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生物质化学工程

生物质化学工程 ›› 2016, Vol. 50 ›› Issue (5): 29-33.doi: 10.3969/j.issn.1673-5854.2016.05.006

• 研究报告 • 上一篇    下一篇

基于单宁模型物的丙烯酸酯单体制备及性能研究

肖凤龙, 卫民, 赵剑, 蒋剑春, 侯敏   

  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
  • 收稿日期:2016-01-28 出版日期:2016-09-30 发布日期:2016-12-03
  • 通讯作者: 卫民(1961-),男,副研究员,硕士生导师,从事生物质利用和合成树脂等方面的研究;E-mail:nanjingwm@163.com。 E-mail:nanjingwm@163.com
  • 作者简介:肖凤龙(1989-),男,山东临沂人,硕士生,研究方向为吸附树脂材料;E-mail:long110511@163.com
  • 基金资助:
    “十二五”国家科技支撑计划资助（2014BAD02B02）

Sythesis and Characterization of Acrylate Monomer Derived from Tannins Model Compound

XIAO Feng-long, WEI Min, ZHAO Jian, JIANG Jian-chun, HOU Min   

  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
  • Received:2016-01-28 Online:2016-09-30 Published:2016-12-03

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摘要： 以没食子酸甲酯（MG）作为单宁模型物，利用丙烯酰氯（AC）对MG进行酯化反应改性，合成丙烯酸没食子酸甲酯（MG-AC）。考察了原料物质的量比和温度对产物得率的影响，并采用傅里叶变换红外光谱（FT-IR）、气相色谱-质谱联用仪（GC-MS）、元素分析、核磁共振碳谱（13C NMR）、凝胶色谱（GPC）对产物进行了分析。结果表明：合适的反应条件是35℃，n（AC）：n（MG）为1.1：1，该条件下产物得率为83.9%。FT-IR分析显示丙烯酸酯官能团成功接枝到没食子酸甲酯上；GC-MS分析产物的纯度为98.86%；元素分析结果显示碳、氢、氧的质量分数分别为55.46%、4.20%和40.33%，接近于MG-AC的理论值，说明产物是单取代丙烯酸没食子酸甲酯；13C NMR分析也表明产物为单取代；GPC分析结果显示，在引发剂作用下MG-AC可以发生溶液聚合，聚合物的重均相对分子质量（Mw）为13 637，数均相对分子质量（Mn）为11 820，Mw/Mn=1.15，表明MG-AC具有较好的聚合活性。

关键词: 丙烯酰氯, 没食子酸甲酯, 单宁模型物

Abstract: Methyl gallate acrylate (MG-AC) was prepared by reaction between methyl gallate (MG) (tannins model compound) and acryloyl chloride (AC).The effects of temperature and raw materials molar ratio on the yield of product were investigated.FT-IR,GC-MS,elemental analysis,13C NMR and GPC were used to characterize its structure and polymerization activity.And then,the optimum synthesis conditions were 35℃,molar ratio of AC and MG 1.1:1.Under these conditions,the yield of product was 83.9%.FT-IR results showed that the acrylate-functional-group was successfully grafted onto methyl gallate.GC-MS results showed that the purity of methyl gallate acrylate was 98.86%.Elemental analysis indicated that the mass fractions of carbon,hydrogen and oxygen were 55.46%,4.20% and 40.33%,respectively.They almost agreed to the theoretical value of MG-AC.Thus,the synthesized MG-AC was monosubsituted monomer.13C NMR results comfirmed the monosubsituted structure of monomer.GPC analysis results showed that the MG-AC could polymerize in the presence of the initiator,and the Mw,Mn and Mw/Mn of the polymer were 13 637,11 820 and 1.15.All the results showed that the methyl gallate acrylate was successfully synthesized and had good polymerization activity.

Key words: acryloyl chloride, methyl gallate, tannins model compound

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