CN105628810B - A kind of seizure heterogeneous catalytic reaction intermediate product device and its application method in situ - Google Patents

Abstract

The invention discloses a device and method for in-situ capturing heterogeneous catalytic reaction intermediates. The device includes a reaction gas control system, an in-situ infrared pool system, and an analysis and testing system. This device can carry out heterogeneous catalytic reaction with variable temperature under low pressure (≤1.0MPa). It can monitor and track the catalyst active species, reaction intermediates and reaction products in the catalytic reaction in real time, and can observe the reaction process online with various catalytic reactions. Changes in reaction conditions, such as the effect of reaction raw material gas ratio, reaction temperature, reaction pressure, etc. Quantitative and qualitative analysis can be carried out by the instrument, especially the online monitoring of intermediates and products with low content (ppm level), so that the performance of catalysts can be compared and the mechanism of heterogeneous catalytic reactions can be studied. Compared with the prior art, the data of the present invention are accurate and easy to operate, and have great significance for the research on the reaction mechanism of heterogeneous catalysis.

Description

A device for in-situ capture of heterogeneous catalytic reaction intermediate products and its application method

technical field

The invention relates to a device for capturing heterogeneous catalytic reaction intermediate products in situ and an application method thereof.

Background technique

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.

Infrared spectroscopy is one of the powerful tools for understanding chemical reactions, because chemical reactions usually involve the breaking and formation of chemical bonds, and infrared spectroscopy can provide information such as relative vibration between atoms in molecules and molecular rotation. However, neither the transmission method nor the diffuse reflectance method can reveal the characteristic peaks of homonuclear diatomic molecules (such as N ₂ , H ₂ , O ₂ , Cl ₂ , etc.), which affects the analysis of homonuclear diatomic molecules. The analysis of reactions involving nuclear diatomic molecules. In addition, the sensitivity and precision of in-situ infrared instruments are not high enough, and components with a content of less than 1% are difficult to be detected, and their analysis is mostly qualitative.

Gas chromatography-mass spectrometry (GC-MS) is a method that combines the characteristics of gas chromatography and mass spectrometry to identify different substances in a sample. Gas chromatography (GAS CHROMATOGRAPHY, GC) has a strong separation ability, and mass spectrometry (MASSSPECTROMETRY, MS) has a unique ability to identify unknown compounds with high sensitivity, so GC-MS is one of the most powerful tools for separating and detecting complex compounds First, it can be used as a useful supplement to capture reaction intermediates by in situ infrared spectroscopy. However, there is no report on the use of gas chromatography-mass spectrometry to capture the intermediate state of the reaction.

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 be monitored online in real time.

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 Real-time online monitoring of O ₂ and H ₂ in the reaction process cannot be achieved.

Patent CN103969186A reports an in-situ infrared spectroscopic cell, which provides an in-situ infrared spectroscopic cell that can perform simultaneous or mutual switching of photothermal reaction conditions and has high heating efficiency and accurate temperature measurement of samples. The homonuclear diatomic molecules cannot be monitored on-line in real time.

It can be seen that although the in-situ infrared instrument can capture the adsorption and desorption forms, reaction process and products of most reactants, it cannot do so for homonuclear diatomic molecules (such as N ₂ , H ₂ , O ₂ , Cl ₂ , etc.). Real-time on-line monitoring cannot provide sufficient data for the research on the reaction mechanism of such substances. For example, for exploring the reaction mechanism of _H2 and _O2 , the existing in-situ infrared instrument cannot provide sufficient data.

At present, there is no report on the capture of adsorption, desorption and reaction processes by in-situ infrared coupled gas chromatography-mass spectrometry. The mechanism of the phase-catalyzed reaction is of great significance.

Contents of the invention

The object of the present invention is to provide a device and method for in-situ capture of heterogeneous catalytic reaction intermediate products. The in-situ infrared system is used to capture and collect the infrared characteristic spectra of reaction raw materials, intermediate products and products. Separation, capture, and collection of reaction raw materials, intermediate products, and product chromatograms and mass spectrometry fragment characteristic spectra. This device can be used to capture intermediate products of heterogeneous catalytic reactions and study the mechanism of catalytic reactions.

