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林产化学与工业 ›› 2019, Vol. 39 ›› Issue (4): 100-104.doi: 10.3969/j.issn.0253-2417.2019.04.014

• 研究报告 • 上一篇    下一篇

膦腈环核腰果酚环氧树脂的制备及表征

李俊杰1,2(),董云1,赵华平1,马红霞2   

  1. 1. 中国葛洲坝集团易普力股份有限公司, 重庆 401121
    2. 华中科技大学化学与化工学院, 湖北 武汉 430074
  • 收稿日期:2019-02-28 出版日期:2019-08-25 发布日期:2019-08-23
  • 作者简介:李俊杰(1990-),男,湖北武汉人,硕士生,主要从事含磷功能高分子材料研究; E-mail:lijunjie027@163.com

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

Junjie LI1,2(),Yun DONG1,Huaping ZHAO1,Hongxia MA2   

  1. 1. China Gezhouba Group Explosive Co. Ltd, Chongqing 401121, China
    2. School of Chemistry and Chemical Engineering, Huazhong University of Science and Technology, Wuhan 430074, China
  • Received:2019-02-28 Online:2019-08-25 Published:2019-08-23

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。

关键词: 腰果酚, 六氯环三磷腈, 腰果酚环氧树脂

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.

Key words: cardanol, hexachlorocyclotriphosphazene, cardanol-based epoxy resin

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