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, a gas cylinder is connected to a solid particle generator through a first gas inlet pipe, and a switch valve and a pressure regulating valve are arranged on the first gas inlet pipe; the solid particle generator is connected to an inlet of the vertical tube furnace inductor through a second air 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 sampling pipe is provided with a pipeline connector, and 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. According to the invention, reactants are generated through the solid particle generator and are collected and sampled by using the copper mesh micro-grid after the reactants react in the vertical tubular furnace reactor, and solid particles in the reaction process can be obtained in real time without changing the front and back flow state reaction environment atmosphere, so that accurate characterization measurement of solid microscopic parameters is realized; and the defect of measurement of the fluidization microscopic gas-solid reaction kinetic parameters in the prior art is overcome.

Description

Technical Field

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

[0002] There are a large number of gas-solid reactions in process engineering fields such as energy and power and materials and chemicals. In-depth detection of their dynamic reaction processes and kinetic parameters has always been a hot topic in the research of these process engineering fields. Among them, vertical tube furnace reactors are widely used in the field of gas-solid reaction kinetic detection technology because of their excellent performance such as efficient heat transfer, good fluidity and the ability to eliminate the heat transfer effect caused by particle aggregation.

[0003] Currently, the mainstream improvement method for vertical tube furnace reaction systems is to improve the measurement of macroscopic kinetic parameters such as gas concentration signals, heating rate signals, reactor precision control and product separation, but it is impossible to carry out precise characterization of microscopic gas-solid reaction kinetic parameters in fluidized state.

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

[0005] The object of the present invention is to provide a sampling device for gas-solid reaction to solve the problem that it is difficult to sample in fluidized microscopic gas-solid reaction and unable to detect product separation kinetic parameters.

[0006] In order to solve the above technical problems, the technical solutions adopted by the present invention are as follows: A sampling device for gas-solid reaction, comprising a gas cylinder, a solid particle generator, a vertical tubular furnace reactor, a vacuum pump and an exhaust pipe; The gas cylinder is connected to the solid particle generator through a first air inlet pipe, and a switch valve and a pressure regulating valve are provided on the first air inlet pipe; a solid particle generator connected to the inlet of the vertical tube furnace reactor through a second air inlet pipe; A vertical tubular furnace reactor, the outlet of which is connected to the first inlet of a three-way valve through a sampling tube, and is connected to the second inlet of the three-way valve through an outlet pipe; the sampling tube is provided with a pipe connector, and the pipe connector is provided with a copper mesh microgrid for sampling; An exhaust pipe, one end of which is connected to the outlet of the three-way valve, and the other end is connected to the vacuum pump.

[0007] As a further technical solution of the above scheme, the vertical tubular 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 air inlet pipe through the upper flange, and the lower end is connected to the sampling tube 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 arranged in the glass tube.

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

[0009] As a further technical solution of the above scheme, the sampling tube includes an upper sampling tube and a lower sampling tube; the upper end of the upper sampling tube is inserted into the glass tube and can be retracted, and 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 the three-way valve.

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

[0011] As a further technical solution of the above solution, there are multiple gas cylinders, all of which are connected to the solid particle generator through a first air inlet pipe.

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

[0013] As a further technical solution of the above solution, flow meters are also provided on the first air 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, and uses a copper mesh microgrid to collect samples after the reaction in a vertical tubular furnace reactor. The solid particles in the reaction process can be obtained in real time without changing the atmosphere of the fluidized reaction environment before and after, so as to achieve accurate characterization and measurement of solid microscopic parameters, thereby making up for the deficiency of the prior art in the measurement of fluidized microscopic gas-solid reaction kinetic parameters. BRIEF DESCRIPTION OF THE DRAWINGS

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

[0016] Figure 2 Schematic diagram of the pipe connector and copper mesh microgrid.

