CN219142659U

CN219142659U - In-situ spectrum device suitable for low-paraffin catalytic system

Info

Publication number: CN219142659U
Application number: CN202223024077.1U
Authority: CN
Inventors: 倪俊; 黄伟峰; 魏航
Original assignee: Beijing Scistar Technology Co ltd; Inner Mongolia University
Current assignee: Beijing Scistar Technology Co ltd; Inner Mongolia University
Priority date: 2022-11-14
Filing date: 2022-11-14
Publication date: 2023-06-06
Anticipated expiration: 2032-11-14

Abstract

The utility model relates to the technical field of spectrum characterization devices, and discloses an in-situ spectrum device suitable for a low-paraffin catalytic system, which comprises an in-situ fixed bed reactor, a spectrometer, a six-way valve, a gas chromatograph and a control display terminal, wherein the control display terminal is arranged on one side of the gas chromatograph, the six-way valve is arranged on the other side of the gas chromatograph, the spectrometer is arranged above the six-way valve, and the in-situ fixed bed reactor is movably connected inside the spectrometer. The in-situ spectrum device suitable for the low-paraffin catalytic system is used for monitoring the molecular structure change of the catalyst surface interface and the two-phase molecular structure change of the gas-solid interface in real time when various solid catalyst particles react with a gas raw material in a high-temperature environment in the gas-solid heterogeneous catalytic reaction, and provides relevant theory and experimental guidance for the design and development of the catalyst system with high activity, high selectivity and high conversion efficiency finally through the in-situ characterization technology of a fixed bed reactor carried light path.

Description

In-situ spectrum device suitable for low-paraffin catalytic system

Technical Field

The utility model relates to the technical field of spectrum characterization devices, in particular to an in-situ spectrum device suitable for a low-paraffin catalytic system.

Background

The low alkane is used as an important byproduct in the petroleum refining industry, the saturated C-H bond is used as a nonpolar bond, the high bond energy ensures that the low alkane is not easy to crack and activate, has extremely strong chemical inertness, has limited application in the industry, needs to catalyze the low alkane to convert the low alkane into a high value-added product, and has the in-situ characterization technology as a technology for realizing real-time monitoring by combining various spectrum instruments, can directly detect the real-time dynamic changes of the microscopic morphology, crystal structure, chemical composition and other information of the catalytic material by changing experimental conditions of different reaction temperatures, different reaction atmospheres and the like, intuitively acquires the real-time evolution process of the catalytic material, and has become a front characterization technical means in the catalytic field.

In the current research, the real-time reaction process of the catalyst and the reactant under the actual working condition and the in-situ characterization process formulated for the experiment are relatively difficult, and the common practice of researchers is that a large number of experiments are carried out firstly, after the conditions of the content of each component of the catalyst, the reaction temperature, the reaction pressure and the like are changed, the optimal reaction condition is further determined, and then an in-situ detection instrument is used for observing the change process of the catalyst under the optimal reaction condition.

Disclosure of Invention

The present utility model is directed to an in situ spectroscopic apparatus suitable for use in a low paraffin catalytic system to solve the above-mentioned problems set forth in the background art.

In order to achieve the above purpose, the present utility model provides the following technical solutions: the utility model provides an in situ spectrum device suitable for low paraffin catalytic system, includes in situ fixed bed reactor, spectrum appearance, six-way valve, gas chromatograph and control display terminal, control display terminal sets up in one side of gas chromatograph, six-way valve sets up in the opposite side of gas chromatograph, the spectrum appearance sets up in the top of six-way valve, in situ fixed bed reactor swing joint is in the inside of spectrum appearance.

The in-situ fixed bed reactor comprises a heat preservation material, a heater, an electric heating wire, a high-temperature heating reaction furnace, a gas circuit sealing, a sealing flange and a gas-solid catalyst filling area, wherein the heat preservation material is arranged in the high-temperature heating reaction furnace, the heater is movably connected in the heat preservation material, the electric heating wire is movably connected in the heater, the gas-solid phase catalytic reaction quartz tube penetrates through the high-temperature heating reaction furnace, the gas circuit sealing is arranged at the top and the bottom of the gas-solid phase catalytic reaction quartz tube, the sealing flange is movably connected to the outside of the gas circuit sealing, and the gas-solid catalyst filling area is movably connected to the middle of the gas-solid phase catalytic reaction quartz tube.

Preferably, a light-in window and a light-out window are arranged in the middle of the high-temperature heating reaction furnace, and an optical path system is arranged in the window.

Preferably, the window projects a raman light source of a particular excitation light wavelength, forming a raman incident signal and a raman scattered signal.

