Multiphase catalytic reaction device for testing in situ solid-state nuclear magnetic resonance

A technology of heterogeneous catalysis and reaction devices, which is applied in the direction of analysis by nuclear magnetic resonance, measurement devices, chemical analysis by catalysis, etc., and can solve the problems of high difficulty consumption and few

Inactive Publication Date: 2010-01-27
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the high difficulty of the experimental technique and the high consumption in the experimental process, there are very few research groups that have been able to realize this technique so far.
Professor Hunger realized the in-situ heterogeneous catalytic reaction on Bruker's solid-state nucle...

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  • Multiphase catalytic reaction device for testing in situ solid-state nuclear magnetic resonance
  • Multiphase catalytic reaction device for testing in situ solid-state nuclear magnetic resonance
  • Multiphase catalytic reaction device for testing in situ solid-state nuclear magnetic resonance

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Embodiment 1

[0043] Example 1: Laser Induced Hyperpolarization 129 Study on the Pore Structure of ZSM-35 Molecular Sieve by Xe Magic Angle Spin NMR

[0044] image 3 It is a structural schematic diagram of ZSM-35 molecular sieve (Zeolites, 1989, 9, 68), which has two pore structures: columnar straight channels parallel to the c-axis and cages along the b-axis (such as Figure 4 bcavity shown). We performed temperature-variable hyperpolarization of the pore structure of ZSM-35 using the aforementioned in situ continuous flow magic-angle spinning probe 129 Xe NMR studies.

[0045] Figure 4 A is the variable temperature hyperpolarization of ZSM-35 under the condition of magic angle rotation speed of 3 kHz 129 Xe NMR spectrum, Figure 4 B is the static hyperpolarization under the corresponding conditions 129 Xe NMR spectrum. The peak of the chemical shift at the low field (larger chemical shift) is assigned to the signal of the straight channel (C channel), and the peak of the chemica...

Embodiment 2

[0046] The adsorption process of embodiment 2 methanol on the HZSM-35 molecular sieve

[0047] Figure 5 is the hyperpolarization of the adsorption process of methanol on HZSM-35 at room temperature 129 Xe magic angle spinning NMR spectra. It can be seen from the relative intensities of the signal peaks of the two channels that as the adsorption time increases, the signal peaks of the straight channels decrease significantly, and after 20 minutes of adsorption, the equilibrium state is reached, and the signals of the straight channels are hardly observed. to, and then into methanol, 129 The Xe spectrum did not change significantly. It shows that methanol is preferentially adsorbed in the straight channel (C channel) of HZSM-35. Stop feeding the above-mentioned samples after methanol vapor adsorption for 40 min, and only feed Xe gas, and investigate the hyperpolarization at different times 129 Xe magic angle spinning NMR spectrum, such as Image 6 shown. It can be seen t...

Embodiment 3

[0048] Example 3: Laser Induced Hyperpolarization 129 Pore ​​structure of CHA-MFI composite molecular sieves studied by Xe magic-angle spinning NMR

[0049] Figure 7 is under continuous flow conditions using the device of the present invention by hyperpolarizing 129 The pore structure of CHA-MFI composite molecular sieves was studied by Xe magic angle spinning NMR technique. It can be seen from the figure that at 25°C 129 There are three signal peaks in the Xe spectrum. In addition to the gas-phase Xe signal at 0ppm, the Xe signal in the adsorbed state in the molecular sieve channel is also observed in the downfield direction. Hyperpolarization of Magic Angle Rotation 129 The Xe spectrum can well distinguish the two pore structures of CHA and MFI. The peak at 84ppm is attributed to the signal of xenon adsorbed in the CHA structure, and the peak at 113ppm is attributed to the signal of xenon adsorbed in the MFI structure. We found that when the temperature increases from ...

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Abstract

The invention relates to a multiphase catalytic reaction device for testing in situ solid-state nuclear magnetic resonance, which is a magic angle spinning multiphase catalytic reactor in which an online solid-state nuclear magnetic resonance system, a quadrupole mass-spectrometer, a gas chromatograph and a laser-induced hyperpolarized 129Xe isotope probe are linked for use. The reactor can apply various solid-state nuclear magnetic resonance techniques to track and detect a catalyst structure, reaction intermediates and species with catalyst activity in the catalytic reaction process; reaction products are qualitatively and quantitatively analyzed by the quadrupole mass-spectrometer and the gas chromatograph, so that the performance of the catalyst is evaluated; simultaneously, laser-induced hyperpolarized 129Xe isotope is used as a probe molecule to study the change of the catalyst structure, adsorption positions and diffusion behaviors of various species in the reaction process and the like. In-situ tracking in the catalytic reaction process and the mechanism of the catalytic reaction can be systematically studied through the various techniques.

Description

technical field [0001] The present invention relates to solid state NMR, specifically an in situ continuous flow magic angle spinning NMR, quadrupole mass spectrometry, gas chromatography and laser induced hyperpolarization 129 A heterogeneous catalytic reaction device for combined detection of Xe isotope probes. Background technique [0002] Heterogeneous catalytic reaction processes have long been the basis of chemical and chemical processes. It is closely related to people's life. Scientists from all over the world have tried various methods over the years, trying to study heterogeneous catalytic reactions in situ on various analytical instruments, in order to uncover the secrets in this "black box". However, due to the complexity of the heterogeneous catalytic reaction process, people only understand the details of the heterogeneous catalytic reaction process in some aspects. Solid-state NMR technology has aroused great interest because it is very suitable for studyin...

Claims

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Application Information

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IPC IPC(8): G01N31/10G01N24/08G01N27/64G01N30/00
Inventor 张维萍刘宪春徐舒涛韩秀文包信和
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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