The present invention provides a device for in-situ capturing of intermediate products of heterogeneous catalytic reactions, including a reaction gas control system X, an in-situ infrared reaction system Y, and an analysis and testing system Z. in:

The reaction gas control system X includes three paths of raw material gas 1, 2, and 3, one path of purge gas 4, and a gas mixer 5. The raw material gas and purge gas pipelines include a mass flow meter a, a shut-off valve b, and a one-way valve c. The raw material gas and purge gas are externally connected to cylinder gas;

The in-situ infrared reaction system Y includes an in-situ infrared cabinet 31 and an in-situ infrared reactor 32;

The in-situ infrared box 31 includes a purge gas inlet 14 , a purge gas outlet 15 , a diffuse reflection light source 16 , and a signal transmission line 17 .

Wherein, the in-situ infrared box 31 is connected to an external power supply for supplying power to the diffuse reflection light source, and the signal transmission line 17 is connected to a computer for transmitting diffuse reflection signals.

The in-situ infrared reactor 32 includes: a reaction pool 7 , a circulating cooling water system 9 , and a top cover 10 for the reaction pool.

The reaction pool 7 is located at the center of the in-situ infrared reactor 32 . It is cylindrical in shape, surrounded by an electric heating belt 11 , and has a thermocouple 17 , a mass spectrometer probe 18 and a stainless steel filter 8 inside. The insertion point of the thermocouple 17 should be in the bed layer of the reaction pool, as close as possible to the position of the mass spectrometer probe 18, so as to ensure the consistency of the data.

The electric heating belt 11 has a temperature programming function, and the thermocouple 19 is used to control the temperature of the electric heating belt.

The stainless steel filter screen 8 is located at the bottom of the reaction tank 7, and the filter screen mesh is 200-500 mesh; the filter screen is used to prevent the catalyst from entering the reaction pipeline, and at the same time plays the role of a gas distributor to make the reaction gas pass through the catalyst bed evenly.

The cooling water circulation system 9 is a cylinder with a cooling water inlet 12 at the bottom and a cooling water outlet 13 at the top; it is used to remove excess heat and maintain the uniformity of the entire temperature. The cooling water is tap water at normal temperature.

The shape of the reaction tank top cover 10 is a cone, and three circular glass mirrors are equidistantly distributed on the cone surface, two of which are used to receive diffuse reflection light sources, and one is used as a visual window with an air outlet on the top, and the bottom of the top cover is used for connecting with the reaction pool. Rubber ring and screw seal connection.

The purge gas 4 and the reaction gas 1, 2 or 3 enter from the bottom 6 of the reaction tank, exit from the top 20 of the reaction tank, respectively pass through the pressure gauge 21, the back pressure valve 22, and the three-way ball valve 23, and the flow direction is controlled by the three-way ball valve, or Vent directly, or enter the analytical test system.

The analysis and test system Z includes a gas chromatograph 24, a mass spectrometer 25, and mass spectrometer probes 30, 18, and 29, wherein the gas chromatograph uses FID and TCD dual detectors, the FID uses a capillary column, the TCD uses a packed column, and three mass spectrometer probes 30, 18, and 29 are respectively inserted into the reaction gas mixer, the catalyst loading area of the in-situ infrared reaction cell, and the gas outlet at the top of the in-situ infrared cell to analyze the composition changes of gases in different parts.

The specific steps of the method for using the device for capturing the intermediate product of the heterogeneous catalytic reaction in situ are as follows:

A. Place a stainless steel filter screen 8 at the bottom of the in-situ reaction pool 7, fill the catalyst sample that is ground into less than 100 meshes into the in-situ infrared reaction pool 7, insert the thermocouple 17 and the mass spectrometer probe 18 into the reaction pool 7, Flatten the catalyst on the surface and cover the top cover 10, tighten the screws, put it into the in-situ reaction box 31 and fix it, the temperature measuring point of the thermocouple and the mass spectrometer probe in the reaction area should be as close as possible, so that the captured The species energy of the intermediate product and the reaction temperature can be related to each other;

B. Connect the reaction gas paths 1, 2 and 3, wherein the reducing gas can be used in one of the three reaction gas paths, and connect the purge gas path 4 of the in-situ infrared reaction cell and the purge gas 14 of the in-situ reaction box;

C. Connect the cooling water 12, 13, connect the heating circuit and the in-situ infrared emission source circuit 16, open the chromatograph 24 and the mass spectrometer 25;

D. Purge inert gas from 4 to the in-situ infrared reaction cell, and purge inert gas from 14 to the in-situ reaction box. The purpose of purging the in-situ reaction box is to reduce the impact of CO ₂ and water vapor in the air. The impact of data collection, the inert gas used can be N ₂ , Ar, He, etc., preferably N ₂ ;

