CN213633278U - Gas-solid reaction kinetic analysis device of miniature spouted bed - Google Patents
Gas-solid reaction kinetic analysis device of miniature spouted bed Download PDFInfo
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- CN213633278U CN213633278U CN202021833942.5U CN202021833942U CN213633278U CN 213633278 U CN213633278 U CN 213633278U CN 202021833942 U CN202021833942 U CN 202021833942U CN 213633278 U CN213633278 U CN 213633278U
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Abstract
The utility model discloses a miniature spouted bed gas-solid reaction kinetics analytical equipment belongs to gas-solid reaction test method and instrument field, and its analytical equipment includes pulse sampling device, isothermal reaction generating device, gas circuit device and online gas analysis testing arrangement. The solid sample is instantly fed into the micro spouted bed reactor by a pulse sample feeding device, the reactions such as combustion, pyrolysis, gasification or decomposition and the like rapidly occur under the isothermal condition, the reaction mechanism is speculated by measuring the generation sequence and the concentration change characteristic of gas components in the reaction by rapid online process mass spectrometry, and then the reaction kinetic parameters are solved. The utility model discloses a miniature spouted bed is as the reactor, can guarantee that the on-line of reaction material is sent into in the twinkling of an eye, realizes reacting under the approximate isothermal condition, makes its reaction condition who is more close among the practical application, and the reaction kinetics parameter that records also is more close intrinsic reaction kinetics parameter.
Description
Technical Field
The utility model belongs to gas-solid reaction test method and instrument field, concretely relates to miniature spouted bed gas-solid reaction kinetics analytical equipment. The micro spouted bed gas-solid reaction kinetic analysis device is suitable for the fields of combustion, pyrolysis and gasification, ore reduction and roasting, salt decomposition and the like of various solid fuels, can realize isothermal rapid reaction, can accurately measure reaction speed and reaction time, and can estimate reaction mechanism by analyzing the change characteristics of products to calculate reaction kinetic parameters.
Background
The gas-solid reaction is widely existed in the conversion process of substances in various fields of industrial production, and the test and analysis of the gas-solid reaction characteristics and dynamics are important contents of basic research of natural science and engineering and are important supports of application technology. Only by the research of gas-solid reaction chemical kinetics, the action relationship between reaction rate and influence factors such as temperature, concentration, mass transfer, particle size, surface, composition, reaction atmosphere and the like and the change rule caused by the action relationship can be known and mastered, so that a mathematical model and necessary quantitative basis are provided for the amplification of laboratory research results and the design of a reactor, and corresponding prediction, diagnosis and treatment measures are taken for problems possibly occurring in engineering application. Therefore, the test analysis of the reaction kinetics not only has important theoretical value, but also has important practical significance, and is an important component in the success or failure of research and development and application of new technologies.
For gas-solid reaction, a differential reactor is generally used for kinetic analysis and test of the reaction, and the analysis method thereof includes both isothermal and non-isothermal methods. Non-isothermal reaction analysis represented by thermogravimetry constitutes the only commercial reaction analysis method and analysis instrument at present, and the basic requirements are as follows: the solid reactant was set at ambient temperature and then temperature programmed. The reaction characteristics are analyzed and the reaction kinetics are calculated by measuring the mass change of the reaction sample in the temperature programming process, and the method has the advantages of good operation stability, high mass change measurement precision and the like. However, the chemical reaction in the thermogravimetric analyzer is seriously affected by diffusion, which easily causes temperature deviation for high-energy reaction, and cannot test the reaction characteristic of any fixed point temperature for unstable substances. Approximate integrals of temperature functions required by reaction kinetics are calculated by adopting a non-isothermal method based on thermogravimetric analysis data, the calculation process is complex, and the reaction model functions are difficult to uniquely determine. Therefore, the gas-solid phase chemical reaction technology field has been dedicated to establishing an isothermal differential reaction analyzer capable of separating a temperature function and a reaction model function, but a standard isothermal differential reaction testing instrument is not yet commercialized.
SUMMERY OF THE UTILITY MODEL
In order to make up the defects of the traditional program temperature rise thermal analysis, the utility model provides a micro spouted bed gas-solid reaction kinetic analysis device; the micro spouted bed gas-solid reaction kinetic analysis device can realize constant temperature sample introduction, rapid heating, low diffusion inhibition and online rapid gas detection of solid reactants, further analyze and determine corresponding reaction kinetic parameters, and establish a corresponding isothermal differential reaction analysis method.