Preferably, the raman incident signal irradiates the surface of the sample in the gas-solid catalyst filling area through the light entrance window, and the scattered low-frequency optical signal can sensitively detect the local coordination structure change caused by different coordination configurations of substances after the molecules in the catalyst absorb part of energy.

Preferably, the optical path system comprises two optical path systems, namely a scattering optical path and a transmission optical path, and is used for switching between different characterization instruments.

Preferably, the high-temperature heating reaction furnace, the heat insulation material, the heating furnace, the electric heating wire, the gas-solid phase catalytic reaction quartz tube, the gas path seal, the sealing flange and the gas-solid catalyst filling area are in linkage control through each subsystem of the device, and are used for matching with a light path system, so that macroscopic physical changes and microscopic structural changes generated in the process of automatically recording the temperature programming of catalyst bed particles in the in-situ fixed bed reactor are realized at a control terminal, and spectral data is obtained through software analysis.

Compared with the prior art, the utility model has the beneficial effects that:

1. the in-situ spectrum device suitable for the low-paraffin catalytic system is used for monitoring the molecular structure change of the catalyst surface interface and the two-phase molecular structure change of the gas-solid interface in real time when various solid catalyst particles react with a gas raw material in a high-temperature environment in the gas-solid heterogeneous catalytic reaction, and provides relevant theory and experimental guidance for the design and development of the catalyst system with high activity, high selectivity and high conversion efficiency finally through the in-situ characterization technology of a fixed bed reactor carried light path.

2. The in-situ spectrum device suitable for the low-paraffin catalytic system can build a specific light path and an in-situ test environment, is based on a brand new innovative research and development on the existing ex-situ device, can be expanded into other similar heterogeneous catalytic systems, and provides a multi-scale in-situ nondestructive testing system which can be universally suitable for heterogeneous catalytic reaction processes for fine chemical industry peers in the field.

Drawings

FIG. 1 is a general structural diagram of an in situ fixed bed reactor according to the present utility model;

FIG. 2 is a cross-sectional view of an in situ fixed bed reactor according to the present utility model;

FIG. 3 is a schematic view of the optical path of an in situ fixed bed reactor according to the present utility model;

FIG. 4 is a schematic view of a transmission-type optical path of an in-situ fixed bed reactor according to the present utility model

FIG. 5 is a schematic view of the scattering optical path of an in situ fixed bed reactor according to the present utility model;

FIG. 6 is an in situ fixed bed unit evaluation system of the present utility model.

In the figure: 1. an in situ fixed bed reactor; 2. a thermal insulation material; 301. a heater; 302. an electric heating wire; 303. heating the reaction furnace at a high temperature; 4. a gas-solid phase catalytic reaction quartz tube; 5. sealing the gas path; 6. a sealing flange; 7. a gas-solid catalyst loading zone; 8. an optical path system; 9. a light entrance window; 10. a light exit window; 11. raman incident signals; 12. raman scattering signals; 13. a spectrometer; 14. a six-way valve; 15. a gas chromatograph; 16. and controlling the display terminal.

Detailed Description

The following description of the embodiments of the present utility model will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present utility model, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the utility model without making any inventive effort, are intended to be within the scope of the utility model.

Referring to fig. 1-6, the present utility model provides a technical solution: the utility model provides an in situ spectrum device suitable for low paraffin catalytic system, includes in situ fixed bed reactor 1, spectrum appearance 13, six logical valve 14, gas chromatograph 15 and control display terminal 16, and control display terminal 16 sets up in one side of gas chromatograph 15, and six logical valve 14 sets up in the opposite side of gas chromatograph 15, and spectrum appearance 13 sets up in the top of six logical valve 14, and in situ fixed bed reactor 1 swing joint is in the inside of spectrum appearance 13.

The in-situ fixed bed reactor 1 comprises a heat preservation material 2, a heater 301, an electric heating wire 302, a high-temperature heating reaction furnace 303, a gas-solid phase catalytic reaction quartz tube 4, a gas path seal 5, a seal flange 6 and a gas-solid phase catalyst filling area 7, wherein the heat preservation material 2 is arranged in the high-temperature heating reaction furnace 303, the heater 301 is movably connected in the heat preservation material 2, the electric heating wire 302 is movably connected at the upper end and the lower end of the heater 301, the gas path seal 5 is arranged at the top of the gas-solid phase catalytic reaction quartz tube 4, the seal flange 6 is movably connected outside the gas path seal 5, the gas-solid phase catalyst filling area 7 is movably connected in the middle of the gas-solid phase catalytic reaction quartz tube 4, a light inlet window 9 and a light outlet window 10 are formed in the middle of the high-temperature heating reaction furnace 303, an optical path system 8 is arranged in the window, a Raman light source with specific excitation wavelength is projected in the window, a Raman incident signal 11 and a Raman scattering signal 12 are formed, the Raman incident signal 11 irradiates to the surface of a sample in the gas-solid phase catalyst filling area 7 through the light inlet window 9, and the molecular energy in the catalyst can be detected in the partial coordination part after the molecular energy in the high-temperature heating reaction furnace 303 is in the middle of the gas-solid phase catalytic reaction furnace, the molecular energy is detected, the molecular energy in the partial coordination part can be different from the molecular energy can be used for detecting the molecular energy in the molecular energy and the molecular energy is different in the molecular energy and the molecular material in the molecular structure.

