A kind of diradical compound based on phosphazene and triazine group and preparation method thereof
A technology of triazine compounds and triazine groups, applied in the fields of flame retardants and their preparation, double-base compounds based on phosphazene and triazine groups and their preparations, achieving high char formation rate, good processability, thermal good stability effect
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Embodiment 1
[0031] Step (1). Dissolve 2.00g cyanuric chloride in 15ml tetrahydrofuran solution, join in the tetrahydrofuran solution 40ml that is dissolved with 0.68g ethanolamine, add sodium carbonate 1.15g, in N 2 In the atmosphere, stir at -15°C for 2 hours to obtain 2,4-dichloro-6-hydroxyethylamino-1,3,5-triazine compound;
[0032] Step (2). Add 0.68g of hexachlorocyclotriphosphazene in 30ml of tetrahydrofuran to the 2,4-dichloro-6-hydroxyethylamino-1,3,5-triazine compound, add 1.15g of sodium carbonate, and heat at 50°C Condensation and reflux under stirring conditions for 5 hours;
[0033] Step (3). Add 1.30 g of ethylenediamine in 10 ml of tetrahydrofuran to the reaction solution; raise the temperature to 40° C., react under stirring and condensation conditions for 3 hours, continue to raise the temperature to 80° C., and react under stirring and condensation conditions 3 hours;
[0034] Step (4). After the reaction, suction filtration, water washing, and drying are performed to ...
Embodiment 2
[0037] Step (1). 4.00g cyanuric chloride is dissolved in 30ml acetone solution, joins in the acetone solution 50ml of 1.36g ethanolamine, adds potassium hydroxide 1.22g, in N 2 In the atmosphere, stir at -10°C for 2 hours to obtain 2,4-dichloro-6-hydroxyethylamino-1,3,5-triazine compound;
[0038] Step (2). Add 1.36g of hexachlorocyclotriphosphazene in 40ml of acetone solution to 2,4-dichloro-6-hydroxyethylamino-1,3,5-triazine compound, add 1.22.00g of potassium hydroxide, Condensation and reflux for 5 hours under stirring at 50°C;
[0039] Step (3). Add 2.80 g of hexamethylenediamine in 15 ml of acetone solution to the reaction solution; raise the temperature to 45° C., react under stirring and condensation conditions for 3 hours, continue to raise the temperature to 85° C., and react under stirring and condensation conditions 3 hours;
[0040] Step (4). After the reaction, suction filtration, water washing, and drying are performed to obtain a diradical compound based on p...
Embodiment 3
[0041]Step (1). 6.00g cyanuric chloride is dissolved in 40ml ethyl acetate solution, joins in the ethyl acetate solution 60ml that is dissolved with 2.05g ethanolamine, adds sodium hydroxide 1.30g, in N 2 In the atmosphere, stir at -5°C for 2.5 hours to obtain 2,4-dichloro-6-hydroxyethylamino-1,3,5-triazine compound;
[0042] Step (2). Add 2.05g of hexachlorocyclotriphosphazene in 50m ethyl acetate solution to 2,4-dichloro-6-hydroxyethylamino-1,3,5-triazine compound, add 1.30g of sodium hydroxide , condensed and refluxed for 5.5 hours under stirring at 55°C;
[0043] Step (3). Add 6.90 g of p-phenylenediamine in 25 ml of ethyl acetate solution to the reaction solution; raise the temperature to 55 ° C, stir and condense for 3 hours, continue to raise the temperature to 85 ° C, stir and condense Under conditions, react for 3 hours;
[0044] Step (4). After the reaction, suction filtration, water washing, and drying are performed to obtain a diradical compound based on phosphaz...
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