Sampling device for gas-solid reaction

Abstract

The invention relates to the field of reaction detection equipment, and particularly discloses a sampling device for gas-solid reaction, which is characterized in that a gas cylinder is connected to a solid particle generator through a first gas inlet pipe; the solid particle generator is connected to an inlet of the vertical tube furnace reactor through a second gas inlet pipe; an outlet of the vertical tubular furnace reactor is connected to a first inlet of the three-way valve through a sampling pipe and is connected to a second inlet of the three-way valve through a gas outlet pipe; the pipeline connector is provided with a copper mesh micro-grid for sampling; and the other end of the exhaust pipe is connected to the vacuum pump. Reactants are generated through the solid particle generator, the reactants are collected and sampled through the copper mesh micro-grid after reacting in the vertical tubular furnace reactor, solid particles in the reaction process can be obtained in real time without changing front and back flow state reaction environment atmospheres, accurate characterization measurement of microscopic characteristic evolution of the solid particles in different flow state reaction environment atmospheres is achieved, and the measurement accuracy is high. And the defect of measuring the kinetic parameters of the fluidization microcosmic gas-solid reaction in the prior art is overcome.

Description

Technical Field

[0001] The present invention relates to the field of reaction detection equipment, and particularly to a sampling device for gas-solid reactions. Background Art

[0002] There are a large number of gas-solid reactions in process engineering fields such as energy power and material chemical engineering. After using a solid particle generator, in-depth detection of its dynamic reaction process and kinetic parameters has always been a hot topic in these process engineering fields. Among them, the vertical tube furnace reactor has excellent performance such as efficient heat transfer, good fluidity, and can eliminate the heat transfer influence caused by particulate matter aggregation, making the vertical tube furnace widely used in the field of gas-solid reaction kinetics detection technology.

[0003] Currently, the mainstream improvement method for the tube furnace reaction system is to improve the measurement of macroscopic kinetic parameters such as gas concentration signal, heating rate signal, reactor precision control, and product separation, and it is impossible to carry out accurate measurement of microscopic gas-solid reaction kinetic parameters under various fluidized state reaction environments.

[0004] Therefore, a sampling device for gas-solid reactions is proposed. Summary of the Invention

[0005] The purpose of the present invention is to provide a sampling device for gas-solid reactions, which solves the problem that during the gas-solid reaction process using a solid particle generator and a vertical tube furnace reactor, it is impossible to detect and analyze the kinetic parameters of the product for different fluidized states.

[0006] To solve the above technical problems, the technical solution adopted by the present invention is: a sampling device for gas-solid reactions, including a gas cylinder, a solid particle generator, a vertical tube furnace reactor, a vacuum pump, and an exhaust pipe; The gas cylinder is connected to the solid particle generator through a first intake pipe, and a switch valve and a pressure regulating valve are provided on the first intake pipe; The solid particle generator is connected to the inlet of the vertical tube furnace reactor through a second intake pipe; The outlet of the vertical tube furnace reactor is connected to the first inlet of a three-way valve through a sampling pipe, and is also connected to the second inlet of the three-way valve through an outlet pipe; a pipe connector is provided on the sampling pipe, and a copper mesh microgrid is provided on the pipe connector for sampling; The exhaust pipe is connected to the outlet of the three-way valve at one end and to the vacuum pump at the other end.

[0007] As a further technical solution of the above scheme, the vertical tube furnace reactor includes a glass tube, a heating element, an upper flange, and a lower flange; the upper end of the glass tube is connected to the second intake pipe through the upper flange, and the lower end is connected to the sampling pipe through the lower flange; the heating element is arranged on the outer wall of the glass tube to heat the glass tube, and a temperature sensor is also provided inside the glass tube.

[0008] As a further technical solution of the above solution, it further includes a control element for controlling the heating time and heating temperature of the heating element.

[0009] As a further technical solution of the above solution, the sampling tube includes an upper sampling tube and a lower sampling tube; the upper end of the upper sampling tube is telescopically inserted into the glass tube, the lower end passes through the lower wall of the glass tube and is connected to the lower sampling tube through a reducer joint, and the lower sampling tube is connected to a three-way valve.

[0010] As a further technical solution of the above solution, it further includes a collection unit for collecting the temperature of the temperature sensor and the gas concentration of the gas outlet pipe and the sampling pipe.

[0011] As a further technical solution of the above solution, a plurality of gas cylinders are provided, and all of them are connected to the solid particle generator through the first inlet pipe.

[0012] As a further technical solution of the above solution, a filter is further provided on the exhaust pipe.

[0013] As a further technical solution of the above solution, flow meters are further provided on the first inlet pipe and the exhaust pipe.

