Neutron scattering high-temperature sample environment and gas control device

Abstract

The utility model belongs to the technical field of neutron scattering catalysis, and particularly relates to a neutron scattering high-temperature sample environment and gas control device. Comprising a gas control device, a pressurization control device, a high-temperature and high-pressure reactor and a tail gas treatment device, wherein the gas control device is sequentially connected with the pressurization device, the high-temperature and high-pressure reactor and the tail gas treatment device through pipelines in the gas flowing direction; the neutron scattering high-temperature and high-pressure sample environment and gas control device is comprehensive in function, flexible to operate, safe and reliable, and provides powerful tool support for research of an in-situ catalytic system.

Description

Technical Field

[0001] The present invention belongs to the technical field of neutron scattering catalysis, and particularly relates to a neutron scattering high-temperature sample environment and gas control device. Background Art

[0002] In-situ catalytic characterization technology is an important means to deeply explore the structure-activity relationship of catalysts. It provides a powerful tool for revealing the principle of catalytic action by real-time monitoring of the structural and performance changes of catalysts during the catalytic reaction process. Neutron scattering technology, due to its high sensitivity to light elements (such as carbon, hydrogen, oxygen, etc.), has been widely used in the study of catalytic reaction mechanisms. This technology can effectively detect the dynamic evolution of key reactive intermediates and active sites during the in-situ catalytic reaction process, thereby deepening our understanding of the catalytic process.

[0003] In the field of catalytic research, in-situ characterization of catalytic reactions under high temperature and high pressure conditions is particularly important. For example, industrial catalytic processes such as ammonia synthesis, carbon dioxide hydrogenation, and Fischer-Tropsch synthesis are often carried out under extreme conditions. The evolution of key reactive intermediates and sites in these processes has a decisive impact on the performance and reaction efficiency of catalysts. Therefore, the development of a neutron scattering sample environment system that can work stably under high temperature and high pressure conditions has become an urgent need.

[0004] The sample environment system is a key component for realizing the application of neutron scattering technology in the in-situ catalytic system, and generally includes two major parts: a sample environment device and a gas control device. Although the existing sample environment systems can simulate catalytic reaction conditions to a certain extent, there are still many deficiencies, especially in terms of stability and control accuracy under high temperature and high pressure conditions. In addition, the catalytic efficiency of existing catalysts is generally low, resulting in a long experimental cycle and high cost, which seriously affects the scientific research efficiency and the popularization of industrial applications. Summary of the Invention

[0005] In order to solve the above problems, the present utility model provides a brand-new neutron scattering high-temperature sample environment and gas control device, aiming to improve the research efficiency and accuracy of the in-situ catalytic system and promote the development of catalytic science.

[0006] The technical solution adopted by the present invention is: a neutron scattering high-temperature sample environment and gas control device, including a gas control device, a pressurizing device, a high-temperature and high-pressure reactor, and a tail gas treatment device, wherein the gas control device is connected to the pressurizing device, the high-temperature and high-pressure reactor, and the tail gas treatment device in sequence through pipelines along the gas flow direction.

[0007] The described gas control device includes a gas cylinder, a pressure reducing valve, a first screw valve, a first three-way valve, a gas purifier, multiple one-way valves, a safety valve with a pressure sensor, a gas mass flow controller, and a second screw valve. When using multiple gases, multiple gas paths can be connected in parallel in front of the second one-way valve.

[0008] The described pressurization device includes an atmospheric pressure mixed gas storage tank, a safety valve with a pressure sensor, a booster pump, and a high-pressure gas mixing tank to maintain the dynamic balance of the supplied gas.

[0009] The described high-temperature and high-pressure reactor includes a heating wire, a sealing cover, a heating assembly, a sample cell, an aviation connector, a temperature probe, a vacuum pumping port, a pressure-bearing housing, a product outlet, and an inlet.

