摘要
为开发含有P、N、Si等多种元素的复合阻燃剂,以六氯三聚磷腈(HCCP)、对羟基苯甲醛、对氨基苯甲酸、9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物(DOPO)和三苯基硅醇为原料,合成了一种含硅磷腈的复合阻燃剂(SCP-DOPO)。采用FTIR、^(1)HNMR和^(31)PNMR对其结构进行了表征,通过DSC、TGA、极限氧指数(LOI)、垂直燃烧(UL-94)、剥离强度测试,考察了SCP-DOPO添加量(质量分数,下同)对环氧树脂(EP)热稳定性、阻燃性能及黏结性能的影响。结果表明,当SCP-DOPO添加量为8%时,制备的改性EP(EP3)残炭的石墨化程度最高,成炭能力最强;Raman测试结果显示,其D峰和G峰分峰的拟合峰面积(A)比值(A_(D)/A_(G)值)最低,为3.28;当SCP-DOPO添加量为4%和8%时,制备的改性EP(EP2和EP3)剥离强度分别为3.06和2.64 kN/m,优于纯EP;当SCP-DOPO添加量为8%和12%时,制备的改性EP(EP3和EP4)UL-94测试均为V-0级,LOI分别达到31.1%和31.6%。SCP-DOPO优异的阻燃性能归因于气相阻燃和凝聚相阻燃的协同作用。
In order to develop compound flame retardant containing P,N,Si and other elements,a compound flame retardant containing silicophosphoronitrile(SCP-DOPO)was synthesized from hexachloro-trihydroxybenzaldehyde,p-aminobenzoic acid,9,10-dihydro-9-oxa-10-phosphophenanthrene 10-oxide(DOPO)and triphenylsilanol,and characterized by FTIR,^(1)HNMR and ^(31)PNMR.The effect of SCP-DOPO addition amount(mass fraction,the same below)on the thermal stability,flame retardant properties and bonding properties of epoxy resin(EP)was evaluated by DSC,TGA,limiting oxygen index(LOI),vertical combustion(UL-94)and peel strength tests.The results showed that the residual carbon of EP(EP3)modified with SCP-DOPO addition amount of 8%exhibited the highest graphitization degree and the strongest carbonization ability,while data from Raman tests indicated that the fitting peak area(A)ratio(A_(D)/A_(G) value)of the D-peak and G-peak sub-peaks was the lowest of 3.28.The peel strength of modified EP(EP2and EP3)prepared with SCP-DOPO addition amount of 4%and 8%was 3.06 and 2.64 kN/m,respectively,better than that of pure EP.The EP(EP3 and EP4)modified with SCP-DOPO addition amount of 8%and 12%were V-0 grade in UL-94 tests,with LOI of 31.1%and 31.6%,respectively.The excellent flame retardancy of SCP-DOPO was attributed to the synergistic effect of vapor phase flame retardancy and condensed phase flame retardancy.
作者
明丽君
张晨
丁明惠
刘欣雨
高泽宇
李墨焱
MING Lijun;ZHANG Chen;DING Minghui;LIU Xinyu;GAO Zeyu;LI Moyan(Key Laboratory of Superlight Materials and Surface Technology,Ministry of Education,Institute of Surface Interface Science and Technology,College of Materials Science and Chemical Engineering,Harbin Engineering University,Harbin 150001,Heilongjiang,China)
出处
《精细化工》
北大核心
2025年第9期2060-2070,共11页
Fine Chemicals
关键词
阻燃剂
环氧树脂
阻燃性能
热稳定性
黏结性能
橡塑助剂
flame retardants
epoxy resins
flame retardancy
thermal stabilities
bond performances
rubber and plastics auxiliaries