[0017] The meanings of the numbers in the figure are: gas cylinder-1; second air inlet pipe-2; switch valve-3; pressure regulating valve-4; solid particle generator-5; flow meter-6; vertical tubular 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; pipeline connector-902; upper sampling tube-903; lower sampling tube-904; three-way valve-10; reducer-11; outlet pipe-12; filter-13; vacuum pump-14; exhaust pipe-15; collection unit-16. DETAILED DESCRIPTION

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

[0019] like Figure 1 and Figure 2 As shown, a sampling device for gas-solid reaction includes 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 through a first air inlet pipe, on which a switch valve 3 and a pressure regulating valve 4 are provided; A solid particle generator 5 is connected to the inlet of a vertical tube furnace reactor 7 via a second air inlet pipe 2; The outlet of the vertical tube furnace reactor 7 is connected to the first inlet of the three-way valve 10 through a sampling tube, and is connected to the second inlet of the three-way valve 10 through an 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; The 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 .

[0020] When using the device, first connect the components together, and connect the gas cylinder 1 to the first air inlet pipe with the switch valve 3 and the pressure regulating valve 4 to conditionally control the atmosphere of the reaction gas. The solid particle generator 5 is connected to the vertical tubular furnace reactor 7 through the second air inlet pipe 2, and the solid particle generator 5 provides the solid required for the reaction; during the reaction, the solid particles fall down along the sampling tube onto the copper mesh microgrid 901, and the collection is completed when the solid particles are evenly spread over a layer of copper mesh. At this time, open the pipeline connector 902, and remove the copper mesh microgrid 901 for subsequent analysis. During the operation, the vacuum pump 14 extracts air through the three-way valve 10 and the outlet pipe 12, and exhausts the air through the exhaust pipe 15, which is used to achieve the low-pressure environment required for the reaction in the vertical tubular furnace reactor 7, and 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 an existing technology, which can control the particle concentration and particle size at the outlet by adjusting the step speed and the brush speed to provide the solid material required for the reaction. The temperature sensor is an N-type thermocouple, which is used to directly measure the real-time temperature in the middle of the quartz glass tube in 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. The heating elements are evenly distributed on both sides of the furnace tube to ensure the uniformity and stability of the heating zone.

[0021] As a preferred embodiment, 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 air inlet pipe 2 through the upper flange 702, and the lower end is connected to the sampling tube 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 in the glass tube 704. In this embodiment, the solid particles react in the glass tube 704, and preferably a quartz glass tube can be vertically penetrated in the middle of the furnace body as a furnace, and the two ends of the glass tube 704 are sealed with an upper flange 702 and a lower flange 705, and the height of the outer frame of the vertical tube furnace reactor 7 should be greater than the length of the external telescopic sampler of the three-dimensional tube furnace reactor 7, which is set to 3600 mm, and the heating elements 701 of the vertical tube furnace reactor 7 are evenly distributed on both sides of the furnace tube, the length of the heating zone is 1800 mm, and the heating temperature range is room temperature to 1200 ° C. In order to obtain the reaction temperature in the glass tube 704 more accurately, the temperature sensor 8 is placed in the middle of the heating zone of the quartz glass tube, so that the real-time temperature of the reaction in the tube can be obtained more accurately.

[0022] As a preferred embodiment, Figure 1 As shown, the control element 703 is further included to control the heating time and heating temperature of the heating element 701. In this embodiment, the heating time and heating temperature of the heating element 701 are controlled by the control element 703.

[0023] As a preferred embodiment, Figure 1 As shown, the sampling tube includes 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 704 and can be retracted, and the lower end passes through the lower wall of the glass tube 704 and is connected to the lower sampling tube 904 through a reducer 11, and the lower sampling tube 904 is connected to a three-way valve 10. In this embodiment, the sampling tube is made of high temperature resistant material and is located in the center of the vertical tubular furnace reactor. The upper sampling tube 903 can be retracted, the lower sampling tube 904 is fixed, and the two parts are connected by a reducer 11. The radius of the upper sampling tube 903 should be greater than the radius of the solid particles and smaller than the radius of the glass tube 704. The shortest single telescopic distance is 15mm. The radius of the lower sampling tube 904 is slightly larger because the copper mesh microgrid 901 needs to be set, and the preferred radius size is set to 8*100 mm. Multiple experiments can be carried out by retracting the upper sampling tube 903 to obtain particles with different reaction times. The height of the telescopic height is determined according to the particle morphology of the corresponding reaction time to be obtained in each experiment.