The utility model provides a technical scheme that above-mentioned problem adopted is: a micro spouted bed gas-solid reaction kinetic analysis device is characterized by comprising a pulse sample introduction device, an isothermal reaction generation device, a gas path device and an online gas analysis testing device;
the pulse sampling device comprises a first pressure sensor, an electromagnetic valve, a programming logic controller and a feeder; the first pressure sensor and the programming logic controller are both connected with an electromagnetic valve, the electromagnetic valve is connected with an inlet of a feeder, and an outlet of the feeder extends into the micro spouted bed;
the isothermal reaction generating device comprises a micro spouted bed, flowing medium particles, a first thermocouple, a plug plate, a rotary stop valve, an electric heating furnace, a second thermocouple, a temperature display meter and a second pressure sensor; the flow medium particles are arranged in the micro-spouted bed, the first thermocouple is inserted into the bed layer of the micro-spouted bed and is positioned above the flow medium particles, the plug plate is arranged above the first thermocouple in the micro-spouted bed, the rotary stop valve is tightly close to the lowest part of the U-shaped bent pipe at the lower part of the micro-spouted bed, the electric heating furnace is arranged outside the micro-spouted bed, the second thermocouple is arranged outside the micro-spouted bed, the temperature display meter is connected with the second thermocouple, and the second pressure sensor is connected with the top of the micro-spouted bed;
the gas path device comprises a first gas source, a second gas source, a micro pulse gas inlet gas path and a mixed gas inlet gas path; the first gas source and the second gas source are connected to the micro-spouted bed through a mixed gas inlet gas path, a first flowmeter, a second flowmeter and a gas mixing tank are arranged on the mixed gas inlet gas path, the first flowmeter and the second flowmeter are respectively connected with outlets of the first gas source and the second gas source, an inlet of the gas mixing tank is respectively connected with the first flowmeter and the second flowmeter, and an outlet of the gas mixing tank is connected with an inlet of the micro-spouted bed; the second gas source is connected to the pulse sampling device through a trace pulse gas inlet circuit;
the on-line gas analysis testing device comprises a flow sensor, a gas filter, a three-way pipe, a capillary and a rapid on-line process mass spectrum; the outlet of the micro spouted bed is connected with a flow sensor, the flow sensor is connected with the inlet of a gas filter, the outlet of the gas filter is connected with the first end of a three-way pipe, the second end of the three-way pipe is connected with one end of a capillary, the third end of the three-way pipe is communicated with the atmosphere, and the other end of the capillary is connected with a rapid online process mass spectrum; the output ends of the first pressure sensor, the second pressure sensor, the temperature display meter and the rapid online process mass spectrum are respectively connected with the input end of a data acquisition unit, and the output end of the data acquisition unit is connected with a computer; the computer analyzes the data collected by the data collector and controls the programmable logic controller to open and close the electromagnetic valve.
Furthermore, the micro-spouted bed is made of quartz or high-temperature-resistant alloy, the cross section of the micro-spouted bed is circular, the diameter of the micro-spouted bed is 20mm, and the height of the micro-spouted bed is 100-150 mm; the reaction sample of the micro spouted bed is sent into the fluidized medium granular layer by a pulse sampling device on the side wall, and a plug plate is arranged above the fluidized layer.
Furthermore, the rotary stop valve is connected with the lowest part of the U-shaped elbow at the lower part of the micro-spouted bed and is used for controlling the discharge of flowing medium particles and reaction products.
Compared with the prior art, the utility model, have following advantage and effect:
1. the utility model discloses a pulse sampling device has realized adding solid-state reactant on line for the reactor can simulate the reaction condition among the practical application better, and the gained data is more true.
2. The utility model discloses the even temperature distribution of well miniature spouted bed, good material mobility and heat transfer characteristic and reactant send into in the twinkling of an eye and make it realize rapid heating up and reach the reaction temperature of settlement to realize isothermal reaction.
3. The utility model discloses an optimization to different reaction experimental conditions, can minimize the influence of diffusion to the reaction, gained kinetic parameter is closer intrinsic kinetics.
4. The utility model discloses the discharge and the change problem of reaction bed material and reaction product can effectively be solved in rotatory stop valve's use, have realized the continuity and the validity of reaction.
