B solution to A solution dropwise at 30°C, the dropping time is controlled at 1h, after the dropwise addition is completed, the temperature is raised to 55°C, and reacted for 3h to obtain a polyhydroxy compound containing a carbon-nitrogen double bond;
[0074] 2. Under the protection of nitrogen, add the silicon hydride trimethoxyhydrosilane to the mixing system in the above 1, and at the same time add 0.25 g of catalyst zinc chloride, raise the temperature of the reaction mixture to 85 ° C, react for 10 h, and cool to room temperature It was poured into 250g (386ml) of petroleum ether and stirred for 1.5h, filtered to obtain a solid product, washed 5 times with cold ...
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