PhN-DOPO改性环氧树脂的制备及性能  

Preparation and properties of PhN-DOPO modified epoxy resin

作　　者：张晨 李笑甜 丁明惠 朱怀清 明丽君 刘欣雨 ZHANG Chen;LI Xiaotian;DING Minghui;ZHU Huaiqing;MING Lijun;LIU Xinyu(College of Materials Science and Chemical Engineering,Harbin Engineering University,Harbin 150001,Heilongjiang,China)

机构地区：[1]哈尔滨工程大学材料科学与化学工程学院,黑龙江哈尔滨150001

出　　处：《精细化工》2024年第11期2522-2530,共9页Fine Chemicals

摘　　要：以对氨基苯甲酸(PABA)、对羟基苯甲醛(PHBA)和9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物(DOPO)为原料合成了一种长链阻燃剂(PhN-DOPO),并经FTIR、^(1)HNMR、ESI-MS对其进行了表征。制备了PhN-DOPO添加量(以环氧树脂质量计,下同)为0、5%、10%、15%的一系列梯度改性环氧树脂(EP1~EP4),通过DSC、TGA、极限氧指数(LOI)、垂直燃烧(UL-94)和剥离强度测试考察了改性环氧树脂的热稳定性、阻燃性及粘接性能。结果表明,PhN-DOPO添加量为10%时,改性环氧树脂EP3的玻璃化转变温度提高至177.2℃,UL-94测试为V-0等级,LOI达32.4%,表现出最好的阻燃性和良好的热稳定性;EP3的剥离强度为2.75 kN/m,比纯环氧树脂(EP1)高0.28 kN/m。改性环氧树脂燃烧时,PhN-DOPO通过凝聚相和气相阻燃协同作用提高了环氧树脂的阻燃性,并且改性环氧树脂对应残炭的石墨化程度提高,表现出良好的成炭能力,其中改性环氧树脂EP3的成炭效果最好。A long chain flame retardant(PhN-DOPO)was synthesized from p-aminobenzoic acid(PABA),p-hydroxybenzaldehyde(PHBA)and 9,10-dihydro-9-oxa-10-phosphame-10-oxide(DOPO),and characterized by FTIR,^(1)HNMR and ESI-MS.A series of gradient modified epoxy resins(EP1~EP4)with 0,5%,10%and 15%addition of PhN-DOPO(based on the mass of epoxy resin,the same below)were then prepared,and evaluated via DSC,TGA,limit oxygen index(LOI),vertical combustion(UL-94)and peel strength tests for analyses on their thermal stability,flame retardancy and bond performance.The results showed that the modified epoxy resin EP3 prepared with 10%PhN-DOPO exhibited the best flame retardancy and good thermal stability,with the glass transition temperature increased to 177.2℃,the UL-94 test of V-0 grade,the LOI of 32.4%,and the peel strength of 2.75 kN/m,0.28 kN/m higher than pure epoxy resin(EP1).During the combustion process of the modified epoxy resin,PhN-DOPO improved the flame retardancy of the epoxy resin through the synergistic effect of condensed phase and gas phase flame retardancy.Meanwhile,the modified epoxy resin showed better carbon forming ability with higher graphitization degree,with EP3 displaying the best carbon forming effect.

关 键 词：阻燃剂 环氧树脂 热稳定性 阻燃性能 粘接性能 橡塑助剂 

分 类 号：TQ323.5[化学工程—合成树脂塑料工业]