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生物质化学工程 ›› 2016, Vol. 50 ›› Issue (4): 13-20.doi: 10.3969/j.issn.1673-5854.2016.04.003

• 研究报告 • 上一篇    下一篇

γ位加成丙烯海松酸的制备及表征

卢言菊1,2, 张海波1, 赵振东1,2, 王迷霞1, 王婧1,2, 陈玉湘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:2015-11-04 出版日期:2016-07-31 发布日期:2016-10-08
  • 通讯作者: 赵振东,研究员,博士生导师,主要从事萜类化学、松树病虫害化学、天然产物化学、应用化学等方面的研究与利用;E-mail:zdzhao@189.cn。 E-mail:zdzhao@189.cn
  • 作者简介:卢言菊(1982-),女,山东临沂人,助理研究员,博士,主要从事萜类化学加工与利用;E-mail:luyanju-1982@163.com
  • 基金资助:
    国家自然科学基金资助项目(31370575);中国林科院林业新技术所基本科研业务费专项资金(CAFINT2013C01)

Synthesis and Characterization of γ-Acrylpimaric Acid

LU Yan-ju1,2, ZHANG Hai-bo1, ZHAO Zhen-dong1,2, WANG Mi-xia1, WANG Jing1,2, CHEN Yu-xiang1,2   

  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:2015-11-04 Online:2016-07-31 Published:2016-10-08

摘要: 在微波辅助条件下以树脂酸和丙烯酸为原料,经Diels-Alder加成反应制备得到丙烯酸改性松香。以气相色谱(GC)跟踪不同反应条件下丙烯酸改性松香主要成分丙烯海松酸(APA)的GC含量,得出APA的GC含量最高的条件为:10g树脂酸,反应温度230℃,微波功率400W,反应时间90min,n(丙烯酸):n(树脂酸)2:1,在此条件下,APA的GC含量为78.4%,枞酸型树脂酸转化为APA的转化率达98.6%。将丙烯酸改性松香通过控制pH值和过柱子进行提纯,制备得到GC纯度为95.7%的γ位加成丙烯海松酸,并对产物结构进行GC、GC-MS、FT-IR、1H NMR和13C NMR的表征,采用二维核磁解析确证了产物结构的正确性;DSC结果表明产物具有玻璃化转变温度,为79.78℃;TG分析表明产物的热失重温度为335.9℃,具有较好的耐热性。

关键词: 丙烯海松酸, 微波辅助, Diels-Alder反应, GC含量

Abstract: Acrylic-modified rosin was synthesized by Diels-Alder reaction using resin acid and acrylic acid as raw materials.The gas chromatography(GC) was employed in analyzing the content of acrylpimaric acid which was the main constituent of acrylic-modified rosin.And the optimum reaction conditions were resin acid 10g, reaction temperature 230℃, microwave energy 400W, reaction time 90min, and n(acrylpimaric acid):n (resin acid) 2:1.Under the optimum conditions, the GC content of acrylpimaric acid was 78.4%, and the conversion rate of abietic-type acid was up to 98.6%. γ-Acrylpimaric acid was isolated by controling pH value and silica gel column, and the GC content of the purified product was 95.7%.The structure of the γ-acrylpimaric acid was characterized by GC, GC-MS, FT-IR, 1H NMR, and 13C NMR.The glass transition temperature and the thermal decomposition temperature of γ-acrylpimaric acid were 79.78℃ and 335.9℃ by DSC and TG analysis, respectively.

Key words: acrylpimaric acid, microwave irradiation, Diels-Alder reaction, GC content

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