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林产化学与工业 ›› 2015, Vol. 35 ›› Issue (1): 51-56.doi: 10.3969/j.issn.0253-2417.2015.01.008

• 研究报告 • 上一篇    下一篇

超临界正己烷中松香酸一元醇酯高压氢解还原反应

尹斌, 曾韬, 王雪源   

  1. 南京林业大学 化学工程学院, 江苏省生物质绿色燃料与化学品重点实验室, 江苏 南京 210037
  • 收稿日期:2013-12-05 出版日期:2015-02-25 发布日期:2015-03-05
  • 通讯作者: 曾韬,教授,博士生导师,从事林产化工教学和科研工作;E-mail:zengtao@njfu.edu.cn。 E-mail:zengtao@njfu.edu.cn
  • 作者简介:尹斌(1989-),男,江西萍乡人,硕士生,研究方向为林产化工;E-mail:njfuyb@126.com
  • 基金资助:
    国家自然科学基金资助项目(30771686);江苏省高校优势学科建设工程项目资助(无编号)

Reduction of Monobasic Alcohol Abietate in Supercritical Hexane

YIN Bin, ZENG Tao, WANG Xue-yuan   

  1. College of Chemical Engineering, Nanjing Forestry University, Jiangsu Key Lab of Biomass-based Green Fuels and Chemicals, Nanjing 210037, China
  • Received:2013-12-05 Online:2015-02-25 Published:2015-03-05

摘要: 在超临界正己烷条件下,采用Cu-Zn催化剂进行了系列松香酸一元醇酯的氢解还原反应。考察了反应条件对反应结果的影响。结果表明:适宜的工艺条件为松香酯15 g,Cu-Zn催化剂用量为松香酯质量的10%,m(松香酯):m(正己烷)为1:3,温度为270 ℃,压力10 MPa,反应时间11 h;该条件下松香甲酯、松香丁酯和松香辛酯的转化率分别为87.9%,75.0%和69.9%,选择性分别为93.4%,92.4%和92.8%,得率分别为82.1%,69.3%和64.9%;FT-IR和GC-MS分析结果表明,松香酯经氢解还原反应后酯基被还原为羟基,还原产物主要成分为二氢海松醇、二氢枞醇、四氢枞醇和脱氢枞醇等。

关键词: 超临界正己烷, 松香酯, 氢解还原反应, 松香醇

Abstract: Reduction of a series of monobasic alcohol abietates over Cu-Zn catalysts was studied in supercritical hexane phase. The effects of the amount of Cu-Zn catalyst, and hexane, reaction temperature, reaction pressure, and reaction time on the conversion rate and selectives of abietate were investigated. Methyl abietate, butyl abietate, and octyl abietate were used as materials. The conversion rates reached 87.9%, 75.0% and 69.9%, the selectivities reached 93.4%, 92.4% and 92.8%, and the yields of abietinol reached 82.1%, 69.3% and 64.9%, respectively, when the reaction was conducted under the conditions of abietate 15 g, the amount of Cu-Zn catalyst 10%, the ratio of m(abietate) to m(hexane) 1:3, temperature 270 ℃, pressure 10 MPa, and reaction time 11 h. The analysis results of FT-IR and GC-MS showed that the ester group of abietate was reduced to hydroxyl group and the main components of the reduction products were dihydropimaric alcohol, dihydroabietic alcohol, tetrahydroabietic alcohol, and dehydropimaric alcohol.

Key words: supercritical hexane, abietate, reduction, abietinol

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