E. The catalyst is reduced or activated, and the reducing gas can be either _H2 or CO or a mixture of both;

F. Introduce the reaction gas to start the reaction, adjust the reaction pressure and reaction temperature according to the reaction conditions, the reaction pressure is controlled at 0-1.0MPa, the reaction pressure is controlled by the linkage of the inlet gas pressure and the back pressure valve 22, and the reaction temperature is controlled at room temperature-500 ℃;

G. Use the in-situ infrared instrument to collect infrared data, and use the gas chromatograph and mass spectrometer of the analysis and testing system to collect intermediate product and product data. In order to ensure the consistency of the reaction data, it is necessary to ensure that the in-situ infrared instrument, gas chromatograph, and mass spectrometer The acquisition time is kept synchronized, so that the collected data can truly reflect the real-time situation of the reaction;

H. Turn off the reaction gas, turn off the heating power supply, cool to room temperature with an inert gas, turn off the cooling water, and end the test;

I. Data analysis.

The device and its method are suitable for gas-solid phase heterogeneous catalytic reactions, such as the reaction of _H2 and _O2 , the reaction of CO and _O2 , the reaction of the mixed gas of CO and _H2 and _O2 , the reaction of CO and MN (sub- Methyl nitrate) to synthesize dimethyl carbonate, _CO and MN to synthesize dimethyl oxalate, NO and _O2 , H2S and _O2 , SO2 and _O2 , _CO and H The Fischer-Tropsch reaction of ₂ , the reaction of _NH3 and _O2 , etc., preferably the reaction of _H2 and _O2 , the reaction of CO and _O2 , the reaction of the mixed gas of CO and _H2 and _O2 , the synthesis of dicarbonate by CO and MN The reaction of methyl ester, the reaction of CO and MN to synthesize dimethyl oxalate, the Fischer-Tropsch reaction of CO and _H2 .

The present invention has the following advantages:

The invention is a heterogeneous catalytic reaction device for capturing reaction intermediate products under in-situ continuous reaction conditions, which can carry out heterogeneous catalytic reactions with variable temperature under low pressure (≤1.0MPa), and can treat catalyst active species and reaction intermediate products in catalytic reactions Real-time monitoring and tracking of reaction products, etc., can observe the change of catalytic reaction process with various reaction conditions online, such as the influence of reaction raw material gas ratio, reaction temperature, reaction pressure, etc. The reactants, intermediate products and products are quantitatively and qualitatively analyzed by in-situ infrared instrument, gas chromatograph and mass spectrometer, especially the intermediate products and products with low content (ppm level) can be monitored online, so that the catalyst can be monitored The performance comparison is of great significance for the study of the mechanism of heterogeneous catalytic reactions.

Description of drawings

Figure 1 is a schematic diagram of a capture heterogeneous catalytic reaction device.

Among them, X is the gas control system, Y is the in-situ infrared reaction system, Z is the analysis and testing system, 1, 2, 3 are the three-way reaction gas circuit, 4 is the purge gas circuit, a is the stop valve, b is the mass flow rate C is a one-way valve, 5 is a gas mixer, 6 is a reaction gas inlet, 7 is a reaction tank, 8 is a stainless steel filter, 9 is a reactor shell, 10 is a cover, and 11 is an electric heating belt for programmed temperature rise , 12 is the cooling water inlet, 13 is the cooling water outlet, 14 is the purge gas inlet, 15 is the purge gas outlet, 16 is the diffuse reflection light source, 17 is the thermocouple, 18 is the in-situ infrared reaction cell mass spectrometer probe, 19 20 is a reaction gas outlet, 21 is a pressure gauge, 22 is a back pressure valve, 23 is a three-way ball valve, 24 is a gas chromatograph, 25 is a mass spectrometer, 26 is a computer, 27 and 28 are signal transmission lines, 29 is a gas mass spectrometer probe after reaction, 30 is a gas mixer mass spectrometer probe, 31 is an in-situ reaction box, and 32 is an in-situ infrared reactor.

FIG. 2 is a cross-sectional view of the in-situ infrared reactor 32 .

Fig. 3 is the in situ infrared spectrum of the reaction of CO and MN on the Pd--Al ₂ O ₃ catalyst at different temperatures (30°C, 90°C, 110°C, 130°C) in Example 1.

Fig. 4 is the in situ infrared spectrum of intermediate products and products when CO and MN react on Pd--Al ₂ O ₃ catalyst at different temperatures (30°C, 90°C, 110°C, 130°C) in Example 1.