[0014] Compared with the prior art, the present invention has the following advantages and beneficial effects: The present invention generates reactants through a solid particle generator, uses a copper mesh microgrid to collect samples after reaction in a vertical tube furnace reactor, and can obtain solid particles during the reaction in real time without changing the front and back fluidized reaction environment atmosphere, so as to realize the accurate characterization and measurement of the evolution of the microscopic characteristics of solid particles in different fluidized reaction environment atmospheres, and make up for the lack of measurement of fluidized microscopic gas-solid reaction kinetic parameters in the prior art. Description of the Drawings

[0015] Figure 1 It is a structural schematic diagram of the present invention.

[0016] Figure 2 It is a schematic diagram of a pipe connector and a copper mesh microgrid.

[0017] The interpretations of each label in the figure are as follows: gas cylinder - 1; second inlet pipe - 2; switch valve - 3; pressure regulating valve - 4; solid particle generator - 5; flow meter - 6; vertical tube furnace reactor - 7; heating element - 701; upper flange - 702; control element - 703; glass tube - 704; lower flange - 705; temperature sensor - 8; copper mesh microgrid - 901; pipe connector - 902; upper sampling tube - 903; lower sampling tube - 904; three-way valve - 10; reducer joint - 11; gas outlet pipe - 12; filter - 13; vacuum pump - 14; exhaust pipe - 15; collection unit - 16. Detailed Embodiments

[0018] Next, in combination with the accompanying drawings in the embodiments of the present invention, the technical solutions in the embodiments of the present invention will be clearly and completely described, so as to have a further understanding of the concept of the present invention, the technical problems to be solved, the technical features constituting the technical solutions, and the technical effects brought about.

[0019] As Figure 1 and Figure 2 shown, a sampling device for gas-solid reaction, characterized in that it includes a gas cylinder 1, a solid particle generator 5, a vertical tube furnace reactor 7, a vacuum pump 14 and an exhaust pipe 15; The gas cylinder 1 is connected to the solid particle generator 5 through a first inlet pipe, and a switch valve 3 and a pressure regulating valve 4 are provided on the first inlet pipe; The solid particle generator 5 is connected to the inlet of the vertical tube furnace reactor 7 through a second inlet pipe 2; The outlet of the vertical tube furnace reactor 7 is connected to the first inlet of a three-way valve 10 through a sampling pipe, and is connected to the second inlet of the three-way valve 10 through an outlet pipe 12; a pipe connector 902 is provided on the sampling pipe, and a copper mesh microgrid 901 is provided on the pipe connector 902 for sampling; The exhaust pipe 15 is connected to the outlet of the three-way valve 10 at one end and to the vacuum pump 14 at the other end.

[0020] When using this device, first connect all components together. The gas cylinder 1 is connected to the first inlet pipe provided with the switch valve 3 and the pressure regulating valve 4 to condition and control the ambient environment of the reaction gas. The solid particle generator 5 is connected to the vertical tube furnace reactor 7 through the second inlet pipe 2, and the solid particle generator 5 provides the solid required for the reaction; during the reaction, the solid particles fall downward along the sampling pipe and fall onto the copper mesh microgrid 901. When the solid particles evenly cover a layer of copper mesh, the collection is completed. At this time, the pipe connector 902 is opened, and the copper mesh microgrid 901 can be removed for subsequent analysis. During operation, the vacuum pump 14 extracts air through the three-way valve 10 and the outlet pipe 12 and discharges the air through the exhaust pipe 15 to achieve the pressure environment required for the reaction in the vertical tube furnace reactor 7. The extraction channel of the vacuum pump 14 is adjusted by controlling the switch of the three-way valve 10. Among them, the solid particle generator 5 is a prior art, and the particle concentration and particle size at the outlet end can be controlled by adjusting the advancement speed and the brush rotation speed to provide the solid material required for the reaction. The temperature sensor is an N-type thermocouple for directly measuring the real-time temperature inside the quartz glass tube in the middle of the heating zone. The heating element is a resistance wire, the length of the heating zone is 1800 mm, and the heating temperature range is from room temperature to 1200 °C. And the heating elements are evenly distributed on both sides of the furnace tube to ensure the uniformity and stability of the heating interval.

[0021] As a preferred embodiment, as Figure 1As shown, the vertical tube furnace reactor 7 includes a glass tube 704, a heating element 701, an upper flange 702, and a lower flange 705; the upper end of the glass tube 704 is connected to the second intake pipe 2 through the upper flange 702, and the lower end is connected to the sampling pipe through the lower flange 705; the heating element 701 is arranged on the outer wall of the glass tube 704 to heat the glass tube 704, and a temperature sensor 8 is also arranged inside the glass tube 704. In this embodiment, solid particles react in the glass tube 704. Preferably, a quartz glass tube can be vertically penetrated through the middle of the furnace body as the furnace chamber. Both ends of the glass tube 704 are sealed with the upper flange 702 and the lower flange 705, and the height of the outer frame of the vertical tube furnace 7 should be greater than the length of the external telescopic sampler of the vertical tube furnace reactor 7, which is set to 3600 mm. The heating elements 701 of the vertical tube furnace 7 are evenly distributed on both sides of the furnace tube, the heating zone length is 1800 mm, and the heating temperature range is from room temperature to 1200 °C. In order to obtain the reaction temperature inside the glass tube 704 more accurately, the temperature sensor 8 is placed in the exact middle of the heating zone of the quartz glass tube, so that the real-time temperature of the reaction inside the tube can be obtained more accurately.

