研究论文

原位固体核磁共振转子插件的设计及其在催化反应中的应用研究

  • 沈雪媛 ,
  • 王瑞琛 ,
  • 齐国栋 ,
  • 徐君 ,
  • 邓风
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  • 1.中国科学院精密测量科学与技术创新研究院,波谱与原子分子物理国家重点实验室,武汉磁共振中心,湖北 武汉 430071
    2.中国科学院大学,北京 100049
*Tel: 027-87197359, E-mail: qgdong@wipm.ac.cn;
# Tel: 027-87197359, E-mail: xujun@wipm.ac.cn.

收稿日期: 2024-05-20

  网络出版日期: 2024-06-21

基金资助

国家重点基础研究发展计划资助项目(2022YFB3504000);中国科学院磁共振技术联盟科研仪器设备研制/功能开发项目(2021gzl004);中国科学院前瞻战略科技先导专项(XDB0540000);国家自然科学基金(22272185);国家自然科学基金(22225205);国家自然科学基金(22320102002);国家自然科学基金(22127801)

Design of in situ Solid-State NMR Rotor Inserts and Their Application to Catalytic Reactions

  • SHEN Xueyuan ,
  • WANG Ruichen ,
  • QI Guodong ,
  • XU Jun ,
  • DENG Feng
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  • 1. National Center for Magnetic Resonance in Wuhan, State Key Laboratory of Magnetic Resonance and Atomic and Molecular Physics, Innovation Academy for Precision Measurement Science and Technology, Chinese Academy of Sciences, Wuhan 430071, China
    2. University of Chinese Academy of Sciences, Beijing 100049, China
*Tel: 027-87197359, E-mail: qgdong@wipm.ac.cn;
# Tel: 027-87197359, E-mail: xujun@wipm.ac.cn.

Received date: 2024-05-20

  Online published: 2024-06-21

摘要

原位固体核磁共振技术(NMR)是研究真实反应条件下催化反应过程的有力工具之一,但传统商用固体NMR转子难以在魔角旋转(MAS)条件下满足反应所需的温度和压力等条件.本文设计并加工了适用于商用固体NMR转子的插件,在转子中能够耐受室温至433 K温度范围以及常压至618.3 kPa密闭压力范围的反应条件,为在NMR磁体内原位研究化学反应提供了一种新的手段.利用该设计,我们通过固体1H MAS NMR实验原位研究了Sn-MFI分子筛上二羟基丙酮的异构化反应,发现二羟基丙酮可经过偕二醇类中间体异构化生成甘油醛的反应途径.

本文引用格式

沈雪媛 , 王瑞琛 , 齐国栋 , 徐君 , 邓风 . 原位固体核磁共振转子插件的设计及其在催化反应中的应用研究[J]. 波谱学杂志, 2025 , 42(1) : 13 -21 . DOI: 10.11938/cjmr20243118

Abstract

In situ solid-state nuclear magnetic resonance (NMR) serves as a powerful means to study catalytic reactions under operating conditions. Standard solid-state NMR rotors typically struggle to match the pressure and temperature of active reactions during sampling. Here, we introduce specialized inserts for commercial solid-state NMR rotors capable of withstanding pressures from atmospheric to 618.3 kPa and temperatures ranging from room temperature up to 433 K. With this innovative design, we examine the isomerization of dihydroxyacetone (DHA) on Sn-MFI zeolite catalyst using in situ 1H MAS NMR, revealing the presence of a gem-diols-type intermediate during the transformation of DHA into glyceraldehyde.

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