二丙基次膦酸铝阻燃剂的中试合成与表征

摘要

以一水合次磷酸钠、丙烯和十水合硫酸铝为原料,采用自由基加成法在50 L反应体系中制备了二丙基次膦酸铝(ADPP-50 L)阻燃剂,并利用FTIR、1 HNMR、31PNMR、TGA等对其进行了表征.结果表明:ADPP-50 L阻燃剂的分子结构与预期结构相符,其粒子形状不规则,是由许多0.5～1 μm左右的小粒子聚集而成,其1％热失重温度为335 ℃,5％热失重温度为385℃,显示出良好的热稳定性.ADPP-50 L的产率、磷含量、铝含量、化学结构和热稳定性能等均与实验室制备的ADPP一致,并与理论值相符.%Dipropylphosphinic acid aluminum(ADPP-50 L)flame retardant was synthesized in 50 L reaction system by free radical addition reaction using sodium hypophosphite monohydrate,propylene and aluminium sulfate octadecahydrate as materials,and characterized by FTIR,1HNMR,31 P-NMR and TGA.Results showed that the structure of ADPP-50 L was consistent with the expectations,whichmany particles of irregular shape was consisted of sizes of nearly 0.5 ～ 1 μm small particles.Meanwhile,ADPP-50 L also possessed excellent thermal stability with 1wt％ and 5wt％ mass loss temperature were 335 ℃ and 385 ℃,respectively.The yield,phosphorus content,aluminum content,chemical structure and thermal stability of ADPP-50 L were in accordance with that of ADPP synthesized by laboratory,which were consistent with the theoretical values.