Nitrogen-boron structural type flame-retardant polyether polyol as well as preparation method and application thereof
A technology of polyether polyol and flame-retardant polyether, which is applied in the field of nitrogen-boron structure flame-retardant polyether polyol, can solve the problems of enhancing the mechanical properties of polyurethane materials, and achieve enhanced thermal stability, good fluidity, and technological conditions simple effect
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Embodiment 1
[0043] (1) Add 25g of 4-carboxyphenylboronic acid and 179g of thionyl chloride into a round-bottomed flask, mix and stir, heat up to 60°C, react for 9 hours, heat up to 90°C, and remove moisture and solvent under vacuum conditions of -0.15MPa , to obtain white powder arylated boroxane;
[0044] (2) With melamine as starting raw material, 19g melamine is dissolved in the NaOH aqueous solution of 76g mass concentration 10%, 25g arylated boroxane is dissolved in the 75g methylene chloride solution, two solutions are mixed and stirred rapidly, react The temperature is 0°C, the stirring time is 10min, and the stirring speed is 150 rpm; after the reaction is completed, filter and wash with 80°C distilled water for 3 times, and then dry in a 60°C drying oven for 4 hours to obtain a boron nitrogen compound, a melamine-modified aryl Boroxane compounds;
[0045] (3) In a three-necked flask, add 50 g of melamine-modified arylated boroxane compound, 50 g of formaldehyde solution with a m...
Embodiment 2
[0050] (1) Add 25g of 4-carboxyphenylboronic acid and 358g of thionyl chloride into a round-bottomed flask, mix and stir, heat up to 90°C, react for 18 hours, heat up to 120°C, and remove moisture and solvent under -0.10MPa vacuum condition , to obtain white powder arylated boroxane;
[0051] (2) Taking melamine as starting raw material, 32g melamine is dissolved in 220g mass concentration 25% NaOH aqueous solution, 25g arylated boroxane is dissolved in 125g methylene chloride solution, two solutions are mixed and stirred rapidly, the reaction temperature 8°C, stirring time 20min, stirring speed 250 rpm; filter after the reaction, wash with 95°C distilled water for 5 times, and then dry in a 90°C drying oven for 8h to obtain boron nitrogen compound, melamine-modified arylation Boroxane compounds;
[0052] (3) In a three-necked flask, add 50g of melamine-modified arylated boroxane compound, 78g of formaldehyde solution with a mass concentration of 30%, and 158g of polyether po...
Embodiment 3
[0057] (1) Add 25g of 4‐carboxyphenylboronic acid and 280g of thionyl chloride in proportion to a round bottom flask, mix and stir, heat up to 80°C, react for 15 hours, heat up to 100°C, and remove moisture under ‐0.085MPa vacuum condition And solvent, obtain the boroxane of white powder arylation;
[0058] (2) Taking melamine as starting raw material, 25g melamine is dissolved in 100g mass concentration 15% NaOH aqueous solution, 25g arylated boroxane is dissolved in 100g methylene chloride solution, two solutions are mixed and stirred rapidly, the reaction temperature 5°C, stirring time 15min, stirring speed 200 rpm; filter after the reaction, wash with 90°C distilled water 4 times, and then dry in a 75°C drying oven for 6h to obtain boron nitrogen compound, melamine-modified arylation Boroxane compounds;
[0059] (3) In a three-necked flask, add 35g of melamine-modified arylated boroxane compound, 65g of formaldehyde solution with a mass concentration of 25%, and 56g of po...
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