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bce ›› 2016, Vol. 50 ›› Issue (4): 13-20.doi: 10.3969/j.issn.1673-5854.2016.04.003

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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

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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