Fig. 5 is the in-situ infrared spectrum of CO, H ₂ and O ₂ reacting on Pd--Al ₂ O ₃ catalyst at 220°C in Example 2.

Fig. 6 is the online mass spectrogram of CO, H ₂ and O ₂ reacting on Pd--Al ₂ O ₃ catalyst at 220°C in Example 2.

Fig. 7 is an online chromatogram of CO, H ₂ and O ₂ reacting on Pd--Al ₂ O ₃ catalyst at 220°C in Example 2.

specific embodiment

Example 1: Research on the reaction of CO and MN (methyl nitrite) over Pd-Al ₂ O ₃ catalyst.

Fill the in-situ infrared reaction cell 7 through grinding to 120 mesh Pd-Al ₂ O ₃ catalyst, insert thermocouple 17 and mass spectrometer probe 18 in the in-situ reaction cell 7, put the catalyst on the surface of the in-situ infrared reaction cell body After flattening, cover the in-situ pool cover 10, tighten the screws and put it into the in-situ reaction box 31, and connect the reaction gas path 1 (connected to the CO gas path) and 2 (connected to the MN gas path), 3 (connected to the reducing gas H ₂ gas path), 4 (connected to inert gas N ₂ ), pass purge gas N ₂ into the box through 14, pass into N ₂ to purge the reaction pool through gas path 4, pass into cooling water through 12, and turn on the heating For the circuit and the in-situ infrared emission source circuit, after purging for 10 minutes, gradually heat up to 80°C, gradually reduce the gas flow in 4, and gradually feed H ₂ in 3, after the flow is stable, heat up to 160°C, and reduce the catalyst with H ₂ for 30 minutes Cool down to room temperature, turn off _H2 , purge the _H2 in the pipeline with _N2 from 4, then feed CO and MN from 1 and 2 to start the reaction, control 22 to keep the reaction pressure at 0.3MPa, and select 30°C respectively , 90°C, 110°C, 130°C 4 temperature points to collect data.

Fig. 3 is the in situ infrared spectrum of the reaction of CO and MN on the Pd--Al ₂ O ₃ catalyst at different temperatures (30°C, 90°C, 110°C, 130°C). In the figure, 1765cm ^-1 , 1211cm ^-1 and 1159cm ^-1 are the characteristic peaks of the product dimethyl oxalate.

Figure 4 is the in situ infrared spectra of intermediate products and products when CO and MN react on Pd--Al ₂ O ₃ catalyst at different temperatures (30°C, 90°C, 110°C, 130°C). In the figure, 1778cm ^-1 , 1754cm ^-1 , 1745cm ^-1 , 1733cm ^-1 , 1717cm ^-1 are the in-situ infrared characteristic peaks of the intermediate products OC-COOCH ₃ , COOCH ₃ , OCCO, and 1865cm ^-1 is the characteristic peak of the product NO.

It can be seen from Figure 3 and Figure 4 that the in-situ infrared device captured the characteristic peaks of OC-COOCH ₃ , COOCH ₃ , and OCCO, the intermediate products of the reaction between CO and MN. These characteristic peaks are the reaction of CO and MN to form dimethyl oxalate. The study of the reaction mechanism provided important information, which enabled us to further understand the course of the CC coupling reaction.

Example 2: Study on the reaction of CO, H ₂ and O ₂ over Pd-Al ₂ O ₃ catalyst.

Fill the in-situ infrared reaction cell 7 through grinding to 300 mesh Pd-Al ₂ O ₃ catalyst, insert thermocouple 17 and mass spectrometer probe 18 in the in-situ reaction cell 7, put the catalyst on the surface of the in-situ infrared reaction cell body After flattening, cover the in-situ pool cover 10, put it into the in-situ reaction box 31 after tightening the screws, and connect the reaction gas circuit 1 (connected to the CO gas circuit) and 2 (connected to the H ₂ gas circuit), 3 (connected to the O ₂ gas circuit) Gas path), 4 (connected to inert gas N ₂ ), pass purge gas N ₂ into the box through 14, pass into N ₂ to purge the reaction pool through gas path 4, pass into cooling water through 12, and connect the heating circuit And the in-situ infrared emission source circuit, after purging for 10 minutes, gradually raise the temperature to 50°C, gradually reduce the flow rate of 4 gases, and gradually feed the three-way reaction gas through 1, 2, 3. After the flow rate is stable, control 22 to keep the reaction pressure at 1.0 MPa, the temperature was raised to 220°C to start the reaction, and the data was collected.