5. The utility model discloses can expand and be applicable to all the requirements and add solid-state reactant on line and the key result is gaseous gas-solid reaction.
Drawings
Fig. 1 is a schematic structural diagram of the gas-solid reaction kinetic analysis device of the middle-micro spouted bed of the utility model.
In the figure: the device comprises a first gas source 1, a second gas source 2, a first flowmeter 3, a second flowmeter 4, a gas mixing tank 5, a first pressure sensor 6, a solenoid valve 7, a programmed logic controller 8, a feeder 9, a pulse sampling device 10, flowing medium particles 11, a first thermocouple 12, a plug plate 13, a rotary stop valve 14, an electric heating furnace 15, a micro-spouted bed 16, a second thermocouple 17, a temperature display meter 18, a second pressure sensor 19, a flow sensor 20, a gas filter 21, a three-way pipe 22, a capillary 23, a fast online process mass spectrum 24, a data collector 25 and a computer 26.
Detailed Description
The present invention will be described in further detail by way of examples with reference to the accompanying drawings, which are illustrative of the present invention and are not intended to limit the present invention.
Referring to fig. 1, a gas-solid reaction kinetic analysis device of a micro spouted bed comprises a pulse sample introduction device 10, an isothermal reaction generation device, a gas path device and an online gas analysis testing device.
The pulse sampling device 10 comprises a first pressure sensor 6, an electromagnetic valve 7, a programming logic controller 8 and a feeder 9; the first pressure sensor 6 and the programmable logic controller 8 are both connected with the electromagnetic valve 7, the electromagnetic valve 7 is connected with the inlet of the feeder 9, and the outlet of the feeder 9 extends into the micro-spouted bed 16, so that the pulse sample introduction can be rapidly mixed with the flowing medium particles 11.
The first pressure sensor 6 is used for controlling pulse air inlet pressure to ensure that the air inlet pressure is the same in each experiment; the solenoid valve 7 is a direct current solenoid valve, the switching state of which is controlled by a programmable logic controller 8, and the switching response time of the switch is generally controlled to be in millisecond level, so that the micro air inlet and air inlet time is ensured, and the influence on the spouted fluidized state in the micro spouted bed 16 is reduced as much as possible.
The isothermal reaction generating device comprises a micro spouted bed 16, flowing medium particles 11, a first thermocouple 12, a plug plate 13, a rotary stop valve 14, an electric heating furnace 15, a second thermocouple 17, a temperature display meter 18 and a second pressure sensor 19; the micro-spouted bed 16 is made of quartz or high-temperature-resistant alloy, and has a circular cross section, a diameter of 20mm and a height of 100-150 mm; the reaction sample of the micro-spouted bed 16 is sent into the layer of the flowing medium particles 11 by the pulse sampling device 10 on the side wall; the flowing medium particles 11 are arranged in the micro-spouted bed 16, the first thermocouple 12 is inserted into the bed layer of the micro-spouted bed 16 and is used for monitoring the actual temperature in the fluidized bed layer, the first thermocouple 12 is positioned above the flowing medium particles 11, the second pressure sensor 19 is used for measuring the actual pressure in the micro-spouted bed 16 and is used as a reference for setting the pressure of the first pressure sensor 6 in the pulse sampling device 10, and the pressure of the pulse air inlet path is greater than the pressure in the micro-spouted bed 16; the plug plate 13 is arranged above the first thermocouple 12 in the micro-spouted bed 16; the plug plate 13 is provided with a large number of uniform micropores, so that the flowing medium particles 11 are prevented from flowing unevenly and overflowing at the initial ventilation moment of the mixed gas inlet gas circuit and the micro pulse inlet gas circuit without influencing the rapid outflow of gas products; the rotary stop valve 14 is arranged close to the lowest part of the U-shaped elbow at the lower part of the micro-spouted bed 16 and is used for controlling the discharge of the flowing medium particles 11 and reaction products, can be freely opened and closed in both cold state and hot state, and can ensure the good air tightness of the micro-spouted bed 16 when closed; the electric heating furnace 15 is arranged outside the micro-spouted bed 16, the second thermocouple 17 is arranged outside the micro-spouted bed 16, the temperature display meter 18 is connected with the second thermocouple 17, and the second pressure sensor 19 is connected with the top of the micro-spouted bed 16; the internal temperature of the electric heating furnace 15 is measured and displayed by the second thermocouple 17 and the temperature display meter 18, and is controlled by the data collector 25 and the computer 26.
