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林产化学与工业

林产化学与工业 ›› 2016, Vol. 36 ›› Issue (5): 61-67.doi: 10.3969/j.issn.0253-2417.2016.05.009

• 研究报告 • 上一篇    下一篇

腰果酚二醚曼尼希碱固化剂的合成及其相分离现象研究

宋健1, 李梅1,2, 李守海1,2, 黄坤1, 夏建陵1,2   

  1. 1. 中国林业科学研究院 林产化学工业研究所;生物质化学利用国家工程实验室;国家林业局 林产化学工程重点开放性实验室;江苏省 生物质能源与材料重点实验室, 江苏 南京 210042;
    2. 中国林业科学研究院 林业新技术研究所, 北京 100091
  • 收稿日期:2016-07-05 出版日期:2016-10-25 发布日期:2016-11-05
  • 通讯作者: 黄坤(1982-),男,副研究员,博士,主要从事天然资源化学利用的研究;E-mail:maotsedong@163.com。 E-mail:maotsedong@163.com
  • 作者简介:宋健(1989-),男,安徽安庆人,硕士生,主要从事生物基高分子材料的研究;E-mail:songjian8979@126.com
  • 基金资助:
    “十二五”国家科技支撑计划资助（2014BAD17B00）；中国林科院林业新技术所基本科研业务费专项资金（CAFINT2015C04）；江苏省生物质能源与材料重点实验室开放基金（JSBEM-S-201508）

Synthesis and Phase Separation Phenomena of Cardanol Diethers-Mannich Base Curing Agent

SONG Jian1, LI Mei1,2, LI Shou-hai1,2, HUANG Kun1, XIA Jian-ling1,2   

  1. 1. Institute of Chemical Industry of Forest Products, CAF;National Engineering Lab. for Biomass Chemical Utilization;Key and Open Lab. of Forest Chemical Engineering, SFA;Key Lab. of Biomass Energy and Material, Jiangsu Province, Nanjing 210042, China;
    2. Research Institute of Forestry New Technology, CAF, Beijing 100091, China
  • Received:2016-07-05 Online:2016-10-25 Published:2016-11-05

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摘要： 腰果酚（CD）和1，3-二溴丙烷经Williamson醚化反应得到一种腰果酚二醚化合物（CDE），然后以CDE、多聚甲醛和二乙烯三胺为原料，经Mannich反应制备得到一种浅色的腰果酚二醚曼尼希碱固化剂（MBCDE）。通过傅里叶红外光谱（FT-IR）和核磁共振氢谱（1H NMR）表征了产物的化学结构，并与氨乙基哌嗪（AEP）进行对比研究其相关性能。通过热重分析（TGA）、扫描电镜（SEM）和力学性能测试研究了两种固化剂与双酚A环氧树脂（DGEBA）固化材料的相关性能。结果表明：MBCDE/DGEBA的最大分解温度为351.6℃，具有良好的热稳定性。AEP/DGEBA环氧固化物的冲击强度为3.641 J/m，而添加80%的MBCDE后固化物的冲击强度则为5.155 J/m，提高了41.6%。SEM分析结果表明MBCDE固化材料中存在相分离。

关键词: 腰果酚, 相分离, 固化剂, 环氧树脂, 酚醛胺, Mannich反应

Abstract: The cardanol diethers (CDE) was obtained from Williamson etherification of cardanol(CD) and 1,3-dibromopropane. Then the cardanol diethers-Mannich baseas curing agent (MBCDE) for epoxy resins was prepared from the Mannich reaction of CDE, paraformadehyde and diethylenetriamine. The chemical structure was confirmed by FT-IR and 1H NMR. N-Aminoethylpiperazine (AEP) was chose as a control to investigate the toughening properties of MBCDE. Thermogravimetric analysis (TGA), scanning electronic microscopy (SEM) and mechanical properties of the cured epoxies were also conducted to investigate the properties of the bisphenol A epoxy resin (DGEBA) cured by two curing agents. The TGA results showed that the maximum decomposition temperature of MBCDE was 351.6℃ and the sample had good thermal stability. The impact strength of cured AEP/DGEBA was 3.641 J/m, while the cured 80% MBCDE sample had an impact strength of 5.155 J/m, which was improved by 41.6%. SEM results indicated that there was phase seperation in the cured materials contained MBCDE.

Key words: cardanol, phase separation, curing agent, epoxy resin, phenol-aldehyde amine, Mannich reaction

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