Figure 5 is the in situ infrared spectrum of CO, H ₂ and O ₂ reacting on Pd--Al ₂ O ₃ catalyst at 220 °C. In the figure, 3680cm ^-1 is the characteristic peak of OH, 2375cm ^-1 is the characteristic peak of _CO2 , 2175cm-1 is the characteristic peak of gaseous CO, 2080cm ^{- 1} is the linear adsorption peak (transition state) of CO, and 1975cm ^-1 is CO The bridge adsorption peak (transition state), 1382cm ^-1 is the characteristic peak of the intermediate product CO ₃ ^2- .

Figure 6 is the online mass spectrum of CO, H ₂ and O ₂ reacting on Pd--Al ₂ O ₃ catalyst at 220 °C. In the figure, the peak with atomic number 1-2 is H peak, the peak with atomic number 14-18 is the peak of OH and H ₂ O, the peak with atomic number 26-32 is the peak of N ₂ , CO, O ₂ , The peak with atomic number 44 is the peak of CO ₂ , and the peak with atomic number 60 is the peak of HCO ₃ ^- .

Figure 7 is the online chromatogram of CO, _H2 and _O2 reacting on Pd _{-- Al2O3} catalyst at 220 °C. Figure 7-1 comes from sampling port 5, which is the chromatogram of the three reactants before the reaction. The first peak (2.2s) represents the peak of _H2 , the second peak (3.9s) represents the peak of _O2 , and the first peak (2.2s) represents the peak of O2. Three peaks (13.1s); Figure 7-2 comes from the sampling port 20, and the peak positions of the three species are consistent with Figure 7-1.

In Figure 5, the in-situ infrared device captured the characteristic peak of CO ₃ ^2- , the intermediate product of the reaction of CO, H ₂ and O ₂ , which gave us a further understanding of the course of the reaction of CO, H ₂ and O ₂ . In Figure 6, the mass spectrum captures the characteristic peaks of the intermediate products H, OH, and HCO ₃ ^- of the reaction of CO, H ₂ and O ₂ , which can be correlated with the in-situ infrared data in Figure 5 to analyze the intermediate products of the reaction. The chromatographic data in Figure 7 can be supplemented to the data in Figures 5 and 6 to verify the effect of the catalyst.

It is illustrated from Fig. 3 to Fig. 7 that the device of the present invention can capture the reaction intermediate product very well, which is beneficial to the research of the catalytic reaction mechanism.

Claims (4)