[0024] As a preferred embodiment, Figure 1As shown, 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 tube. In this embodiment, the collection unit 16 transmits the temperature, gas generation and other signals measured for the vertical tube furnace reactor to the computer, thereby performing real-time measurement of the macroscopic parameter data of the gas-solid reaction in the vertical tube furnace reactor.

[0025] As a preferred embodiment, Figure 1 As shown, the gas cylinder 1 is provided with a plurality of gas cylinders, all of which are connected to the solid particle generator 5 through the first air inlet pipe. In this embodiment, the test is carried out by using a plurality of gas cylinders to improve the efficiency.

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

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

[0028] After the gas-solid reaction in the vertical tubular furnace reactor 7 is stabilized, the switch valve of the reducer 11 and the three-way valve 10 connected to the telescopic sampling tube are opened, and the switch of the three-way valve 10 connected to the gas outlet pipe is closed. The solid particles are quickly deposited on the surface of the copper mesh microgrid 901 inside the telescopic sampling tube through suction. During this process, the macro data acquisition unit 16 measures the temperature of the temperature sensor 8 and the data of the concentration of each gas in the telescopic sampling tube in real time.

[0029] By adjusting the length of the telescopic upper sampling tube 903, the solid reaction time is controlled, and the solid particles in the gas-solid reaction process are sampled for subsequent precise characterization and measurement of solid microscopic parameters. Note that the height of the telescopic sampling tube cannot be changed arbitrarily during an experiment to avoid the solid particles deposited on the surface of the copper mesh microgrid 901 from different reaction times, which makes it impossible to distinguish and affects the microscopic characterization measurement results.

[0030] After a layer of solid particles is uniformly deposited on the surface of the copper mesh microgrid 901, the three-way valve 10 connected to the gas outlet pipe is opened, the switch valve of the reducer 11 and the three-way valve 10 connected to the sampling pipe are closed, and the pipeline connector 902 is opened to take out the copper mesh microgrid 901 inside for microscopic characterization testing. Subsequently, the vertical tubular furnace reactor 7 is closed, and when the temperature in the furnace drops below 100°C, the vacuum pump 14, the gas cylinder 1 and the switch valves are closed successively to complete the experiment.

[0031] The device for real-time sampling and measuring fine particle evolution of fluidized reaction kinetics provided by the present invention can obtain solid particles in the reaction process in real time without changing the atmosphere of the fluidized reaction environment before and after. While the data acquisition unit accurately measures the macroscopic reaction kinetic parameters, it also samples and obtains fine solid particles in the reaction process in real time, and can further obtain accurate characterization and measurement of microscopic gas-solid reaction kinetic parameters, making up for the shortcomings of the existing technology in the measurement of fluidized microscopic gas-solid reaction kinetic parameters, and at the same time laying a solid foundation for the development of new fluidized detection technology and equipment.

[0032] The terms “connection” and “fixation” mentioned in the description of the present invention may refer to fixed connection, processing and forming, welding or mechanical connection. The specific meanings of the above terms in the present invention shall be understood according to the specific circumstances.

[0033] In the description of the present invention, the terms "center", "upper", "lower", "horizontal", "inside", "outside", etc., which indicate the orientation or position relationship, are only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying a specific orientation that the device or element referred to must have, and therefore cannot be understood as a limitation on the present invention.

[0034] 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 it. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that the technical solutions described in the aforementioned embodiments can still be modified, or some or all of the technical features therein can be replaced by equivalents. However, 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 second 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 (704) and is retractable, and the lower end passes through the lower wall of the glass tube (704) 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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