[0010] The described pressure-bearing housing is the main housing of the high-temperature and high-pressure sample environment device. Its internal cavity is evacuated and is equipped with an aviation connector, a temperature probe, a vacuum pumping port, a pressure-bearing housing, a product outlet, and an inlet, as well as connecting pipes for connecting various components.

[0011] The described sample cell is used to place the catalyst required for the reaction. The sealing cover is used to seal the sample cell. The heating assembly is used to heat the reactor. The heating wire is installed outside the connecting pipe and is used to preheat the reaction gas and heat the generated product.

[0012] The tail gas treatment device includes a filter, a buffer tank, a pressure reducing valve, a gas flow controller, and a product absorption pool. The product absorption pool is connected to the outlet end of the high-temperature and high-pressure sample environment device.

[0013] The described heating assembly is installed at the upper and lower ends of the sample cell. The heating wire is installed outside the connecting pipe, and the circuit is connected to the external control system through the aviation connector.

[0014] The components inside the described device are connected through pipes and adapters for the transportation of high-pressure reaction gases and products.

[0015] During the operation of the described device, the gases participating in the reaction and the purging gas are proportioned in the gas control device according to the set ratio and adjusted to an atmospheric pressure mixed gas, and then pressurized to the high-pressure mixed gas required for the reaction. The products generated after the high-temperature and high-pressure reaction are treated by the tail gas treatment device.

[0016] The beneficial effects of the present invention are as follows: The present invention provides a neutron scattering high-temperature sample environment and gas control device with comprehensive functions, flexible operation, safety and reliability, which provides strong tool support for the research of in-situ catalytic systems. Through the precise proportioning and flow control of the gas control device, the present invention can achieve flexible mixing and precise control of various gases to meet the requirements of different catalytic reactions; the safety valve and pressure sensor in the pressurizing device ensure the safe operation of the system under high-pressure conditions. At the same time, the design of the high-pressure gas mixing tank makes the gas supply more stable and reliable; the efficient heating system and precise temperature control of the high-temperature and high-pressure reactor enable the catalytic reaction to proceed efficiently at the set temperature and pressure, improving the repeatability and accuracy of the experiment; the design of the tail gas treatment device effectively reduces the emission of harmful gases, meeting the environmental protection requirements. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1 It is a schematic structural principle diagram of the present invention applied to the research of in-situ catalytic systems;

[0018] Figure 2 It is a detailed design diagram of the gas control device in the present invention;

[0019] Figure 3 It is a detailed design diagram of the pressurizing device in the present invention;

[0020] Figure 4 It is a three-dimensional structural schematic diagram of the high-temperature and high-pressure sample environment device disclosed in the embodiment of the present invention;

[0021] Figure 5 The top view structural schematic diagram of the embodiment of the present invention;

[0022] Figure 6 It is a cross-sectional structural schematic diagram of the embodiment of the present invention;

