In-situ capture heterogeneous catalytic reaction intermediate product device and use method thereof

A heterogeneous catalysis and reaction technology, applied in measurement devices, instruments, scientific instruments, etc., can solve the problems of inability to provide sufficient reaction mechanism research, insufficient data, and inability to achieve real-time online monitoring.

Active Publication Date: 2016-06-01
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Patent CN102590090A reports an in-situ infrared spectroscopic cell for studying the gas-liquid-solid three-phase interface, which can study the adsorption, desorption and reaction behaviors that occur at the gas-liquid-solid three-phase interface, but the device is not sensitive to homonuclear double Atoms and molecules cannot achieve real-time online monitoring
[0006] Patent CN103846072A reports a reaction cell for in-situ infrared monitoring, which is used in conjunction with the Mettler-Toledo online infrared analyzer for in-situ monitoring of high-temperature and high-pressure liquid phase reactions such as oxidation and hydrogenation. Similarly, the device O in the reaction process 2 and H 2 Unable to achieve real-time online monitoring
[0007] Patent CN103969186A reports an in-situ infrared spectroscopic cell, which provides an in-situ infrared spectroscopic cell that can perform simultaneous or mutual switchin

Method used

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  • In-situ capture heterogeneous catalytic reaction intermediate product device and use method thereof
  • In-situ capture heterogeneous catalytic reaction intermediate product device and use method thereof
  • In-situ capture heterogeneous catalytic reaction intermediate product device and use method thereof

Examples

Experimental program
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Embodiment 1

[0045] Embodiment 1: CO and MN (methyl nitrite) in Pd-Al 2 o 3 Reaction studies on catalysts.

[0046] After grinding to 120 mesh Pd-Al 2 o 3 Load the catalyst into the in-situ infrared reaction cell 7, insert the thermocouple 17 and the mass spectrometer probe 18 into the in-situ reaction cell 7, flatten the catalyst on the surface of the in-situ infrared reaction cell body, cover the in-situ cell cover 10, and tighten the screws Put it into the in-situ reaction box 31, connect the reaction gas circuit 1 (connect the CO gas circuit) and 2 (connect the MN gas circuit), 3 (connect the reducing gas H 2 Gas path), 4 (connected to inert gas N 2 ), pass the purge gas N into the box through 14 2 , into N through gas path 4 2 Purge the reaction tank, pass cooling water through 12, connect the heating circuit and in-situ infrared emission source circuit, gradually heat up to 80°C after purging for 10 minutes, gradually reduce the gas flow rate in 4, and gradually pass in H throu...

Embodiment 2

[0050] Example 2: CO, H 2 and O 2 In Pd-Al 2 o 3 Reaction studies on catalysts.

[0051] After grinding to 300 mesh Pd-Al 2 o 3 Load the catalyst into the in-situ infrared reaction cell 7, insert the thermocouple 17 and the mass spectrometer probe 18 into the in-situ reaction cell 7, flatten the catalyst on the surface of the in-situ infrared reaction cell body, cover the in-situ cell cover 10, and tighten the screws Put it into the in-situ reaction box 31, connect the reaction gas path 1 (connected to the CO gas path) and 2 (connected to the H 2 gas path), 3 (connected to O 2 Gas path), 4 (connected to inert gas N 2 ), pass the purge gas N into the box through 14 2 , into N through gas path 4 2 Purge the reaction tank, pass cooling water through 12, connect the heating circuit and the in-situ infrared emission source circuit, gradually heat up to 50°C after purging for 10 minutes, gradually reduce the gas flow rate of 4, and gradually pass through 1, 2, 3 into the th...

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Abstract

The invention discloses an in-situ capture heterogeneous catalytic reaction intermediate product device and a use method thereof. The device comprises a reaction gas control system, an in-situ infrared pool system and an analyzing and testing system. The device can be used for carrying out a temperature-variable heterogeneous catalytic reaction at low pressure (smaller than or equal to 1.0 MPa), a catalyst active species, the reaction intermediate product, a reaction product and the like in the catalytic reaction can be monitored and tracked in real time, the changes, such as the influence of matching of raw material gas, reaction temperature, reaction pressure and the like on the catalytic reaction, of the reaction process along with various catalytic reaction conditions can be observed online, reactants, an intermedium and the product in the catalytic reaction process can be subjected to qualitative and quantitative analysis through an in-situ infrared instrument, a gaschromatograph and the mass-spectrography, especially the intermedium and the product with low content (ppm grade) can be monitored online, and therefore the performance of catalysts can be compared, and the heterogeneous catalytic reaction mechanism can be studied. Compared with the prior art, data is precise, operation is easy, and the device has great significance on heterogeneous catalytic reaction mechanism study.

Description

technical field [0001] The invention relates to a device for capturing heterogeneous catalytic reaction intermediate products in situ and an application method thereof. Background technique [0002] The heterogeneous catalytic reaction process is closely related to people's life, and has always been the basis of chemical and chemical processes. Over the years, scientists from all over the world have tried various methods and tried to use some in-situ analyzers on various analytical instruments, such as in-situ infrared, in-situ Raman, in-situ electron microscopy, in-situ NMR and other means to capture multiple The transition state and intermediate state of the phase catalysis reaction, study the reaction mechanism, in order to uncover the "black box" in the reaction process. 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. [0003] Infrared spe...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/025
Inventor 姚元根周张锋乔路阳陈瑞平崔国静宗珊珊吴小满潘鹏斌林凌覃业燕
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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