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日用化学工业 ›› 2020, Vol. 50 ›› Issue (10): 711-716.doi: 10.3969/j.issn.1001-1803.2020.10.010

• 开发与应用 • 上一篇    下一篇

活性炭负载磷钨酸季铵盐催化合成罗汉柏木烷酮

张胜1(),朱凯1,2()   

  1. 1.南京林业大学 化学工程学院,江苏 南京 210037
    2.南京林业大学 江苏省林业资源高效加工利用协同创新中心,江苏 南京 210037
  • 收稿日期:2019-12-10 修回日期:2020-09-09 出版日期:2020-10-22 发布日期:2020-10-22
  • 通讯作者: 朱凯
  • 作者简介:张 胜(1995-),男,硕士研究生,电话:15251878910,E-mail: 1071929101@qq.com
  • 基金资助:
    国家重点研发计划(2018YFD0600405);江苏高校优势学科建设工程项目(PAPD)

Synthesis of thujopsanone catalyzed by activated carbon supported quaternary ammonium phosphotungstate

ZHANG Sheng1(),ZHU Kai1,2()   

  1. 1. College of Chemical Engineering, Nanjing Forestry University, Nanjing, Jiangsu 210037, China
    2. Co-Innovation Center of Efficient Processing and Utilization of Forest Resources, Nanjing Forestry University, Nanjing, Jiangsu 210037, China
  • Received:2019-12-10 Revised:2020-09-09 Online:2020-10-22 Published:2020-10-22
  • Contact: Kai ZHU

摘要:

以磷钨酸、H2O2和十六烷基三甲基氯化铵为原料制备磷钨酸季铵盐催化剂(QAP),并将磷钨酸季铵盐负载在活性炭上制备活性炭负载磷钨酸季铵盐催化剂,通过FT-IR、XRD、SEM等对催化剂进行表征,将其用作合成罗汉柏木烷酮的催化剂。考察了反应条件对氧化反应的影响,得到最佳工艺条件为:磷钨酸季铵盐负载量为30%,反应温度为70 ℃,n(H2O2)∶n(罗汉柏木烯)=1.8∶1,反应时间为6 h,催化剂用量为8%(以罗汉柏木烯质量计,下同)。在此条件下,罗汉柏木烷酮的收率为65.7%,罗汉柏木烯的转化率为90.9%,罗汉柏木烷酮的选择性为72.3%,催化剂可循环使用3次。

关键词: 罗汉柏木烷酮, 活性炭负载磷钨酸季铵盐, 罗汉柏木烯, 香精

Abstract:

A catalyst, namely quaternary ammonium phosphotungstate, was prepared by using phosphotungstic acid, H2O2 and cetyltrimethylammonium chloride as raw materials. Then, activated carbon was used to support the catalyst to form an activated carbon-supported phosphotungstic acid quaternary ammonium salt catalyst. The structure of the catalyst was characterized by FT-IR, XRD and SEM. It was used as a catalyst for the synthesis of thujopsanone. The effects of reaction conditions on the oxidation were studied. The optimized reaction was obtained under the conditions as follows: quaternary ammonium phosphotungstate loading was 30%; the reaction temperature was 70 ℃; the molar ratio of raw materals was n(H2O2)∶n(thujopsene) of 1.8∶1; the reaction time was 6 h; the catalyst was added in the amount corresponding to 8% of thujopsene. Meanwhile, the yield of thujopsanone, the conversion of thujopsene and the selectivity to thujopsanone were 65.7%, 90.9% and 72.3%, respectively, and the catalyst could be recycled for three times.

Key words: thujopsanone, activated carbon supported quaternary ammonium phosphotungstate, thujopsene, essence

中图分类号: 

  • TQ655