[0023] Figure 7 It is a structural design schematic diagram of the tail gas treatment device in the present invention. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0024] The present invention provides a neutron scattering high-temperature sample environment and gas control device, which is particularly suitable for the study of in-situ catalytic systems. The device includes a gas control device 1, a pressurizing device 2, a high-temperature and high-pressure reactor 3, and an exhaust gas treatment device 4. The gas control device 1 is connected to the pressurizing device 2, the high-temperature and high-pressure reactor 3, and the exhaust gas treatment device 4 in sequence through pipelines along the gas flow direction. The gas control device 1 includes a gas cylinder 5, a pressure reducing valve 6, a first screw valve 7, a first three-way valve 8, a gas purifier 9, multiple one-way valves 10, 13, a safety valve 11 with a pressure sensor, a gas mass flow controller 12, and a second screw valve 14. When using multiple gases, multiple gas paths can be connected in parallel in front of the second one-way valve 13. The pressurizing device 2 includes an atmospheric pressure mixed gas storage tank 15, safety valves 16, 18 with pressure sensors, a booster pump 17, and a high-pressure gas mixing tank 19 to maintain the dynamic balance of the supplied gas. The high-temperature and high-pressure reactor 3 includes a heating wire 23, a sealing cover 24, a heating assembly 25, a sample cell 26, an aviation connector 27, a temperature probe 28, a vacuum pumping port 29, a pressure-bearing housing 30, a product outlet 31, and an air inlet 32. The pressure-bearing housing 30 is the main housing of the high-temperature and high-pressure sample environment device, with a vacuum chamber inside, equipped with an aviation connector 27, a temperature probe 28, a vacuum pumping port 29, a pressure-bearing housing 30, a product outlet 31, and an air inlet 32, as well as connecting pipelines for connecting various components. The sample cell 26 is used to place the catalyst required for the reaction, the sealing cover 24 is used for sealing the sample cell, the heating assembly 25 is used for heating the reactor, and the heating wire 23 is installed outside the connecting pipeline for preheating the reaction gas and heating the generated product. The exhaust gas treatment device 4 includes a filter 33, a buffer tank 34, a pressure reducing valve 35, a gas flow controller 36, and a product absorption pool 37. The product absorption pool is connected to the outlet end of the high-temperature and high-pressure sample environment device. The heating assembly 25 is installed at the upper and lower ends of the sample cell 26, the heating wire 23 is installed outside the connecting pipeline, and the circuit is connected to the external control system through the aviation connector 27. Each component inside the neutron scattering high-temperature sample environment and gas control device is connected through pipelines and adapters for the transportation of high-pressure reaction gases and products. During the operation of the neutron scattering high-temperature sample environment and gas control device, the gases participating in the reaction and the purging gas are mixed in the gas control device 1 in a set ratio to form an atmospheric pressure mixed gas, and then pressurized to the high-pressure mixed gas required for the reaction. The products generated after the high-temperature and high-pressure reaction are treated by the exhaust gas treatment device 4.

[0025] In this embodiment, the gas control device 1 is the gas source and proportioning unit of the whole system. It includes a plurality of gas cylinders, and a pressure reducing valve is equipped at the outlet of each gas cylinder to reduce the high-pressure gas to atmospheric pressure. Subsequently, the gas enters the gas purifier through the first screw valve and the first three-way valve for purification to ensure the purity of the reaction gas. The purified gas then passes through the one-way valve and the safety valve with a pressure sensor and enters the gas mass flow controller for precise flow control. When multiple gases are needed, it can be achieved by paralleling multiple gas passages in front of the second one-way valve. These passages all include components such as the above-mentioned pressure reduction, purification, and flow control. Finally, the mixed atmospheric-pressure gas enters the pressurization device.

[0026] In this embodiment, the main function of the pressurization device is to pressurize the atmospheric-pressure mixed gas to the high-pressure state required for the reaction. The atmospheric-pressure mixed gas first enters the atmospheric-pressure mixed gas storage tank and then is pressurized to the required pressure by the booster pump. During the pressurization process, the safety valve with a pressure sensor ensures the safe operation of the system. The pressurized high-pressure mixed gas is stored in the high-pressure gas mixing tank for subsequent reaction use.

[0027] In this embodiment, the high-temperature and high-pressure reactor is the core part of the present invention, in which heating wires and heating components are installed for heating the reactor and the connecting pipelines. The sample tank is used to place the catalyst and is sealed by a sealing cover. The heating components and the heating wires work together to heat the reactor to the required temperature. At the same time, the temperature probe monitors the reaction temperature in real time to ensure the precise progress of the reaction. The pressure-bearing housing is the main structure of the reactor and can withstand the high-temperature and high-pressure environment. The reaction product is discharged through the product outlet and enters the tail gas treatment device.

