茶皂素基膨胀型阻燃剂的制备及其在涂料中的应用

摘要

A novel polyphosphoester class trinity tea saponin based environmentally friendly intumescent flame retardant(TTS-IFR)was prepared by using the active natural product tea saponin containing multiple hydroxyl and carboxyl radicals as the raw material reacting with ammonium polyphosphate and pentaerythritol under specific conditions. Its structure characterization and thermal degradation properties were studied with FTIR spectrometer and simultaneous thermal analyzer. Tea saponin reacted with ammonium polyphosphate and pentaerythritol,and generated polyphosphoester class tea saponin-based trinity intumescent flame retardant with good thermal stability,small degradation heat release,large residual rate at high temperature,and final residual rate up to 30.77%. In addition,the tea saponin-based trinity intumescent flame retardant was used in flame retardant coatings,and the flame retardance and pyrolysis performance of flame retardant coatings was evaluated with oxygen index tester and cone calorimeter. Tea saponin based trinity intumescent flame retardant significantly improved the performance of flame-retardant coatings,and LOI value of the flame retardant coating was 34.2%,refractory time was 11.1 min. In cone calorimeter experiments,the flame retardant coatings sample had low mean heat release rate (m-HRR) for 36.18 kW/m2,total heat release (THR) for 5.25 kJ/m2 and mean effective heat of combustion (m-EHC) for only 5.11 kJ/kg,and the flame retardant performance was greatly improved compared with flame retardant coatings containing unreacted flame retardant. This flame retardant was free from halogen and consisted of three source to form an organic whole,so it had advantages of excellent flame retardance,good compatibility with polymer,high efficiency and environmental friendliness.%采用多羟基、多羧基的活性天然产物茶皂素为原料，与聚磷酸铵和季戊四醇在一定条件下反应，制备一种聚磷酸酯类茶皂素基三位一体新型环保膨胀型阻燃剂。采用傅里叶红外分析技术对阻燃剂进行了结构表征，采用综合热分析仪对阻燃剂的热降解性能进行了研究。结果表明，茶皂素与聚磷酸铵、季戊四醇发生反应，生成聚磷酸酯类茶皂素基膨胀型阻燃剂，且该阻燃剂具有良好的热稳定性，降解热释放较小，高温残留率高，最终的质量残留率高达30.77%。将制备阻燃剂用于阻燃涂料中，并采用氧指数测试仪和锥形量热仪研究了阻燃涂料的阻燃性能和热解性能。研究表明，茶皂素基三位一体膨胀型阻燃剂能显著提高涂料的阻燃性能，阻燃涂料的氧指数值高达34.2%，耐火时间为11.1 min，且锥形量热实验中，该阻燃涂料试样的平均热释放速率（m-HRR）为36.18 kW/m2，总热释放量（THR）为5.25 kJ/m2，平均有效燃烧热（m-EHC）为5.11 kJ/kg，与含复合型阻燃剂的阻燃涂料试样相比，阻燃性能得到极大提高。该制备阻燃剂不含卤素，集三源一体，具有阻燃性能优越，相容性能良好，高效环保等优点。