为了制备水溶且耐高温的环氧树脂,提升其贮存稳定性和使用安全性,减少环境污染,以环氧树脂E20和E44为原料,通过原位共混磷酸化合成工艺对混合环氧树脂进行改性,制备出耐高温的磷酸化改性水溶性环氧树脂,并对其合成条件进行了优化,确定了最佳工艺参数。通过傅里叶变换红外光谱仪、核磁共振波谱仪、热重分析仪等对磷酸化改性水溶性环氧树脂的结构和性能进行表征。磷酸化改性水溶性环氧树脂最佳工艺条件为:m(E20)∶m(E44)=5∶5,环氧树脂环氧值与磷酸摩尔比为1∶1.2,反应温度为50℃,反应时间为150min,m(H2O)∶m(H3PO4)=2.3∶1。制备的磷酸化改性水溶性环氧树脂粒径小,质量分数为1%的改性环氧树脂乳液平均粒径为11.8nm,以4000r/min转速分离30min稳定不分层;改性水溶性环氧树脂耐高温性能优良,初始分解温度为297.4℃,400℃时质量残留率为72.20%,600℃时质量残留率高达36.68%;临界胶束浓度为0.5%,表面张力为38.86mN/m,显示了良好的表面活性;改性水溶性环氧树脂乳液的黏温特性良好,黏度敏感性小。
In order to prepare water-soluble and high-temperature resistant epoxy resin,improve its storage stability and safety,and reduce environmental pollution,epoxy resin E20 and E44 were used as raw materials,and the mixed epoxy resin was modified by in-situ blending phosphorylation synthesis process to prepare the high-temperature resistant phosphorylation-modified water-soluble epoxy resin.Its synthesis process was optimized and the optimal process parameters were determined.The structure and properties of phosphorylated-modified water-soluble epoxy resin were characterized by Fourier transform infrared spectrometer,nuclear magnetic resonance spectrometer and thermogravimetric analyzer.The optimum process conditions were as follows:m(E20)∶m(E44)=5∶5,the molar ratio of epoxy value to phosphoric acid was 1∶1.2,the reaction temperature was 50℃,the reaction time was 150min,m(H2O)∶m(H3PO4)=2.3∶1.The prepared phosphorylated modified water-soluble epoxy resin had a small particle size,and the average particle size of the modified epoxy resin emulsion with a mass fraction of 1% was 11.8nm,and it was stable without delamination after centrifugation at a speed of 4000r/min for 30min.It had excellent high-temperature resistance,with an initial decomposition temperature of 297.4℃,a mass residue rate of 72.20% at 400℃,and a mass residue of up to 36.68% at 600℃.The critical micelle concentration of the modified resin was 0.5%,and the surface tension was 38.86mN/m,showing good surface activity.The viscosity-temperature characteristics of the modified water-soluble epoxy resin emulsion was good,and the viscosity sensitivity was small.
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基金资助
中国石油化工股份有限公司科技开发项目(421068-3)
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