[0028] In this embodiment, the tail gas treatment device filters, buffers, and reduces the pressure of the reaction gas. The filter removes impurity particles in the gas, the buffer tank stabilizes the gas pressure, the pressure reducing valve reduces the high-pressure gas to atmospheric pressure, and finally the gas flow controller controls the tail gas emission rate. The treated tail gas finally enters the product absorption pool for absorption treatment.

Claims

1. A neutron scattering high temperature sample environment and gas control device, characterized in that: The invention comprises a gas control device (1), a pressure boosting device (2), a high-temperature and high-pressure reactor (3) and an exhaust gas treatment device (4), wherein the gas control device (1) is connected to the pressure boosting device (2), the high-temperature and high-pressure reactor (3) and the exhaust gas treatment device (4) in sequence via pipelines along the gas flow direction.

2. The neutron scattering high temperature sample environment and gas control device according to claim 1, characterized in that: The gas control device (1) comprises a gas cylinder (5), a pressure reducing valve (6), a first rotary valve (7), a first three-way valve (8), a gas purifier (9), a plurality of one-way valves (10, 13), a safety valve (11) with a pressure sensor, a gas mass flow controller (12) and a second rotary valve (14). When multiple gas channels are used, a plurality of gas channels can be connected in parallel at the front end of the second one-way valve (13).

3. The neutron scattering high temperature sample environment and gas control device according to claim 1, characterized in that: The boosting device (2) comprises a normal pressure mixed gas storage tank (15), a safety valve (16, 18) with a pressure sensor, a boosting pump (17) and a high pressure gas mixing tank (19) to maintain a dynamic balance of the supplied gas.

4. The neutron scattering high temperature sample environment and gas control device according to claim 1, characterized in that: The high temperature and high pressure reactor (3) comprises a heating wire (23), a sealing cover (24), a heating assembly (25), a sample slot (26), an aviation joint (27), a temperature probe (28), a vacuum pumping port (29), a pressure-bearing shell (30), a product outlet (31) and an air inlet (32).

5. The neutron scattering high temperature sample environment and gas control device according to claim 4, characterized in that: The pressure-bearing shell (30) is the main shell of the high-temperature and high-pressure sample environment device, and has a vacuum chamber inside, equipped with an aviation joint (27), a temperature probe (28), a vacuum exhaust port (29), a pressure-bearing shell (30), a product outlet (31) and an air inlet (32), as well as connecting pipes connecting various components.

6. The neutron scattering high temperature sample environment and gas control device according to claim 5, characterized in that: The sample slot (26) is used to place the catalyst required for the reaction, the sealing cover (24) is used to seal the sample slot, the heating component (25) is used to heat the reactor, and the heating wire (23) is installed on the outside of the connecting pipeline to preheat the reaction gas and heat the generated product.

7. The neutron scattering high temperature sample environment and gas control device according to claim 1, characterized in that: The tail gas treatment device (4) comprises a filter (33), a buffer tank (34), a pressure reducing valve (35), a gas flow controller (36) and a product absorption pool (37), and the product absorption pool is connected to the outlet end of the high-temperature and high-pressure sample environment device.

8. The neutron scattering high temperature sample environment and gas control device according to claim 6, characterized in that: The heating assembly (25) is installed at the upper and lower ends of the sample tank (26), the heating wire (23) is installed outside the connecting pipeline, and the circuit is connected to the external control system through the aviation connector (27).

9. The neutron scattering high temperature sample environment and gas control device according to any one of claims 1 to 8, characterized in that: The various components inside the device are connected by pipelines and adapters for conveying high-pressure reaction gas and products.

10. The neutron scattering high temperature sample environment and gas control device according to any one of claims 1 to 8, characterized in that: During operation of the device, the gas involved in the reaction and the purge gas are adjusted to a normal pressure mixed gas in a gas control device (1) according to a set ratio, and then pressurized to a high pressure mixed gas required for the reaction. The product generated after the high temperature and high pressure reaction is treated by the tail gas treatment device (4).

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