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林产化学与工业 ›› 2015, Vol. 35 ›› Issue (6): 63-68.doi: 10.3969/j.issn.0253-2417.2015.06.011

• 研究报告 • 上一篇    下一篇

二元端乙烯基型松香衍生物的微波辅助制备及表征

卢言菊1,2, 王迷霞1, 古研1, 陈玉湘1,2, 毕良武1,2, 赵振东1,2   

  1. 1. 中国林业科学研究院 林业新技术研究所, 北京 100091;
    2. 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:2014-07-21 出版日期:2015-12-25 发布日期:2015-12-28
  • 通讯作者: 赵振东,研究员,博士生导师,研究领域为萜类化学、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,博士生,主要从事萜类化学加工与利用;E-mail:luyanju-1982@163.com
  • 基金资助:
    中国林科院林业新技术所基本科研业务费专项资金(CAFINT2013C01);国家自然科学基金资助项目(31370575)

Synthesis and Characterization of Di-vinyl-terminated Rosin Derivatives under Microwave Irradiation

LU Yan-ju1,2, WANG Mi-xia1, GU Yan1, CHEN Yu-xiang1,2, BI Liang-wu1,2, ZHAO Zhen-dong1,2   

  1. 1. Research Institute of Forestry New Technology, CAF, Beijing 100091, China;
    2. 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:2014-07-21 Online:2015-12-25 Published:2015-12-28

摘要: 以丙烯酸改性松香酸钠和氯丙烯为原料,十六烷基三甲基溴化铵为催化剂,对苯二酚为阻聚剂(用量为丙烯酸改性松香钠质量的0.2%),N,N-二甲基甲酰胺为溶剂(用量为丙烯酸改性松香钠质量的3倍),在微波辅助条件下,探讨了工艺条件对二元端乙烯基型松香衍生物丙烯酸改性松香烯丙酯得率的影响,确定了最佳工艺条件为:微波功率400 W,反应时间100 min,催化剂用量4%,物料配比n(氯丙烯):n(丙烯酸改性松香钠)2:1,反应温度50 ℃,在此条件下产物得率高达92.2%。采用GC、GC-MS和FT-IR等技术表征了反应产物的结构,结果表明合成产物结构与目标产物结构一致。

关键词: 微波辅助, 松香衍生物, 丙烯酸海松酸烯丙酯

Abstract: Allyl acrylate-modified rosinate was synthesized by using sodium acrylic modified rosinate(SAMR) and allyl chloride as raw materials, cetyl trimethyl ammonium bromide as catalyst, hydroquinone as polymerization inhibitor(0.2% of the mass of SAMR) and N, N-dimetylformamide as solvent(treble the mass of SAMR) under microwave irradiation.The influence of different reaction conditions on the yield of product was investigated.The optimum reaction conditions were microwave energy 400 W, reaction time 100 min, catalyst amount 4%, molar ratio of allyl chloride and sodium acrylic modified rosinate 1:1, reaction temperature 50 ℃, and the yield was 92.2% under these conditions.The structure of the product was characterized by GC, GC-MS and FT-IR.The results showed that the structure of the synthesized product and the target product was consistent.

Key words: microwave irradiation, rosin derivative, allyl acrylpimarate

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