光谱学与光谱分析, 2013, 33 (10): 2655, 网络出版: 2013-10-23  

新型腰果酚基不饱和树脂的结构及其紫外光固化行为的红外光谱研究

Research on Structure and UV Curing Behaviors of Novel Cardanol-Based Unsaturated Resins Using FTIR Spectrum Analysis Method
李守海 1,2,3,*杨雪娟 1,2李梅 1,2黄坤 1,2,3夏建陵 1,2,3
作者单位
1 中国林业科学研究院林产化学工业研究所
2 江苏省生物质能源与材料重点实验室, 国家林业局林产化学工程重点开放性实验室, 生物质化学利用国家工程实验室, 江苏 南京210042
3 中国林业科学研究院林业新技术研究所, 北京100091
摘要
以天然产物腰果酚为原料, 利用其酚羟基与环氧基的反应活性, 通过开环醚化反应制备了两种腰果酚基不饱和树脂单体。 通过傅里叶红外光谱研究了合成过程中主要活性基团的变化, 结合核磁共振氢谱及凝胶渗透色谱分析进一步确定了合成树脂单体的分子结构, 并利用红外光谱法对树脂单体的紫外光固化行为进行了研究, 且对其光固化物进行了热重分析。 研究表明: 分子结构分析确认了目标产物的成功合成, 树脂单体的分子结构以及不饱和双键含量对树脂的固化速度和固化物的热稳定性有着重要影响, 两种单体在30 s内均已基本达到最高固化水平, 光固化物的主分解初始温度均可达到350 ℃以上。
Abstract
Two dissimilar cardanol-based unsaturated resin monomers were prepared via simple ring-opening and etherification reaction by utilizing the reactivity between phenolic hydroxyl and epoxy group with the aid of cardanol as raw material. The transformations of different groups were characterized using Fourier transform infrared (FTIR) during the synthesis process, the resin monomers’ structure was further analyzed using the 1H-nuclear magnetic resonance (1H-NMR) and gel permeation chromatography (GPC), and the UV curing behaviors of resin monomers were studied by means of FTIR method. In addition, the thermal stability of UV cured resin monomers were also tested by thermogravimetric analysis(TGA). The molecular structure analysis demonstrated that these two target products were successfully synthesized. UV curing behaviors analysis showed that the prepared cardanol-based unsaturated resin monomers could reach ultimate curing level within 30 s. TGA results showed that the molecular structure and the content of double bond had critical influence on their thermal stability. The main initial thermal decomposition temperature of these two cured resin monomers was all above 350 ℃.

李守海, 杨雪娟, 李梅, 黄坤, 夏建陵. 新型腰果酚基不饱和树脂的结构及其紫外光固化行为的红外光谱研究[J]. 光谱学与光谱分析, 2013, 33(10): 2655. LI Shou-hai, YANG Xue-juan, LI Mei, HUANG Kun, XIA Jian-ling. Research on Structure and UV Curing Behaviors of Novel Cardanol-Based Unsaturated Resins Using FTIR Spectrum Analysis Method[J]. Spectroscopy and Spectral Analysis, 2013, 33(10): 2655.

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