The device comprises a high-temperature heating reaction furnace 303, a heat insulation material 2, a heater 301, an electric heating wire 302, a gas-solid phase catalytic reaction quartz tube 4, a gas circuit seal 5, a sealing flange 6 and a gas-solid catalyst filling area 7, wherein linkage control is carried out among subsystems of the device, the device is used for matching with a light path system 8, macroscopic physical change and microscopic structural change generated in the process of automatically recording the temperature programming of catalyst bed particles in the in-situ fixed bed reactor 1 at a control terminal are realized, and spectral data is obtained through software analysis.

When the device is used, the device and the spectrometer 13 are reasonably fixed in position, the normal passing of an optical path is ensured, then a sample is filled, quartz cotton is put into the gas-solid phase catalytic reaction quartz tube 4, after the quartz cotton is fixed in a preset position, catalyst particles are filled in the gas-solid catalyst filling area 7, the temperature raising program of the in-situ fixed bed reactor 1 is set, the heating is carried out through the high-temperature heating reaction furnace 303, the catalytic reaction is started, and at the moment, a spectrogram signal monitored by the optical path through the surface of the sample particles is displayed in real time at the control display terminal 16.

Although embodiments of the present utility model have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the utility model, the scope of which is defined in the appended claims and their equivalents.

Claims

1. An in-situ spectroscopic device suitable for a low paraffin catalytic system, comprising an in-situ fixed bed reactor (1), a spectrometer (13), a six-way valve (14), a gas chromatograph (15) and a control display terminal (16), and being characterized in that: the control display terminal (16) is arranged on one side of the gas chromatograph (15), the six-way valve (14) is arranged on the other side of the gas chromatograph (15), the spectrometer (13) is arranged above the six-way valve (14), and the in-situ fixed bed reactor (1) is movably connected inside the spectrometer (13);

the in-situ fixed bed reactor (1) comprises a heat preservation material (2), a heater (301), an electric heating wire (302), a high-temperature heating reaction furnace (303), a gas-solid phase catalytic reaction quartz tube (4), a gas circuit seal (5), a sealing flange (6) and a gas-solid catalyst filling area (7), wherein the heat preservation material (2) is arranged in the high-temperature heating reaction furnace (303), the heater (301) is movably connected in the heat preservation material (2), the electric heating wire (302) is movably connected in the heater (301), the gas-solid phase catalytic reaction quartz tube (4) penetrates through the high-temperature heating reaction furnace (303), the gas circuit seal (5) is arranged at the top and the bottom of the gas-solid phase catalytic reaction quartz tube (4), the sealing flange (6) is movably connected in the outer part of the gas circuit seal (5), and the gas-solid catalyst filling area (7) is movably connected in the middle of the gas-solid phase catalytic reaction quartz tube (4).

2. An in situ spectroscopic device suitable for use in a low paraffin catalytic system as claimed in claim 1, wherein: the middle part of the high-temperature heating reaction furnace (303) is provided with a light-in window (9) and a light-out window (10), and an optical path system (8) is arranged in the window.

3. An in situ spectroscopic device suitable for use in a low paraffin catalytic system according to claim 2, characterized in that: the window projects a raman light source of a specific excitation light wavelength forming a raman incident signal (11) and a raman scattering signal (12).

4. An in situ spectroscopic device suitable for use in a low paraffin catalytic system as claimed in claim 3, wherein: the Raman incident signal (11) irradiates the sample surface of the gas-solid catalyst loading area (7) through the light entrance window (9).

5. An in situ spectroscopic device suitable for use in a low paraffin catalytic system according to claim 2, characterized in that: the optical path system (8) comprises two optical path systems, namely a scattering optical path and a transmission optical path.

6. An in situ spectroscopic device suitable for use in a low paraffin catalytic system as claimed in claim 1, wherein: the high-temperature heating reaction furnace (303), a heat insulation material (2), a heater (301), an electric heating wire (302), a gas-solid phase catalytic reaction quartz tube (4), a gas circuit seal (5), a seal flange (6) and a gas-solid catalyst filling area (7) are in linkage control through each subsystem of the device and are used for being matched with a light path system (8).