Application of Mass Spectrometer in Detection of Ionized Intermediates in Catalytic Reaction

A catalytic reaction and mass spectrometry detection technology, applied in the field of catalytic reaction micro-reactors, can solve the problems of limited reaction mechanism research, accurate evaluation of catalytic reaction conditions, limited types of catalytic reaction intermediates, low detection sensitivity and resolution, etc., to achieve rapid Evaluation, scanning speed, high resolution effect

Active Publication Date: 2018-06-29
ZHANGJIAGANG IND TECH RES INST CO LTD DALIAN INST OF CHEM PHYSICS CHINESE ACADEMY OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the existing mass spectrometry technology can only carry out off-line detection of stable products and intermediates after the chemical reaction is completed, and the sample must enter the mass spectrometer through the electrospray ionization process, which has the following disadvantages: (1) For the Intermediate products with a short lifespan cannot be detected; (2) During the process of sample collection, sample injection, electrospray, etc. after the completion of the chemical reaction and before mass spectrometry detection, especially during the electrospray process, additional chemical reactions may occur in the intermediate product. reaction, thus affecting the accuracy of mass spectrometry detection
However, due to the low detection sensitivity and resolution of solid-state nuclear magnetic technology, the types of catalytic reaction intermediates detected are very limited, which limits further research on the reaction mechanism and accurate evaluation of catalyst performance and catalytic reaction conditions.

Method used

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  • Application of Mass Spectrometer in Detection of Ionized Intermediates in Catalytic Reaction
  • Application of Mass Spectrometer in Detection of Ionized Intermediates in Catalytic Reaction

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Embodiment 1

[0032] Such as figure 1 As shown, the catalytic reaction microreactor includes three parts: an inlet, a reaction preparation chamber and a catalytic reaction chamber. The inner diameter and length of the reaction preparation chamber can be designed according to the mass spectrometer model, and the inlet is directly connected to the reaction preparation chamber; The reaction preparation chamber is directly connected to the catalytic reaction chamber, separated by a filter in the middle, and the filter has more than two through holes with a diameter of 0.1-10 microns; the catalytic reaction chamber is directly connected to the entrance of the ion transmission capillary entering the mass spectrometer, and the intermediate passage The filter sheet is separated, and the filter sheet has more than two through holes with a pore size of 0.01-5 microns; the interior of the catalytic reaction chamber is filled with acidic silica-alumina molecular sieves as a reaction catalyst, and the te...

Embodiment 2

[0034] Such as figure 1 As shown, the catalytic reaction micro-reactor includes three parts: an inlet, a reaction preparation chamber and a catalytic reaction chamber. The inner diameter and length of the reaction preparation chamber can be designed according to the mass spectrometer model. In this embodiment, the designed reaction preparation chamber The inner diameter is 0.2mm, the length is 15mm, the diameter of the catalytic reaction chamber is 0.1mm, and the length is 0.8mm. The sample inlet is directly connected to the reaction preparation chamber; With more than 2 through holes with a pore size of 0.1-10 microns; the catalytic reaction chamber is directly connected to the inlet end of the ion transmission capillary entering the mass spectrometer, separated by a filter in the middle, and the filter has more than 2 holes with a pore size of 0.01-5 microns Through holes; the interior of the catalytic reaction chamber is filled with 15 mg of acidic silica-alumina molecular ...

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Abstract

The invention relates to the application of a mass spectrometer in the process of detecting ionized intermediates in a catalytic reaction. The catalytic reaction is carried out in a catalytic reaction microreactor, and the ion channel inlet of the mass spectrometer is directly connected to the catalytic reaction chamber of the catalytic reaction microreactor. integrated. The main advantage of the present invention is that rapid mass spectrometric detection can be performed on ionized intermediates produced in catalytic reactions without additional sample ionization steps, and rapid mass spectrometric detection can be performed on some reaction intermediates with short lifetimes. The catalytic reaction micro-reactor involved in the invention can be used for reaction mechanism research, rapid and accurate evaluation, optimization and screening of catalyst performance and catalytic reaction conditions.

Description

technical field [0001] The present invention relates to a catalytic reaction micro-reactor, specifically a micro-reactor integrated in the entrance of a mass spectrometer ion channel capable of catalytic reaction and its detection of ionized intermediates in catalytic reaction and evaluation of catalyst performance and catalytic reaction conditions in the application. Background technique [0002] In recent years, mass spectrometry technology has developed rapidly, mainly in faster scanning speed, higher resolution, and higher mass accuracy. For example, the Orbitrap mass spectrometer newly launched by Thermo Electric Company of the United States can simultaneously realize fast high-resolution mass spectrometry scanning. Qualitative ability is significantly improved (Senko M.W., ect, Anal. Chem., 2013, 85, 11710). The application of mass spectrometry to the products and intermediates of chemical reactions, including some long-lived free radical intermediates, has played an ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N31/10G01N27/62
Inventor 王方军邹汉法
Owner ZHANGJIAGANG IND TECH RES INST CO LTD DALIAN INST OF CHEM PHYSICS CHINESE ACADEMY OF SCI
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