波谱学杂志

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利用时域核磁共振研究脲醛树脂的固化过程

邵朱伟,张明辉,李新宇*   

  1. 内蒙古农业大学材料科学与艺术设计学院,内蒙古 呼和浩特 010018
  • 收稿日期:2013-10-16 修回日期:2014-07-17 出版日期:2014-09-05 发布日期:2014-09-05
  • 作者简介:邵朱伟(1989-),男,辽宁铁岭人,硕士研究生,材料加工工程专业,E-mail: 570168719@qq.com. *通讯联系人:张明辉,电话:15849376426,E-mail: zhangmh_email@aliyun.com.
  • 基金资助:

    国家自然科学基金资助项目(30800866,31160141).

Curing Process of Urea-Formaldehyde Resin Studied by Time-Domain Nuclear Magnetic Resonance

SHAO Zhu-wei,ZHANG Ming-hui,LI Xin-yu*   

  1. College of Material Science and Art Design, Inner Mongolia Agricultural University, Huhhot 010018, China
  • Received:2013-10-16 Revised:2014-07-17 Online:2014-09-05 Published:2014-09-05
  • About author:*Corresponding author:ZHANG Ming-hui, Tel: 15849376426,E-mail: zhangmh_email@aliyun.com.
  • Supported by:

    国家自然科学基金资助项目(30800866,31160141).

摘要:

利用时域核磁共振(TD NMR)技术对无固化剂的脲醛树脂在不同温度下固化过程进行了研究,实验结果表明:脲醛树脂在120 ℃左右时开始固化,在180 ℃左右时固化反应基本结束.随着温度的升高,自旋-自旋弛豫时间(T2)的总峰面积逐渐减少,当温度高于140 ℃时,总峰面积减少的程度较大.在30 ℃~140 ℃温度范围内,自旋-晶格弛豫时间T1(1) = 0.014 ms 时,随着温度的升高,峰面积先逐渐减少而后略微增加;T1(2) = 327.455 ms 时,随着温度的升高,峰面积逐渐减少.在30 ℃~180℃温度范围内,自旋-晶格弛豫时间(T1)分布的总峰面积随着温度的升高而逐渐减少.在固化过程中,随着温度的升高,脲醛树脂体系的质量逐渐减少,说明脲醛树脂胶黏剂体系发生了缩聚交联反应,同时生成了甲醛和水.

关键词: 时域核磁共振(TD NMR), 固化, 自旋-自旋弛豫时间(T2), 自旋-晶格弛豫时间(T1), 脲醛树脂

Abstract:

The curing process urea-formaldehyde resin without the use of hardeners was studied by time-domain nuclear magnetic resonance (TD NMR) at different temperatures. The results showed that urea-formaldehyde resin started curing at about 120 ℃ and ended around 180 ℃. The total peak area for T2 decrease gradually with increasing temperature; and larger changes were observed when the temperature was above 140 ℃. At temperature range between 30 ℃ to 140 ℃, the peak areas decreased gradually and then increased slightly with increasing temperature at T1 (1) = 0.014 ms; the peak areas decreased gradually with increasing temperature at T1 (2) = 327.455 ms. The total peak area for T1 decrease gradually with increasing temperature between 30 ℃ and 180 ℃. The urea-formaldehyde resin system weight decreased gradually with increasing temperature in the solidification process, confirming that cross-linking condensation reaction may occur, giving off formaldehyde and water.

Key words: time-domain nuclear magnetic resonance, solidification, spin-spin relaxation time, spin-lattice relaxation time, urea-formaldehyde resin

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