有机化学 ›› 2016, Vol. 36 ›› Issue (6): 1412-1418.DOI: 10.6023/cjoc201510037 上一篇    下一篇

研究简报

一种新型竹纤维负载钯催化剂的制备及催化性能

周文俊a,b, 王丹a, 张霞忠a,b, 曾彬a   

  1. a 内江师范学院化学化工学院内江 641112;
    b 四川省高等学校果类废弃物资源化重点实验室内江 641112
  • 收稿日期:2015-10-29 修回日期:2016-01-30 出版日期:2016-06-25 发布日期:2016-02-18
  • 通讯作者: 张霞忠 E-mail:chemzhwj@126.com
  • 基金资助:

    四川省教育厅成果转化培育(No.15CZ0026)、四川省青年基金(Nos.12ZB074,13ZB0002,11ZB024)和内江师范学院博士科研启动费(No.2012B05)资助项目.

Preparation and Catalytic Properties of a Novel Bamboo Fiber Supported-Palladium Catalyst (Fiber-Pd)

Zhou Wenjuna,b, Wang Dana, Zhang Xiazhonga,b, Zeng Bina   

  1. aCollege of Chemistry and Chemical Engineering, Neijiang Normal University, Neijiang 641112;
    b Key Laboratory of Fruit Waste Treatment and Resource Recycling of the Sichuan Provincial College, Sichuan 641112
  • Received:2015-10-29 Revised:2016-01-30 Online:2016-06-25 Published:2016-02-18
  • Supported by:

    Project supported by the Sichuan Province Education Office Fostering Projects (No. 15CZ0026), the Youth Found of Sichuan Province Education Office (Nos. 12ZB074, 13ZB0002, 11ZB024), and the Startup Foundation of Ph. D. Scientific Research of Neijiang Normal University (No. 2012B05).

以竹纤维为原料制备得到一种新型竹纤维负载钯催化剂, 通过X射线光电子能谱(XPS)、X射线衍射(XRD)、热重分析(TG)、电感耦合等离子体原子发射光谱(ICP)、透射电镜(TEM)等技术对催化剂进行了表征, 并将其成功应用于催化四苯硼钠与卤代芳烃的交叉偶联反应中. 该竹纤维负载钯催化剂具有良好的催化活性, 当体系以PEG 400和水(V:V=1:1)为溶剂, NaHCO3为碱, 在85 ℃条件下能以较好的产率获取联芳烃类化合物. 该方法具有条件温和, 反应时间短且收率高, 催化剂经简单过滤即可循环使用等优点.

关键词: 竹纤维负载钯, 制备, Suzuki反应, 四苯硼钠, 卤代芳烃

A novel bamboo fiber supported palladium (Fiber-Pd) catalyst was prepared with diphenylphosphinite fiber and palladium dichloride in ethanol. The as-prepared Fiber-Pd catalyst was characterized by X-ray photoelectron spectrometer (XPS), X-ray diffraction (XRD), thermogravimetric analyses (TGA), inductively coupled plasma-atomic emission spectrometry (ICP-AES), and transmission electron microscopy (TEM). The catalyst was applied to the Suzuki cross-coupling reaction between sodium tetraarylborate and aryl halides. Excellent yields of the corresponding functionalized biaryls were obtained when the reaction was performed in the presence of NaHCO3 as base in PEG 400/H2O at 85 ℃ within a short reaction time. It is noteworthy that the present protocol is highly efficient as 4 equiv. aryl halides reacted with 1 equiv. sodium tetraarylborate cleanly to provide high yield of the cross-coupling products in short reaction time. The catalyst can be easily separated and recovered from the reaction mixture by filtration and reused. This process has significant features of short reaction time, broad substrate scopes, easy isolation of the product, and atom-efficient coupling under mild conditions in environmentally friendly media in air.

Key words: bamboo fiber supported palladium, preparation, Suzuki reaction, sodium tetraphenylborate, aryl halide