摘要
以三聚氯氰、对羟基苯甲醛和9,10-二氢-9-氧杂-10-膦菲-10-氧化物(DOPO)为主要原料,经两步反应合成了一种新型含三嗪结构氧杂膦菲阻燃剂PN-FR。第一步反应以三聚氯氰、对羟基苯甲醛为原料,二氯甲烷和水为混合溶剂,相转移催化剂作用下回流反应2 h,得2,4,6-三(4-醛基苯氧基)-1,3,5-三嗪(ZJT),收率98.8%;第二步在n(DOPO)∶n(ZJT)∶n(催化剂)=3.2∶1∶0.8,66℃回流反应3 h条件下得目标产物PN-FR,收率95.8%。用FTIR、EA、1HNMR、LC/MS、TG和DSC对中间体和产物作了结构表征和热性能分析。将该阻燃剂初步应用于环氧树脂绝缘层压板的阻燃,当阻燃剂质量分数为15%时,绝缘层压板氧指数达到36.2,通过UL-94 V-0级测试。该文研究工作的新颖性,已为四川省科学技术信息研究所2006年10月26日出具的第A0601512号《科技查新报告》所证实。
A novel phosphaphenanthrene flame retardant containing triazine structure PN-FR was synthesized through a two-step process With trichloro-1,3,5-triazine,4-hydroxybenzaldehyde and 9,10- dihydro-9-oxa-10-phosphaphenanthrene-10-oxide （ DOPO ）. The intermediate 2, 4, 6-tris （ 4- formylphenoxy） -1,3,5-triazine （ ZJT ） was prepared by refluxing trichioro-1,3,5-triazine and 4- hydroxybenzaldehyde in dichloromethane and water. The yield was 98.8%. Then the target product PN- FR was obtained by reacting the intermediate and with DOPO. Under the optimized reaction conditions： n （DOPO） ： n （ZJT） ： n （ catalyst ） = 3.2 ： 1 ： 0. 8, reaction time 3 h, temperature 66 ℃, the yield was 95.8%. Both the intermediate and target product were characterized by FTIR,EA,1HNMR,LC/MS, TG, DSC, etc. The flame retardant has been preliminarily applied in epoxy resin insulating laminate, the LOI was up to 36. 2 and V - 0 rating was observed from UL - 94 when the percentage of PN-FR in insulating laminate was 15%.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2009年第2期187-191,共5页
Fine Chemicals
基金
“十一五”国家科技支撑计划课题(2006BAE03B05-3)~~