[0022] As a preferred embodiment, as Figure 1 shown, it further includes a control element 703 to control the heating time and heating temperature of the heating element 701. In this embodiment, the control element 703 is used to control the heating time and heating temperature of the heating element 701.

[0023] As a preferred embodiment, as Figure 1 shown, the sampling pipe includes an upper sampling pipe 903 and a lower sampling pipe 904; the upper end of the upper sampling pipe 903 is inserted into the glass tube 904 and can be telescopic, and the lower end passes through the lower wall of the glass tube 904 and is connected to the lower sampling pipe 904 through a reducing joint 11, and the lower sampling pipe 904 is connected to a three-way valve 10. In this embodiment, the sampling pipe is made of a high-temperature resistant material and is located at the center of the vertical tube furnace reactor. The upper sampling pipe 903 can be telescopic, and the lower sampling pipe 904 is fixed. The two parts are connected through a reducing joint 11. The radius of the upper sampling pipe 903 should be greater than the radius of the solid particles and less than the radius of the glass tube 704, and the shortest single telescopic distance is 15 mm. The radius of the lower sampling pipe 904 is slightly larger because a copper mesh microgrid 901 needs to be set, and the preferred radius size is set to 8 * 100 mm. By telescoping the upper sampling pipe 903, multiple experiments can be carried out to obtain particles with different required reaction times. The telescopic height is determined according to the particle morphology corresponding to the reaction time desired for each experiment.

[0024] As a preferred embodiment, as Figure 1As shown, it further includes a collection unit 16 for collecting the temperature of the temperature sensor 8, and the gas concentrations of the outlet pipe 12 and the sampling pipe. In this embodiment, the collection unit 16 transmits signals such as the temperature and gas generation measured for the vertical tubular reactor to a computer, thereby performing real-time measurement of the macroscopic parameter data of the gas-solid reaction in the vertical tubular reactor.

[0025] As a preferred embodiment, as Figure 1 shown, there are multiple gas cylinders 1, all of which are connected to the solid particle generator 5 through the first inlet pipe. In this embodiment, experiments are carried out with multiple gas cylinders, improving the efficiency.

[0026] As a preferred embodiment, as Figure 1 shown, a filter 13 is further provided on the exhaust pipe 15. In this embodiment, the filter 13 is provided on the exhaust pipe 15 to filter the residual solid particles in the exhaust pipe 15, ensuring that the discharged gas does not pollute the environment.

[0027] As a preferred embodiment, as Figure 1 shown, flow meters 6 are further provided on the first inlet pipe and the exhaust pipe 15. In this embodiment, the gas flow is controlled by the flow meters, and the flow of each branch of the gas cylinder is adjusted by calculation to obtain the gas flow atmosphere required for different reactions.

[0028] As a preferred embodiment, as Figure 1 shown, the vacuum pump 14 extracts air via the three-way valve 10 and the outlet pipe 12, and discharges the air through the exhaust pipe 15 to achieve the pressure environment required for the reaction in the vertical tubular furnace reactor 7. The extraction channel of the vacuum pump 14 is adjusted by controlling the opening and closing of the three-way valve 10. In this embodiment, real-time sampling measurement of the solid particle reaction in a special reaction environment - a dilute laminar flow environment can be achieved.

[0029] After the gas-solid reaction in the vertical tubular furnace 7 stabilizes, open the switch valve of the variable-diameter joint 11 and the switch of the three-way valve 10 connecting the telescopic sampling pipe 9, close the switch of the three-way valve 10 connecting the outlet pipe, and quickly deposit the solid particles onto the surface of the copper mesh grid 901 inside the telescopic sampling pipe 9 by suction. During this process, the macroscopic data collection unit 16 measures the temperature of the temperature sensor 8 and the data of the gas concentrations in each of the telescopic sampling pipes 9 in real time.

[0030] By adjusting the length of the telescopic upper sampling pipe 903, the solid reaction time is controlled, and solid particles in the gas-solid reaction process are sampled for subsequent precise characterization and measurement of the solid microscopic parameters. Note that the height of the telescopic sampling pipe should not be randomly changed during one experiment to avoid the solid particles deposited and sampled on the surface of the copper mesh grid 901 coming from different reaction times, resulting in inability to distinguish and affecting the microscopic characterization measurement results.

