周继亮,张俊珩,张道洪,李廷成.TGIC/DOPO/HFMA改性水性环氧固化剂的制备与性能[J].中南民族大学学报自然科学版,2020,39(5):450-457
TGIC/DOPO/HFMA改性水性环氧固化剂的制备与性能
Preparation of TGIC/DOPO/HFMA modified waterborne epoxy curing agents and their properties
  
DOI:10.12130/znmdzk.20200502
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
基金项目:湖北省自然科学基金资助项目(2015CFC875);中央高校基本科研业务费专项资金资助项目(CZY19008)
作者单位
周继亮 中南民族大学 化学与材料科学学院湖北省能源高分子材料工程技术研究中心武汉 430074 
张俊珩 中南民族大学 化学与材料科学学院湖北省能源高分子材料工程技术研究中心武汉 430074 
张道洪 中南民族大学 化学与材料科学学院湖北省能源高分子材料工程技术研究中心武汉 430074 
李廷成 中南民族大学 化学与材料科学学院湖北省能源高分子材料工程技术研究中心武汉 430074 
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中文摘要:
      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)、具有有效阻燃性能的9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物(DOPO)以及具有良好的防腐性能的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.探讨了其合成工艺条件,采用FTIR、TGA、极限氧指数(LOI)、UL-94垂直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、残炭率及固化试样的阻燃性能进行了研究.结果表明:先在TGIC/DOPO摩尔比为1︰1~2︰1,催化剂三苯基膦用量2%,反应温度145 ℃, 时间5 h下合成了TGIC-nDOPO加成物;再在70 ℃下,将其逐滴地与自制的含氟碳链段(HFMA)、亲水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 h,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;涂膜机械性能良好,铅笔硬度为2H~3H,抗冲击性50~55 kg?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%;它还具有良好阻燃性能:LOI值可达到36.3,并通过UL-94垂直燃烧测试,达到V0等级.
英文摘要:
      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 to synthesize the aqueous epoxy curing agents. The synthesis conditions were investigated, 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 by means of FT-IR, thermogravimetric analysis(TGA), limit oxygen index(LOI), UL-94 vertical combustion test and so on. The results showed that TGIC-nDOPO adduct could be synthesized with the initial molar ratio of TGIC and DOPO between 1:1~2:1 under the condition of reaction temperature 145 ℃, reaction time 5 hours, and the amount of catalyst triphenylphosphine 2%. The TGIC/DOPO/HFMA modified curing agent could then be synthesized by adding TGIC-nDOPO dropwise to the self-prepared TETA-PEGGE-DGEBA-HFMA&HGE polyamine compound containing fluorinated carbon chain, hydrophilic toughened polyether alcohol chain and epoxy resin (DGEBA) chain and reacted at 70 ℃ for 6 hours. The synthesized curing agent has good water dispersion property, good compatibility with epoxy resin and can form transparent and uniform cured film. The film has good mechanical properties, with a pencil hardness of 2H~3H and an impact resistance of 50~55 kg?cm. The anti-corrosion properties were better than that of the ordinary waterborne curing agent. The heat resistance and carbon residue rate at high temperature (500?800 ℃) of the cured film was significantly improved, for example, at 600 ℃, the carbon residue rate can be increased to 20.6% relative to 5.5% of the normal water-based curing agent. The synthesized curing agent also demonstrated excellent flame retardancy: the LOI value of the cured specimen reached 36.3, and passed the UL-94 vertical combustion V0 test.
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