High-temperature and high-pressure sample environment device and gas-liquid control device

Abstract

The utility model relates to the technical field of neutron scattering experimental equipment, in particular to a high-temperature and high-pressure sample environment device and a gas-liquid control device which are applied to an in-situ catalysis system of a neutron scattering technology. Comprising a gas cylinder, the gas cylinder is sequentially connected with a pressure reducing valve, a first screwing valve, a ball valve, a gas purifier, a first check valve, a first pressure sensor, a mass flow controller, a second check valve, a second screwing valve, a second pressure sensor and a three-way valve through pipelines, the lower surface of the three-way valve is connected with a bubbling tank, and the three-way valve is further connected with a reactor. One end of the reactor is connected with a liquid tank through an infusion pump; according to the invention, accurate control of experimental conditions is facilitated, in-situ catalysis research is realized, experimental efficiency and accuracy are improved, research in the fields of new materials and new energy is promoted, and the design of a tail gas treatment and collection device not only protects the environment, but also ensures the safety of the experimental process. Meanwhile, an accurate gas-liquid control system is also beneficial to reducing waste and pollution in the experiment process.

Description

Technical Field

[0001] The invention relates to the technical field of neutron scattering experimental equipment, in particular to a high-temperature and high-pressure sample environment device and a gas-liquid control device applied to neutron scattering technology in an in-situ catalytic system. Background Art

[0002] Neutron scattering technology, with its unique properties, namely its high sensitivity to light elements (such as carbon, hydrogen, oxygen, etc.), has become an important means to deeply study the microstructure and dynamics of matter. Especially in the field of catalytic science, this technology can detect key reactive intermediates and key active sites of reactions that are difficult to capture by conventional photoelectric methods, thus providing us with a powerful tool to reveal the structure-activity relationship of catalysts; however, to give full play to the advantages of neutron scattering technology in the study of catalytic systems, a stable and efficient sample environment system is essential. Such a system needs to be able to work stably under high temperature conditions and provide precise gas-liquid control to ensure that the catalytic reaction can be carried out in a simulated actual working environment.

[0003] Although the existing sample environment system can meet the needs of neutron scattering experiments to a certain extent, it still has many shortcomings under high temperature conditions, especially in complex environments involving gas and liquid supply. For example, the gas and liquid control accuracy in high temperature environments is not high, the stability is poor, and the system's tolerance to high temperature and corrosive gas and liquid is insufficient. Therefore, for the application of neutron scattering technology in in-situ catalytic systems, it is particularly important to design a dedicated high-temperature and high-pressure sample environment device and gas-liquid control device. Such a device can not only improve the accuracy and repeatability of the experiment, but also help us to have a deeper understanding of the catalytic reaction mechanism, thereby promoting the development of catalytic science. Summary of the invention

[0004] In neutron scattering experiments, in-situ observation of the structure and dynamic behavior of matter under high temperature, high pressure, and gas-liquid-solid multiphase reaction conditions is an important field of scientific research. Existing experimental equipment often cannot meet the needs of in-situ observation under complex reaction conditions. This paper aims to provide a neutron scattering experimental equipment, a high-temperature and high-pressure sample environment device and a gas-liquid control device that can meet the needs of high temperature and gas-liquid control.

[0005] The technical scheme adopted by the present invention is: a high-temperature and high-pressure sample environment device and a gas-liquid control device, which are applied to the neutron scattering technology in the in-situ catalytic system, and include a gas cylinder, which is sequentially connected to a pressure reducing valve, a first rotary valve, a ball valve, a gas purifier, a first check valve, a first pressure sensor, a mass flow controller, a second check valve, a second rotary valve, a second pressure sensor, and a three-way valve through a pipeline, wherein the lower surface of the three-way valve is connected to a bubbling tank, and the three-way valve is also connected to a reactor, one end of the reactor is connected to a liquid tank through an infusion pump, and the lower surface of the reactor is connected to a catalytic reactor.

