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日用化学工业 ›› 2019, Vol. 49 ›› Issue (2): 108-112.doi: 10.3969/j.issn.1001-1803.2019.02.009

• 开发与应用 • 上一篇    下一篇

过氧磷钨酸季铵盐催化合成环氧柏木烷

高炜琳,朱凯()   

  1. 南京林业大学 化学工程学院 江苏省农林生物质化学与利用国家重点实验室培育点,江苏 南京 210037
  • 收稿日期:2018-07-12 修回日期:2019-01-24 出版日期:2019-02-22 发布日期:2019-03-15
  • 通讯作者: 朱凯
  • 作者简介:高炜琳(1993-),女,江苏南通人,硕士研究生,电话:15720610696,E-mail:1151186890@qq.com。
  • 基金资助:
    国家重点研发计划项目(2018YFD0600405)

Synthesis of epoxycedrane catalyzed by quaternary ammonium peroxy phosphotungstate

Wei-lin GAO,Kai ZHU()   

  1. Jiangsu Key Laboratory for the Chemistry & Utilization of Agricultural and Forest Biomass, College of Chemical Engineering, Nanjing Forestry University, Nanjing, Jiangsu 210037, China
  • Received:2018-07-12 Revised:2019-01-24 Online:2019-02-22 Published:2019-03-15
  • Contact: Kai ZHU

摘要:

以钨酸钠、磷酸、过氧化氢(H2O2)和十六烷基三甲基氯化铵为原料制备了过氧磷钨酸季铵盐催化剂。通过FT-IR、TG对催化剂进行了结构和热稳定性的表征。在H2O2为氧化剂,无溶剂条件下,采用过氧磷钨酸季铵盐催化α-柏木烯环氧化合成环氧柏木烷。考察了各反应条件对环氧化反应的影响。结果表明,在反应温度60 ℃,反应时间3.5 h,H2O2α-柏木烯摩尔比为1∶2,催化剂过氧磷钨酸季铵盐用量3.0% (以H2O2质量计,下同),助剂Na2HPO4用量1.6%条件下,环氧柏木烷的收率为65.7%,α-柏木烯的转化率为90.1%,环氧产物选择性可达72.9%。

关键词: 环氧柏木烷, 磷钨酸盐, α-柏木烯;

Abstract:

A catalyst, namely quaternary ammonium peroxy phosphotungstate, was prepared using sodium tungstate, phosphoric acid, hydrogen peroxide and cetyltrimethylammonium chloride. The structure and thermal stability of the catalyst were characterized by infrared spectroscopy (FT-IR) and thermogravimetric analysis (TG). The synthesized catalyst was used in the epoxidation of α-cedrene using H2O2 as oxidant and without any solvent. The effects of reaction conditions on the epoxidation were studied. The optimized reaction conditions were obtained as follows: the reaction temperature was 60 ℃; the reaction time was 3.5 h; the molar ratio of raw materials was n(H2O2)∶nα-cedrene)=1∶2; the catalyst and cocatalyst (Na2HPO4) were added in the amounts corresponding to 3.0% and 1.6% of H2O2, respectively. Meanwhile, the yield of epoxycedrane, the conversion of α-cedrene and the epoxy-product selectivity were 65.7%, 90.1% and 72.9%, respectively.

Key words: epoxycedrane, phosphotungstate, α-cedrene;