Polymeric phosphorus-containing flame retardant with DOPO as lateral group and preparation method thereof
A phosphorus flame retardant, polymeric technology, applied in the field of polymeric phosphorus-containing flame retardants and its preparation, can solve the problems of large environmental pollution, leaching, poor compatibility of polymer matrix, etc., and achieve good flame retardant effect , Overcoming the effect of low thermal decomposition temperature and good expansion into charcoal
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[0024] Example 1:
[0025] In a 500ml three-necked flask equipped with a mechanical stirrer, a nitrogen inlet and a condenser, 29.7g (0.10mol) pentaerythritol diphosphate diphosphoryl chloride, 150ml anhydrous acetonitrile and 32.4g (0.10mol) 9,10-dihydrogen were added -9-oxa-10-phosphaphenanthrene-10-oxide-hydroquinone, heated to 80°C, reacted with continuous stirring until no HCl gas was released, cooled to room temperature, and the solvent was removed under reduced pressure to obtain pink color solid product. The yield was 95%, the melting point was 220°C.
[0026] Infrared analysis of the resulting product, 583-541 cm in pentaerythritol diphosphate diphosphoryl chloride -1 The characteristic peak of P-Cl bond disappears, 929, 1189cm -1 P-O-Ph characteristic peak, 1442cm -1 P-Ph characteristic peak appeared. It can be seen that the product of this example is a polymeric phosphorus-containing flame retardant whose side group is 9,10-dihydro-9-oxa-10-phosphaphenanthrene...
Example Embodiment
[0029] Example 2:
[0030] In a 500ml three-necked flask equipped with a mechanical stirrer, a nitrogen inlet and a condenser, 29.7g (0.10mol) pentaerythritol diphosphate diphosphoryl chloride, 150ml anhydrous acetonitrile and 39.8g (0.10mol) 9,10-dihydrogen were added -9-oxa-10-phosphaphenanthrene-10-oxide-p-naphthalene diol, heated to 80°C, reacted under continuous stirring until no HCl gas was released, cooled to room temperature, and the solvent was removed under reduced pressure to obtain a pink color the solid product. Yield 92%, melting point 235°C.
[0031] Infrared analysis of the resulting product, 583-541 cm in pentaerythritol diphosphate diphosphoryl chloride -1 The characteristic peak of P-Cl bond disappears, 929, 1189cm -1 P-O-Ph characteristic peak, 1442cm -1 P-Ph characteristic peak appeared. It can be seen that the product of this example is a polymeric phosphorus-containing flame retardant with a side group of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-1...
Example Embodiment
[0034] Example 3:
[0035] In a 500ml three-necked flask equipped with a mechanical stirrer, a nitrogen inlet and a condenser, 29.7g (0.10mol) pentaerythritol diphosphate diphosphoryl chloride, 150ml anhydrous acetonitrile and 39.8g (0.10mol) 9,10-dihydrogen were added -9-oxa-10-phosphaphenanthrene-10-oxide-bisphenol A, warmed to 80°C, reacted with continuous stirring until no HCl gas was released, cooled to room temperature, and removed the solvent under reduced pressure to obtain a red solid product. Yield 85%, melting point 240°C.
[0036] Infrared analysis of the resulting product, 583-541 cm in pentaerythritol diphosphate diphosphoryl chloride -1 The characteristic peak of P-Cl bond disappears, 929, 1189cm -1 P-O-Ph characteristic peak, 1442cm -1 P-Ph characteristic peak appeared. It can be seen that the product obtained in this example is a polymeric phosphorus-containing flame retardant with a side group of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide.
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