1. An in-situ device for capturing heterogeneous catalytic reaction intermediate products, including a reaction gas control system X, an in-situ infrared reaction system Y, and an analysis and testing system Z, wherein: The reaction gas control system X includes three paths of raw material gas (1), (2), (3), one path of purge gas (4), a gas mixer (5), and the raw material gas and purge gas pipelines include mass flow meters ( a), cut-off valve (b) and one-way valve (c), raw material gas and purge gas are externally connected to cylinder gas; The in-situ infrared reaction system Y includes an in-situ infrared cabinet (31) and an in-situ infrared reactor (32); The in-situ infrared box (31) includes a purge gas inlet (14), a purge gas outlet (15), a diffuse reflection light source (16), and a signal transmission line (17); Wherein, the in-situ infrared box (31) is connected to an external power supply for supplying power to the diffuse reflection light source, and the signal transmission line (17) is connected to a computer for transmitting diffuse reflection signals; The in-situ infrared reactor (32) includes: a reaction tank (7), a circulating cooling water system (9), and a reaction tank top cover (10); The reaction pool (7) is located at the center of the in-situ infrared reactor (32), and is cylindrical in shape, surrounded by an electric heating belt (11), and inside is a thermocouple (17), a mass spectrometer probe (18), and a stainless steel filter screen (8); the insertion point of the thermocouple (17) should be in the reaction pool bed, as close as possible to the position of the mass spectrometer probe (18), to ensure the consistency of the data; The electric heating belt (11) has a temperature programming function, and the thermocouple (19) is used to control the temperature of the electric heating belt; The stainless steel filter screen (8) is positioned at the bottom of the reaction tank (7), and the filter screen mesh is at 200-500 mesh; The cooling water circulation system (9) is a cylinder with a cooling water inlet (12) at the bottom and a cooling water outlet (13) at the top; The shape of the reaction tank top cover (10) is a cone, and three circular glass mirrors are equidistantly distributed on the cone surface, two of which are used to receive diffuse reflection light sources, and one is used as a visual window with an air outlet on the top, and the bottom of the top cover is connected to the reaction tank. The pool is sealed with rubber rings and screws; The purge gas (4) and reaction gas (1), (2) or (3) enter from the bottom of the reaction tank (6), exit from the top of the reaction tank (20), and pass through the pressure gauge (21) and the back pressure valve ( 22), three-way ball valve (23), the flow direction is controlled by the three-way ball valve, or it is directly vented, or enters the analysis and testing system; Analytical testing system Z comprises gas chromatograph (24), mass spectrometer (25), mass spectrometer probe (30), (18), (29), wherein gas chromatograph adopts FID and TCD double detector, and FID adopts capillary column, TCD uses a packed column, and three mass spectrometer probes (30), (18), (29) are respectively inserted into the reaction gas mixer, the catalyst loading area of the in-situ infrared reaction cell, and the gas outlet at the top of the in-situ infrared cell to analyze the gases in different parts compositional changes. 2. a method for using the in-situ capture heterogeneous catalytic reaction intermediate product device according to claim 1: the specific steps are as follows: A. Place a stainless steel filter (8) at the bottom of the in-situ reaction cell (7), fill the catalyst sample that is ground to a size less than 100 mesh into the in-situ infrared reaction cell (7), insert the thermocouple (17) and the mass spectrometer Insert the needle (18) into the reaction pool (7), flatten the catalyst on the surface and cover the top cover (10), tighten the screws, put it into the in-situ reaction box (31) and fix it, the temperature measuring point of the thermocouple The mass spectrometer probe in the reaction area should be as close as possible, so that the captured intermediate species can be correlated with the reaction temperature; B. Connect the reaction gas paths (1), (2) and (3), among which the reducing gas can be used in one of the three reaction gas paths, and connect the purge gas path (4) of the in-situ infrared reaction cell with the in-situ Reaction cabinet purge gas (14); C. Connect the cooling water (12), (13), connect the heating circuit and the in-situ infrared emission source circuit (16), open the chromatograph (24) and the mass spectrometer (25); D. Purge inert gas from (4) to the in-situ infrared reaction cell, and purge inert gas from (14) to the in-situ reaction box. The purpose of purging the in-situ reaction box is to reduce CO ₂ in the air , The impact of water vapor on the collected data, the inert gas used is one of N ₂ , Ar, He; E. The catalyst is reduced or activated, and the reducing gas can be either _H2 or CO or a mixture of both; F. Feed the reaction gas to start the reaction, adjust the reaction pressure and reaction temperature according to the reaction conditions, the reaction pressure is controlled at 0-1.0MPa, the reaction pressure is controlled by the linkage of the inlet gas pressure and the back pressure valve (22), and the reaction temperature is controlled at room temperature -500°C; G. Use the in-situ infrared instrument to collect infrared data, and use the gas chromatograph and mass spectrometer of the analysis and testing system to collect intermediate and product data. In order to ensure the consistency of the reaction data, it is necessary to ensure that the in-situ infrared instrument, gas chromatograph, and mass spectrometer The acquisition time is kept synchronized, so that the collected data can truly reflect the real-time situation of the reaction; H. Turn off the reaction gas, turn off the heating power supply, cool to room temperature with an inert gas, turn off the cooling water, and end the test; I. Data analysis. 3. The method for using the in-situ capture heterogeneous catalytic reaction intermediate product device according to claim 2, characterized in that the device is suitable for the reaction of _H2 and _O2 , the reaction of CO and _O2 , the reaction of CO and _H2 The reaction of mixed gas and _O2 , the reaction of CO and methyl nitrite to synthesize dimethyl carbonate, the reaction of _CO and methyl nitrite to synthesize dimethyl oxalate, the reaction of NO and _O2 , the reaction of H2S and _O2 Any gas-solid heterogeneous catalytic reaction in the reaction, the reaction of SO ₂ and O ₂ , the Fischer-Tropsch reaction of CO and H ₂ , the reaction of NH ₃ and O ₂ . 4. The method for using the in-situ capture heterogeneous catalytic reaction intermediate product device according to claim 2, characterized in that the device is suitable for the reaction of _H2 and _O2 , the reaction of CO and _O2 , the reaction of CO and _H2 Any gas-solid heterogeneous catalytic reaction in the reaction of mixed gas and _O2 , the reaction of CO and MN to synthesize dimethyl carbonate, the reaction of CO and MN to synthesize dimethyl oxalate, and the Fischer-Tropsch reaction of CO and _H2 .