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林产化学与工业 ›› 2012, Vol. 32 ›› Issue (6): 17-21.

• 1研究报告 • 上一篇    下一篇

微波辐射松香季戊四醇酯的合成研究

李建芳1, 商士斌1,2, 宋湛谦1, 王丹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:2012-05-30 修回日期:1900-01-01 出版日期:2013-12-30 发布日期:2013-12-30
  • 通讯作者: 商士斌(1964-),研究员,博士生导师,从事生物质材料与化学品研究开发;E-mail:shangsb@163.com。

Synthesis of Rosin Pentaerythritol Ester under Microwave Heating Conditions

LI Jian-fang1, SHANG Shi-bin1,2, SONG Zhan-qian1, WANG Dan1,2   

  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. Institute of New Technology of Forestry,CAF, Beijing 100091, China
  • Received:2012-05-30 Revised:1900-01-01 Online:2013-12-30 Published:2013-12-30

摘要: 在密闭条件下,利用微波辐射快速有效地合成了松香季戊四醇酯。常规酯化反应需要270min,在微波密闭条件下,不仅反应时间大幅度地缩短至40min,而且所得产品的质量也有提高。为了研究各反应因素对产品酸值和软化点的影响,设计了正交试验L9(34),并得出了微波密闭条件下合成松香季戊四醇酯的最佳反应条件:催化剂BEP用量0.30%、季戊四醇用量16%、反应时间40min、微波功率200W。该条件下合成的松香季戊四醇酯加纳色号为4、酸值12.7mg/g、软化点102℃。

关键词: 松香, 季戊四醇, 合成, 微波

Abstract: An efficient and rapid method of synthesizing rosin pentaerythritol ester is described under microwave conditions in a closed system. Conventional heating process of rosin esterification needs 270 min. This unprecedented synthesis improves the performance of the products significantly and reduces reaction time to 40 min. Furthermore, an orthogonal test of L9(34) was also designed in order to study factors which affected the color and acid value of the products. The optimized synthesis conditions are as follows: the dosage of BEP, 0.30%; the dosage of pentaerythritol, 16%; heating time, 40 min; microwave power, 200W. The rosin pentaerythritol ester with light color (Gardner 4), low acid value (12.7 mg/g), and high softening point (102℃) was obtained under optimized conditions.

Key words: rosin, pentaerythritol, synthesis, microwave

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