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膦腈环核腰果酚环氧树脂的制备及表征

Synthesis and Characterization of Cardanol-based Epoxy Resin Containing A Cyclotriphosphazene Core

  • 摘要: 以腰果酚、六氯环三磷腈(HCCP)为原料,利用NaH作为缚酸剂制备了膦腈环核六取代腰果酚(HCPP),并采用H2O2/HCOOH体系对HCPP进行环氧化反应得到膦腈环核腰果酚环氧树脂(EHCPP),实验优化了EHCPP的合成条件,并采用FT-IR和1H NMR对中间产物HCPP和最终产物EHCPP进行了分析和表征。实验结果表明:EHCPP较佳合成条件为以腰果酚的双键为基准,n(双键):n(甲酸)=1.0:1.0,n(双键):n(H2O2)=1.0:1.8,催化剂TsOH添加量为1%(以HCPP质量为基准),反应温度65℃,反应时间6 h;此条件下得到的产物EHCPP环氧值为4.1 mmol/g。FT-IR和1H NMR分析结果表明:实验得到的HCPP和EHCPP的结构与预期结构基本相符。

     

    Abstract: A novel six armed cardanol-derived epoxy resin containing a cyclotri phosphazene core(EHCPP) was successfully synthesized by two steps. Firstly, cardanol reacted with hexachlorocyclotriphosphazene(HCCP) to produce hexasubstituted cardanol with cyclotriphosphazene core(HCPP) with NaH as acid binding agent; secondly, EHCPP was generated by epoxidation of HCPP with the H2O2/HCOOH system, the synthesis conditions of EHCPP were optimized by orthogonal experiment, and the intermediate product HCPP and the final product EHCPP were analyzed and characterized by FT-IR and 1H NMR. The results showed that the optimum synthesis conditions of EHCPP were as follows n(double bond of cardanol):n(formic acid)=1.0:1.0, n(double bond of cadanol):n(H2O2)=1.0:1.8, catalyst TsOH 1% relative to the mass of HCPP, the reaction temperature 65℃, the reaction time 6 h, and the results of FT-IR and 1H NMR analysis showed that the structures of HCPP and EHCPP were basically consistent with the expected structures and its epoxy value was 4.1 mmol/g.

     

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