[0006] The three-way valve is provided with a liquid interface and a gas interface, which are used to connect the liquid pipeline and the gas pipeline respectively.

[0007] The lower surface of the gas interface is connected to a quartz sample rod, a sealing cover is provided in the middle of the outer surface of the quartz sample rod, and the lower surface of the sealing cover is connected to a quartz protection tube.

[0008] The upper surface of the sealing cover is provided with a temperature probe for measuring the reaction temperature.

[0009] The top of the outer surface of the quartz sample rod is connected with a three-way connector, the three-way connector is connected to the mixed gas through the gas pipe, and the mixed gas is connected to the tail gas treatment and collection device through one side of the gas pipe.

[0010] The three-way valve can control the gas flow direction by adjusting the valve knob, so that the gas flows through the bubbling tank to input the liquid into the reactor in the form of bubbles, or the gas is directly input into the reactor.

[0011] The infusion pump can pump the liquid in the liquid tank into the reactor when the gas is directly input into the reactor.

[0012] The connection modes among the gas cylinder, the pressure reducing valve, the first rotary valve, the ball valve, the gas purifier, the first check valve, the first pressure sensor, the mass flow controller, the second check valve, the second rotary valve and the second pressure sensor are all fixed connections.

[0013] The connection mode between the gas interface and the quartz sample rod is a fixed connection, and the connection mode between the sealing cover and the quartz protection tube is a fixed connection.

[0014] The beneficial effects of the present invention are: a high-temperature and high-pressure sample environment and gas-liquid control device is applied to the in-situ catalytic system of neutron scattering technology, including gas cylinders, pressure reducing valves, multiple valves, sensors, gas purifiers, mass flow controllers, bubbling tanks, reactors, catalytic reactors, infusion pumps and liquid tanks. These components are connected in sequence through pipelines to form a complete gas-liquid control system; the beneficial effects are mainly reflected in the following aspects:

[0015] Helps to accurately control experimental conditions: This technical solution provides precise experimental conditions for catalytic reactions through precise gas flow control, liquid quantitative delivery, and real-time temperature and pressure monitoring. This helps scientists to more accurately explore the mechanism and influencing factors of catalytic reactions.

[0016] Realize in-situ catalytic research: Using neutron scattering technology to conduct in-situ catalytic research can observe the structural changes and kinetic behavior during the reaction in real time. This technical solution makes in-situ catalytic research possible through specially designed high-temperature and high-pressure sample environment devices and gas-liquid control devices, providing a powerful tool for the development of catalytic science.

[0017] Improve experimental efficiency and accuracy: The automated gas-liquid control system reduces errors caused by human operation and improves the efficiency and accuracy of the experiment. At the same time, the design of the high-temperature sample environment device also ensures that the experimental samples can be tested in an environment close to the actual working conditions, thereby more realistically reflecting the process of the catalytic reaction.

[0018] Promote research in the field of new materials and new energy: Catalytic reaction is an important research direction in the field of new materials and new energy. This technical solution provides an advanced experimental platform and means for research in these fields, which helps to accelerate the research and development of new materials and new energy.

[0019] Environmentally friendly and safe: The design of the exhaust gas treatment and collection device not only protects the environment, but also ensures the safety of the experimental process. At the same time, the precise gas and liquid control system also helps to reduce waste and pollution during the experiment. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] Figure 1 A schematic diagram of the structural principle of the present invention in which the neutron scattering technology is applied in an in-situ catalytic system;

[0021] Figure 2 This is a schematic diagram of the main structure of the high temperature and high pressure sample environment device of the present invention;

[0022] Figure 3 It is a schematic diagram of the top view of the high temperature and high pressure sample environment device in the present invention;

[0023] Figure 4 It is a right side structural schematic diagram of the high temperature and high pressure sample environment device in the present invention;

[0024] Figure 5 It is a schematic diagram of the planed structure of the high temperature and high pressure sample environment device in the present invention;

[0025] Figure 6 It is a schematic diagram of the sealing cover structure in the present invention.

