TGIC/DOPO/HFMA改性 水性环氧固化剂的制备与性能
Preparation of waterborne epoxy curing agents modificated by TGIC/DOPO/HFMA and its properties
投稿时间:2020-01-03  修订日期:2020-03-25
中文关键词: 固化剂  环氧树脂  合成  水性
英文关键词: curing agent  epoxy resin  synthesis  waterborne
周继亮 中南民族大学 
张俊珩 中南民族大学  
张道洪 中南民族大学  
李廷成 中南民族大学  
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      摘要:通过在水性环氧固化剂分子结构中引入含刚性三嗪环结构的异氰尿酸三缩水甘油酯(TGIC)、9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物(DOPO)以及甲基丙烯酸六氟丁酯(HFMA)等分子链段,来合成综合性能优良的水性环氧固化剂。研究探讨其合成工艺条件,采用FTIR、TGA、极限氧指数(LOI)、UL-94燃烧测试等手段对固化剂的结构、固化涂膜的机械性能、防腐性能、耐热性、残炭率及阻燃性能进行表征和考察。结果表明:先在摩尔比(n(TGIC)/n(DOPO))为1: 1~2,催化剂三苯基膦用量2%,反应温度145℃, 时间5小时下合成TGIC-nDOPO加成物;再70℃下,将其与自制的含氟碳链段(HFMA)、聚醚醇链段及环氧树脂(DGEBA)链段的多胺化合物(TETA-PEGGE-DGEBA-HFMA&HGE)加成反应6小时,可合成出TGIC/DOPO/HFMA改性水性环氧固化剂。所合成的固化剂具有良好的水分散性,应用时与环氧树脂组分相容性良好,固化涂膜透明均匀;涂膜铅笔硬度为2H~3H,抗冲击性50~55kg?cm,其防腐性能优于普通水性固化剂。固化涂膜在500℃-800℃下的耐热性和残炭率显著提高:如在600℃下,其残炭率相对于普通水性固化剂的5.5%可提高到20.6%。且具有良好阻燃性能:LOI值可达到36.3,并通过UL-94垂直燃烧测试,达到V0等级。
      In order to improve the comprehensive performance of waterborne epoxy resin coating,Triglycidyl Isocyanurate(TGIC) containing a rigid triazine ring, 9,10-Dihydro-9-oxa-10-phosphaphenanthren-10-oxide (DOPO) with effective flame retardant performance and Hexafluorobutyl Methacrylate(HFMA) with good anti-corrosion performance were used simultaneously as materials to synthesize the aqueous epoxy curing agents. The synthetic process conditions were studied and discussed, and the structure of the curing agent, the mechanical properties, the corrosion resistance, the heat resistance and the residual carbon rate of the cured films and the flame retardancy of the cured specimen were studied and characterized by means of FT-IR, thermogravimetric analysis(TGA), limit Oxygen index(LOI), UL-94 vertical combustion determination and so on. The results of the synthesis process conditions showed that TGIC-nDOPO adduct can be synthesized with the initial molar ratio between TGIC and DOPO of 1:1~2 under the condition of reaction temperature 145℃, reaction time 5 hours, the amount of catalyst triphenylphosphine 2%. And the TGIC/DOPO/HFMA modified water-based curing agent can be synthesized when TGIC-nDOPO addut reacted dropwise with the self-preparated TETA-PEGGE-DGEBA-HFMA&HGE polyamine compound containing fluorinated carbon chain, hydrophilic toughened polyether alcohol chain and epoxy resin (DGEBA) chain on the condition of reaction temperature 70℃, reaction time 6 hours. The synthesized curing agent has good water dispersion, good compatibility with epoxy resin components and can form transparent and uniform cured film. The cured film has good mechanical properties with pencil hardness of 2H~3H and impact resistance of 50~55kg?cm. The anti-corrosion properties of the synthesized waterborne curing agent were better than that of the ordinary waterborne curing agent. The heat resistance and residual carbon rate at high temperature (500℃~800℃) of the cured film was significantly improved, for example, at 600 ℃, the residual carbon rate can be increased to 20.6% relative to 5.5% of the normal water-based curing agent. The synthesized curing agent also has good flame retardancy because the LOI value of its cured specimen may achieve 36.3, and can pass the UL-94 vertical combustion test, up to V0 grade.
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