新型含氮阻燃剂／PEPA协同阻燃PP的性能  

Performance of Polypropylene Treated with PEPA and a Novel Nitrogen Containing Flame Retardant

作　　者：黄高能 刘盛华[1] 路风辉[2] 尹标林[1] Huang Gaoneng;Liu Shenghua;Lu Fenghui;Yin Biaolin(Key Laboratory of Green Chemical Technology of Guangdong Province,South China University of Technology,Guangzhou 510640,China;Shunde Polytechnic,Shunde 528300,China)

机构地区：[1]华南理工大学,广东省绿色化学产品技术重点实验室,广州510640 [2]顺德职业技术学院,广东顺德528300

出　　处：《工程塑料应用》2017年第2期6-11,共6页Engineering Plastics Application

基　　金：国家自然科学基金项目(21272078,21572068);国家重点研发计划项目(2016YFA0602900)

摘　　要：以三聚氯氰、对羟基苯甲酸甲酯、水合肼为原料经两步反应合成了一种新型含氮阻燃剂4,4′,4″–(1,3,5–三嗪–2,4,6–三取代)三氧三苯甲酰肼(TNTN),并通过核磁共振等对其进行表征。将合成的含氮阻燃剂TNTN与1–氧–4–羟甲基–2,6,7–三氧杂–1–磷杂双环[2.2.2]辛烷(PEPA)以不同配比制备膨胀型阻燃聚丙烯(PP)材料(IFR–PP)。通过极限氧指数(LOI)、垂直燃烧(UL–94)、热重(TG)分析、锥形量热(CCT)法以及扫描电子显微镜(SEM)对阻燃PP燃烧及热稳定性能进行表征。结果表明,IFR–PP同时具有良好的阻燃性及抗熔滴能力,当PEPA∶TNTN=2∶1时,UL–94达到V–0级,LOI值达到了33.7%,表现出良好的阻燃性能。TG测试表明:阻燃剂的加入使IFR–PP材料提前降解,同时提高了材料的成炭性能,当PEPA∶TNTN=5∶1时,600℃时IFR–PP材料的残炭量由空白样的0.07%提高到了20.6%。CCT测试表明:相对于纯PP,经阻燃剂改性后的PP热释放率和总热释放量均显著减少。SEM测试表明:不同配比阻燃剂的加入使PP在燃烧过程中形成膨胀、致密的炭层,很好地保护了下层材料,提高了PP材料的阻燃性能。A novel nitrogen containing flame retardant,4,4',4''–(1,3,5–triazine–2,4,6-triyl)tris(oxy) tribenzohydrazide (TNTN) was synthesized from cyanuric chloride,methyl–4–hydroxybenzoate,hydrazine hydrate. The structure of TNTN was characterized by 1H NMR,13C NMR spectrum analysis. The synthesized compound and 2,6,7-trioxa-1-phosphabicyclo-[2.2.2]octane-4-methanol-1-oxide(PEPA) was incorporated into polypropylene (PP) with different ratio to prepare intumescent flame retardant polypropylene thermosets (IFR–PP).The combustion and thermal properties of PP thermosets were investigated by limiting oxygen index (LOI),vertical burning (UL–94),thermogravimetric (TG) analysis,cone calorimetry (CCT) and scanning electronmicroscopy (SEM) tests. The results demonstrate that IFR–PP has both excellent flame retardancy and anti-dripping ability. Whenthe ratio of PEPA and TNTN is 2∶1,PP thermosets pass UL–94 V–0 flammability rating and its LOI value reach 33.7%,whichshows a good flame retardant performance. TG test results reveal that the incorporation of IFR–PP into PP stimulate the degradationof thermosets ahead of time and charring formation,when the ratio of PEPA and TNTN is 5∶1,char yield of thermosets increasefrom 0.07% to 20.6% at 600℃ . CCT parameter show that heat release rate and total heat release is also obviously reduced comparedto pure PP. The incorporation of TNTN and PEPA promote PP thermosets forming more homogeneous and compact char layer during combustion by SEM tests,which prevente the underlying matrix from further decomposition and combustion,consequ entlyenhancing the flame retardancy of PP thermosets.

关 键 词：含氮阻燃剂 聚丙烯 膨胀型阻燃 热性能 阻燃性能 

分 类 号：TQ325.14[化学工程—合成树脂塑料工业]