[0026] Explanation of the reference numerals: 1. gas cylinder; 2. pressure reducing valve; 3. first rotary valve; 4. ball valve; 5. gas purifier; 6. first check valve; 7. first pressure sensor; 8. mass flow controller; 9. second check valve; 10. second rotary valve; 11. second pressure sensor; 12. three-way valve; 13. bubbling tank; 14. liquid tank; 15. infusion pump; 16. reactor; 17. catalytic reactor; 18. exhaust gas treatment and collection device; 19. temperature probe; 20. liquid interface; 21. gas interface; 22. quartz sample rod; 23. mixed gas through gas pipe; 24. three-way connector; 25. sealing cover; 26. quartz protective tube. DETAILED DESCRIPTION

[0027] The present invention provides a high temperature and high pressure sample environment device and a gas-liquid control device in an in-situ catalytic system applied to neutron scattering technology, which has a unique structure and flexible operation, and can realize in-situ neutron scattering experiments on gas-liquid-solid reactions, so as to deeply explore the mechanism of catalytic reactions. The following is a specific embodiment of the present invention.

[0028] like Figure 1-6As shown, a high-temperature and high-pressure sample environment device and a gas-liquid control device are used in an in-situ catalytic system of neutron scattering technology, comprising a gas cylinder 1, the gas cylinder 1 is connected to a pressure reducing valve 2, a first rotary valve 3, a ball valve 4, a gas purifier 5, a first check valve 6, a first pressure sensor 7, a mass flow controller 8, a second check valve 9, a second rotary valve 10, a second pressure sensor 11, and a three-way valve 12 in sequence through a pipeline, the lower surface of the three-way valve 12 is connected to a bubbling tank 13, the three-way valve 12 is also connected to a reactor 16, one end of the reactor 16 is connected to a liquid tank 14 through an infusion pump 15, and the lower surface of the reactor 16 is connected to a catalytic reactor 17; the three-way valve 12 is provided with a liquid interface 20 and a gas interface 21, which are respectively used to connect a liquid pipeline and a gas pipeline; the lower surface of the gas interface 21 is connected to a quartz sample rod 22, the middle part of the outer surface of the quartz sample rod 22 is provided with a sealing cover 25, and the lower surface of the sealing cover 25 is connected to a quartz protection tube 26; the upper surface of the sealing cover 25 is provided with a temperature probe 19 for measuring reaction temperature; the top of the outer surface of the quartz sample rod 22 is connected with a three-way connector 24, the three-way connector 24 is connected to the mixed gas through the gas pipe 23, and the mixed gas is connected to the tail gas treatment and collection device 18 through one side of the gas pipe 23; the three-way valve 12 can control the gas flow direction by adjusting the valve knob, so that the gas flows through the bubbling tank 13 to input the liquid into the reactor 16 in the form of bubbles, or the gas is directly input into the reactor 16; the infusion pump 15 can pump the liquid in the liquid tank 14 into the reactor 16 when the gas is directly input into the reactor 16; the connection between the gas cylinder 1, the pressure reducing valve 2, the first rotary valve 3, the ball valve 4, the gas purifier 5, the first check valve 6, the first pressure sensor 7, the mass flow controller 8, the second check valve 9, the second rotary valve 10, and the second pressure sensor 11 are all fixedly connected; the connection between the gas interface 21 and the quartz sample rod 22 is fixedly connected, and the connection between the sealing cover 25 and the quartz protection tube 26 is fixedly connected.

[0029] With respect to the device structure and connection in the present invention, especially the gas cylinder and the gas purification system, the present invention first provides the gas required for the reaction through the gas cylinder 1. The upper surface of the gas cylinder 1 is fixedly connected to a pressure reducing valve 2 through a pipeline for adjusting the pressure of the gas. The outer surface of the pressure reducing valve 2 is fixedly connected to a first rotary valve 3 for manually controlling the flow of the gas. The outer surface of the first rotary valve 3 is further fixedly connected to a ball valve 4 to further enhance the control ability of the gas flow. The gas then enters the gas purifier 5 through the ball valve 4 to purify the gas to ensure the purity of the reaction gas.