[0031] After a layer of solid particles is evenly deposited on the surface of the copper mesh microgrid 901, turn on the switch of the three-way valve 10 connected to the outlet pipe, close the switch valve of the reducer joint 11 and the switch of the three-way valve 10 connected to the sampling pipe, turn on the pipe connector 902, and take out the copper mesh microgrid 901 inside for carrying out microscopic characterization tests. Subsequently, turn off the vertical tube furnace 7. After the temperature inside the furnace drops below 100 °C, turn off the vacuum pump 14, the gas cylinder 1, and each switch valve in sequence to complete the experiment.

[0032] The real-time sampling and measurement device for fine particle evolution in fluidized reaction kinetics provided by the present invention can obtain solid particles during the reaction in real time without changing the ambient atmosphere of the front and rear fluidized reaction environments. While accurately measuring the macroscopic reaction kinetics parameters by the data acquisition unit, it also samples in real time to obtain fine solid particles during various environmental reaction processes, and can further obtain the accurate characterization and measurement of the microscopic gas-solid reaction kinetics parameters, making up for the deficiency of the existing technology in measuring the fluidized microscopic gas-solid reaction kinetics parameters, and at the same time laying a foundation for the development of new fluidization detection technologies and equipment.

[0033] The "connection" and "fixation" mentioned in the description of the present invention can be fixed connection, machining, welding, or mechanical connection. Understand the specific meanings of the above terms in the present invention according to the specific situation.

[0034] In the description of the present invention, terms such as "center", "upper", "lower", "horizontal", "inner", "outer", etc. indicate the orientation or positional relationship only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation. Therefore, it should not be construed as a limitation to the present invention.

[0035] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit them; although the present invention has been described in detail with reference to the foregoing embodiments, those of ordinary skill in the art should understand that they can still modify the technical solutions described in the foregoing embodiments, or perform equivalent replacements for some or all of the technical features; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. A sampling device for gas-solid reaction, characterized in that: It comprises a gas cylinder (1), a solid particle generator (5), a vertical tubular furnace reactor (7), a vacuum pump (14) and an exhaust pipe (15); A gas cylinder (1) is connected to a solid particle generator (5) via a first air inlet pipe, and a switch valve (3) and a pressure regulating valve (4) are provided on the first air inlet pipe; A solid particle generator (5) connected to the inlet of the vertical tube furnace reactor (7) via a second air inlet pipe (2); A vertical tubular furnace reactor (7), the outlet of which is connected to the first inlet of a three-way valve (10) via a sampling tube, and is connected to the second inlet of the three-way valve (10) via an air outlet pipe (12); the sampling tube is provided with a pipe connector (902), and the pipe connector (902) is provided with a copper mesh microgrid (901) for sampling; An exhaust pipe (15) has one end connected to the outlet of the three-way valve (10) and the other end connected to the vacuum pump (14).

2. A sampling device for gas-solid reaction according to claim 1, characterized in that: The vertical tube furnace reactor (7) comprises a glass tube (704), a heating element (701), an upper flange (702), and a lower flange (705); the upper end of the glass tube (704) is connected to the air inlet pipe (2) via the upper flange (702), and the lower end is connected to the sampling tube via the lower flange (705); the heating element (701) is arranged on the outer wall of the glass tube (704) to heat the glass tube (704), and a temperature sensor (8) is also arranged in the glass tube (704).

3. A sampling device for gas-solid reaction according to claim 2, characterized in that: It also includes a control element (703) for controlling the heating time and heating temperature of the heating element (701).

4. A sampling device for gas-solid reaction according to claim 2, characterized in that: The sampling tube comprises an upper sampling tube (903) and a lower sampling tube (904); the upper end of the upper sampling tube (903) is inserted into the glass tube (904) and is retractable, and the lower end passes through the lower wall of the glass tube (904) and is connected to the lower sampling tube (904) via a reducing joint (11); the lower sampling tube (904) is connected to a three-way valve (10).

5. A sampling device for gas-solid reaction according to claim 1, characterized in that: It also includes a collection unit (16) for collecting the temperature of the temperature sensor (8), the gas concentration of the gas outlet pipe (12) and the sampling pipe.

6. A sampling device for gas-solid reaction according to claim 1, characterized in that: The gas cylinders (1) are provided in plurality, and are all connected to the solid particle generator (5) via a first air inlet pipe.

7. A sampling device for gas-solid reaction according to claim 1, characterized in that: The exhaust pipe (15) is also provided with a filter (13).

8. A sampling device for gas-solid reaction according to claim 1, characterized in that: The first air inlet pipe and the exhaust pipe (15) are also provided with a flow meter (6).

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