含磷/氮/硫协效阻燃剂的合成及对环氧树脂的阻燃作用

Synthesis of a Phosphorus/Nitrogen/Sulphur containing synergistic flame retardant and its flame retardancy on epoxy resin

本文以DOPO(9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物)、苯甲醛和4,4’-二氨基二苯砜(DDS)为原料,一锅法合成了含磷、氮、硫的化合物PNS。以PNS为阻燃剂,双酚A型树脂DGEBA为基材,DDS为环氧固化剂,制备了阻燃环氧固化物PNS/DGEBA/DDS,研究了PNS对DGEBA阻燃性能的影响,并与商业化有机磷阻燃剂DOPO作对比,同时初步探讨了PNS的阻燃机理。研究结果表明,PNS呈现磷/氮/硫协效阻燃作用,具有比DOPO更优异的残炭生产促进作用、抑烟效果和阻燃作用。在体系磷含量为1.5 wt%时,PNS-1.5/DGEBA/DDS的LOI值高达33.2%,并获UL 94最高阻燃级别V-0级,总烟释放量相较于DOPO-1.5/DGEBA/DDS降低15.4%,DGEBA/DDS降低2.86%,呈现良好的抑烟性能。

A phosphorus-nitrogen-sulphur containing compound named PNS was synthesized by 9,10-Dihydro-9-oxa-10-phosphaphenanthrene 10-oxide(DOPO),benzaldehyde and 4,4’-diaminodiphenylsulfone(DDS)in one pot.With PNS as the flame retardant,DGEBA as the base material and DDS as the epoxy curing agent,the corresponding flame retardant epoxy resin thermosets PNS/DGEBA/DDS were prepared.Then the influences of PNS on the flame retardancy of DGEBA/DDS were investigated and compared with DOPO.The flame-retardant mechanisms of modified thermosets were also discussed.The results showed that PNS presented a P/N/S synergistic flame retardant effect,and showed more excellent properties such as formation of char residues,smoke suppression and flame retardancy in comparation with DOPO.With the addition of 1.5 wt%phosphorus,PNS-1.5/DGEBA/DDS showed a LOI value of 33.2%and obtained the highest UL94 level of V-0,and also presented a lower total smoke release than DOPO-1.5/DGEBA/DDS and DGEBA/DDS by 15.4%and 2.86%,respectively.