[0030] Regarding pressure sensing and flow control, the outer surface of the gas purifier 5 in the present invention is fixedly connected to a first check valve 6 to prevent gas backflow. The outer surface of the first check valve 6 is fixedly connected to a first pressure sensor 7 for real-time monitoring of the gas pressure. The gas then passes through a mass flow controller 8, which can accurately control the flow of the gas. The outer surface of the mass flow controller 8 is fixedly connected to a second check valve 9 and a second rotary valve 10 to further enhance the control of the gas. The second pressure sensor 11 is connected to the outer surface of the second rotary valve 10 to monitor the gas pressure there.

[0031] Regarding the three-way valve and reactor system, the outer surface of the second pressure sensor 11 is fixedly connected to a three-way valve 12, which is one of the core components of the present invention. The three-way valve 12 has multiple connection ports, and a bubbling tank 13 is fixedly connected to its lower surface, so that the gas can bring the liquid into the reactor in the form of bubbling. At the same time, the outer surface of the three-way valve 12 is also fixedly connected to a reactor 16, which is the main place for gas-liquid-solid reaction.

[0032] One end of the reactor 16 is connected to the liquid tank 14 via an infusion pump 15, and the infusion pump 15 can quantitatively transport the liquid in the liquid tank 14 to the reactor 16. The lower surface of the reactor 16 is also fixedly connected to a catalytic reactor 17, which contains a catalyst for promoting gas-liquid-solid reaction.

[0033] Regarding tail gas treatment and collection, in this embodiment, the top of the outer surface of the quartz sample rod 22 is connected with a three-way connector 24, and the three-way connector 24 is connected to the tail gas treatment and collection device 18 through the mixed gas through the gas pipe 23. In this way, the reaction product can be transported to the tail gas treatment and collection device 18 through the mixed gas through the gas pipe 23 for treatment and collection.

[0034] The working principle of the present invention is as follows: first, open the gas cylinder 1 and allow the gas to pass through the above-mentioned components in sequence. The gas can be directly delivered to the quartz sample rod 22 of the reactor through the three-way valve 12, or the liquid can be delivered to the quartz sample rod 22 of the reactor through the bubbling tank 13 in the form of bubbles. At the same time, the liquid in the liquid tank 14 can be quantitatively delivered to the reactor 16 through the infusion pump 15 to achieve a quantitative reaction of gas, liquid and solid. During the reaction process, the reaction temperature can be monitored in real time by the temperature probe 19, the gas pressure can be monitored in real time by the pressure sensor, and the gas flow rate can be accurately controlled by the mass flow controller 8. The product after the reaction is treated and collected by the tail gas treatment and collection device 18. The present invention provides strong support for the application of neutron scattering technology in in-situ catalytic systems through precise gas-liquid control and the design of high-temperature sample environment devices, which helps to deeply explore the mechanism and dynamic process of catalytic reactions.

[0035] Among them, gas cylinders are used to store reaction gases, pressure reducing valves are used to adjust gas pressure, multiple valves are used to control the flow direction and flow of gases, sensors are used to monitor parameters such as pressure and temperature during the reaction process, gas purifiers are used to purify gases, mass flow controllers are used to accurately control the flow of gases, bubbling tanks are used to input liquids into reactors in the form of bubbles, reactors are the main place for gas-liquid-solid reactions, catalytic reactors are filled with catalysts, infusion pumps are used to quantitatively transport liquids in liquid tanks into reactors, and liquid tanks are used to store reaction liquids.

