化工学报 ›› 2011, Vol. 62 ›› Issue (2): 515-519.

• 材料化学工程与纳米技术 • 上一篇    下一篇

Pd/CMK-3的合成及其在Suzuki-Miyaura碳-碳偶联反应中的应用

高婷婷,姬广斌   

  1. 南京航空航天大学材料科学与技术学院
  • 出版日期:2011-02-05 发布日期:2011-02-05

Synthesis of Pd/CMK-3 and its application in Suzuki-Miyaura carbon-carbon coupling reaction

GAO TingtingJI Guangbin   

  • Online:2011-02-05 Published:2011-02-05

摘要:

利用介孔二氧化硅(SBA-15)为模板、蔗糖为碳源,制备了有序介孔碳材料CMK-3,然后以CMK-3为载体,利用浸渍还原法得到介孔碳负载Pd纳米粒子的复合催化剂(Pd/CMK-3),通过XRDTEM以及氮气吸附-脱附等手段对催化剂的微结构和组分进行分析,结果表明CMK-3为有序介孔结构,孔径约为5nmPd/CMK-3保留了介孔结构,且孔道中负载有不同尺寸的Pd粒子。应用于无配体催化的Suzuki-Miyaura

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Abstract:

Ordered mesoporous carbon material of CMK-3 was prepared with mesoporous silica SBA-15 as template and sucrose as carbon source, then CMK-3 was loaded mono-dispersed Pd by the impregnation-reduction method.The catalyst system nanoparticles Pd/CMK-3 was characterized by X-ray diffraction (XRD), transmission electron microscope (TEMand N2 adsorption-desorption, and the results indicated that CMK-3 was ordered mesoporous structure with pore diameter of 5 nm, and Pd/CMK-3 retained the mesoporous structure with Pd particles of different sizes loaded in the channels.Pd/CMK-3 was used in the ligand-free Suzuki-Miyaura CC coupling reaction as catalyst.The result showed that Pd/CMK-3 had higher stability and activity compared with activated carbon, and addition of water in the solvent was helpful in increasing yield, so when bromobenzene and benzene boric acid reacted at 70 for 6 h with potassium carbonate as the base and EtOH / water as the solvent and Pd/CMK-3 as the catalyst, the yield of biphenyl was up to 89.0%.

Key words: FONT-FAMILY: Calibri,sans-serif, mso-bidi-font-size: 11.0pt, mso-bidi-font-family: 宋体, mso-font-kerning: 1.0pt, mso-ansi-language: EN-US, mso-fareast-language: ZH-CN, mso-bidi-language: AR-SA, mso-fareast-font-family: 宋体, mso-hansi-font-family: 宋体">SBA-15FONT-FAMILY: 宋体, mso-bidi-font-size: 11.0pt, mso-ascii-font-family: Calibri, mso-bidi-font-family: 宋体, mso-font-kerning: 1.0pt, mso-ansi-language: EN-US, mso-fareast-language: ZH-CN, mso-bidi-language: AR-SA">;有序介孔碳;FONT-FAMILY: Calibri,sans-serif, mso-bidi-font-size: 11.0pt, mso-bidi-font-family: 宋体, mso-font-kerning: 1.0pt, mso-ansi-language: EN-US, mso-fareast-language: ZH-CN, mso-bidi-language: AR-SA, mso-fareast-font-family: 宋体, mso-hansi-font-family: 宋体">Pd/CMK-3FONT-FAMILY: 宋体, mso-bidi-font-size: 11.0pt, mso-ascii-font-family: Calibri, mso-bidi-font-family: 宋体, mso-font-kerning: 1.0pt, mso-ansi-language: EN-US, mso-fareast-language: ZH-CN, mso-bidi-language: AR-SA">;FONT-FAMILY: Calibri,sans-serif, mso-bidi-font-size: 11.0pt, mso-bidi-font-family: 宋体, mso-font-kerning: 1.0pt, mso-ansi-language: EN-US, mso-fareast-language: ZH-CN, mso-bidi-language: AR-SA, mso-fareast-font-family: 宋体, mso-hansi-font-family: 宋体">Suzuki-Miyaura FONT-FAMILY: 宋体, mso-bidi-font-size: 11.0pt, mso-ascii-font-family: Calibri, mso-bidi-font-family: 宋体, mso-font-kerning: 1.0pt, mso-ansi-language: EN-US, mso-fareast-language: ZH-CN, mso-bidi-language: AR-SA">碳