广州化学2024,Vol.49Issue(6) :53-59.DOI:10.16560/j.cnki.gzhx.20240612

MS-NH2@Pd-MS纳米催化剂的制备及其在Suzuki反应中的应用

Synthesis of MS-NH2@Pd-MS Nano-catalyst and Its High Catalytic Performance in Suzuki Reaction

戴维清 杨召 梁鹏飞 宋娟
广州化学2024,Vol.49Issue(6) :53-59.DOI:10.16560/j.cnki.gzhx.20240612

MS-NH2@Pd-MS纳米催化剂的制备及其在Suzuki反应中的应用

Synthesis of MS-NH2@Pd-MS Nano-catalyst and Its High Catalytic Performance in Suzuki Reaction

戴维清 1杨召 2梁鹏飞 3宋娟2
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作者信息

  • 1. 南京邮电大学 材料科学与工程学院,江苏 南京 210023
  • 2. 南京邮电大学 材料科学与工程学院,江苏 南京 210023;南京邮电大学 信息材料与纳米技术研究院,江苏 南京 210023
  • 3. 南京邮电大学 信息材料与纳米技术研究院,江苏 南京 210023
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摘要

采用软模板法制备了孔径 4~7 nm的介孔二氧化硅球,经APTS修饰后,通过化学还原法将纳米钯颗粒负载于该介孔二氧化硅球.随后,在负载了纳米钯颗粒的介孔二氧化硅表面再次封装二氧化硅,经表面保护碱蚀刻后形成第二层介孔结构,外层壳体的孔径约为 12~15 nm.通过 XRD、SEM、TEM、XPS、ICP等仪器对其进行的形貌表征结果发现,Pd纳米颗粒在载体上分布均匀,其晶粒尺寸大约为 3~5 nm.此催化剂在Suzuki偶联反应中表现出极好的催化活性和官能团兼容性,收率在90%以上.在回收实验中,催化活性在6次回收后未见明显降低,显示出极好的稳定性和可回收性.

Abstract

This paper reported a nano-palladium catalyst with double-layer mesoporous structure.The inner layer of mesoporous SiO2(MS)was prepared by soft-template method with a pore size of 4~7 nm.After modification with APTS,the nano palladium particles were loaded onto this layer to form MS-NH2@Pd.Subsequently,the silica was then encapsulated on the surface of MS-NH2@Pd,and a second mesoporous structure is formed by surface-protected base etching.The pore diameter of the outer shell is about 12~15 nm.The characterization of XRD,SEM,TEM,XPS showed that the size of Pd nanoparticles was about 3~5 nm which evenly distributed on the carrier.This catalyst showed excellent catalytic activity and functional group compatibility in the Suzuki coupling reaction,and there was no significantly reduction in catalytic activity after 6 times of recovery,which showing excellent stability.

关键词

介孔二氧化硅/纳米Pd/Suzuki偶联反应/非均相催化/过渡金属催化

Key words

mesoporous silica/nano-palladium/Suzuki coupling reaction/heterogeneous catalyst/transition-metal catalysis

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出版年

2024
广州化学
中国科学院广州化学研究所

广州化学

影响因子:0.291
ISSN:1009-220X
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