[0036] The invention is characterized in that, by precisely controlling the flow direction, flow rate and pressure of the gas and the quantitative delivery of the liquid, an in-situ neutron scattering experiment of a high-temperature gas-liquid-solid reaction is realized. At the same time, the device also has an exhaust gas treatment and collection device, which can collect and process the gas after the reaction.

[0037] In addition, the present invention also has components such as a temperature probe and a sealing cover for measuring the reaction temperature and ensuring the sealing of the reaction. The design of these components enables the present invention to meet the in-situ observation requirements under high temperature, high pressure, gas-liquid-solid multiphase reaction conditions.

[0038] By using the device of the present invention, it is possible to explore the evolution of key active intermediates and key active sites, and achieve the goal of building catalysts at the atomic level and understanding the mechanism and dynamics of catalytic reactions at the molecular level.

Claims

1. A high temperature and high pressure sample environment device and a gas-liquid control device, characterized in that: The invention is applied to an in-situ catalytic system of neutron scattering technology, comprising a gas cylinder (1), wherein the gas cylinder (1) is connected to a pressure reducing valve (2), a first rotary valve (3), a ball valve (4), a gas purifier (5), a first check valve (6), a first pressure sensor (7), a mass flow controller (8), a second check valve (9), a second rotary valve (10), a second pressure sensor (11), and a three-way valve (12) in sequence through pipelines; the lower surface of the three-way valve (12) is connected to a bubbling tank (13); the three-way valve (12) is also connected to a reactor (16); one end of the reactor (16) is connected to a liquid tank (14) through an infusion pump (15); and the lower surface of the reactor (16) is connected to a catalytic reactor (17).

2. A high temperature and high pressure sample environment device and a gas-liquid control device according to claim 1, characterized in that: The three-way valve (12) is provided with a liquid interface (20) and a gas interface (21), which are used to connect the liquid pipeline and the gas pipeline respectively.

3. A high temperature and high pressure sample environment device and a gas-liquid control device according to claim 1, characterized in that: The lower surface of the gas interface (21) is connected to a quartz sample rod (22), a sealing cover (25) is provided in the middle of the outer surface of the quartz sample rod (22), and the lower surface of the sealing cover (25) is connected to a quartz protection tube (26).

4. A high temperature and high pressure sample environment device and a gas-liquid control device according to claim 3, characterized in that: The upper surface of the sealing cover (25) is provided with a temperature probe (19) for measuring the reaction temperature.

5. A high temperature and high pressure sample environment device and a gas-liquid control device according to claim 3, characterized in that: The top of the outer surface of the quartz sample rod (22) is connected to a three-way connector (24), the three-way connector (24) is connected to the mixed gas through the gas pipe (23), and the mixed gas is connected to the tail gas treatment and collection device (18) through one side of the gas pipe (23).

6. A high temperature and high pressure sample environment device and a gas-liquid control device according to claim 1, characterized in that: The three-way valve (12) can control the gas flow direction by adjusting the valve knob, so that the gas flows through the bubbling tank (13) to input the liquid into the reactor (16) in the form of bubbles, or the gas is directly input into the reactor (16).

7. A high temperature and high pressure sample environment device and a gas-liquid control device according to claim 1, characterized in that: The infusion pump (15) is capable of pumping the liquid in the liquid tank (14) into the reactor (16) when the gas is directly input into the reactor (16).

8. The high temperature and high pressure sample environment device and gas-liquid control device according to claim 1, characterized in that: The connection between the gas cylinder (1), the pressure reducing valve (2), the first rotary valve (3), the ball valve (4), the gas purifier (5), the first check valve (6), the first pressure sensor (7), the mass flow controller (8), the second check valve (9), the second rotary valve (10), and the second pressure sensor (11) is fixedly connected.

9. A high temperature and high pressure sample environment device and a gas-liquid control device according to claim 2, characterized in that: The connection between the gas interface (21) and the quartz sample rod (22) is a fixed connection, and the connection between the sealing cover (25) and the quartz protection tube (26) is a fixed connection.

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