The gas circuit device is used for adjusting atmosphere and flow in the pulse sampling device 10 and the micro spouted bed 16, and comprises a first gas source 1, a second gas source 2, a micro pulse gas inlet circuit and a mixed gas inlet circuit.
The first gas source 1 and the second gas source 2 are connected to the micro-spouted bed 16 through a mixed gas inlet gas path, a first flowmeter 3, a second flowmeter 4 and a gas mixing tank 5 are arranged on the mixed gas inlet gas path, the first flowmeter 3 and the second flowmeter 4 are respectively connected with outlets of the first gas source 1 and the second gas source 2, an inlet of the gas mixing tank 5 is respectively connected with the first flowmeter 3 and the second flowmeter 4, and an outlet of the gas mixing tank 5 is connected with an inlet of the micro-spouted bed 16; the gas flowing out of the first flowmeter 3 and the second flowmeter 4 is uniformly mixed by the gas mixing tank 5 and then is introduced into the micro-spouted bed 16, and the flowing medium particles 11 at the bottom of the micro-spouted bed are blown up to be in a spouted fluidization state.
The second gas source 2 is connected to the pulse sample injection device 10 through a trace pulse gas inlet circuit, and provides a trace pulse inert gas flow during sample injection.
The on-line gas analysis testing device is used for determining the generation sequence and concentration change characteristics of gas components in the reaction process of the solid sample, further inferring a reaction mechanism and calculating reaction kinetic parameters. The on-line gas analysis testing device comprises a flow sensor 20, a gas filter 21, a three-way pipe 22, a capillary 23 and a rapid on-line process mass spectrum 24; the outlet of the micro spouted bed 16 is connected with a flow sensor 20, the flow sensor 20 is connected with the inlet of a gas filter 21, the outlet of the gas filter 21 is connected with the first end of a three-way pipe 22, the second end of the three-way pipe 22 is connected with one end of a capillary 23, the third end of the three-way pipe 22 is communicated with the atmosphere, and the other end of the capillary 23 is connected with a rapid online process mass spectrum 24.
The gas at the outlet of the micro-spouted bed 16 passes through the flow sensor 20 and then enters the gas filter 21 for purification, the ash and moisture in the gas are removed and then flows into the three-way pipe 22, the second end of the three-way pipe 22 is connected with an ultrafine capillary 23, the third end is communicated with the atmosphere, the rapid online process mass spectrum 24 sucks in trace gas through the capillary 23 for detection, and most of the rest gas is discharged from the third end of the three-way pipe 22.
The output ends of the first pressure sensor 6, the second pressure sensor 19, the temperature display meter 18 and the rapid online process mass spectrum 24 are respectively connected with the input end of a data acquisition unit 25, and the output end of the data acquisition unit 25 is connected with a computer 26; the computer 26 analyzes the data collected by the data collector 25 and controls the programmable logic controller 8 to open and close the electromagnetic valve 7.
The analysis method of the micro spouted bed gas-solid reaction kinetic analysis device comprises the following steps:
before the experiment, the rotary stop valve 14 is closed, bed materials with a certain bed height are put into the micro-spouted bed 16, the electric heating furnace 15 is started to be heated to a preset temperature and then stays for a period of time, and the bed materials are dried; opening the first gas source 1, the second gas source 2, the first flowmeter 3 and the second flowmeter 4 and setting corresponding gas flow rates to enable the bed material to be in a stable spouted fluidized state and stay for a period of time to discharge impurity gas in the micro-spouted bed 16; the first thermocouple 12 measures the actual temperature in the stationary flow bed to correct the temperature to a set value;
opening the rapid online process mass spectrum 24, scanning and detecting outlet gas, and proving that impurity gas in the micro-spouted bed 16 is completely discharged when the components and concentration of the detected gas are stable; weighing 10-50mg of sample, putting the sample into a feeder 9, switching on a solenoid valve 7 to be in a closed state, opening a second gas source 2, and regulating to generate a trace pulse gas with certain pressure through a first pressure sensor 6; starting a programming logic controller 8, opening a switch of an electromagnetic valve 7, instantly sending the sample in a feeder 9 into the fluidized bed layer by pulse airflow, rapidly mixing the sample with the materials and starting to react; at this point, the fast online process mass spectrum 24 begins to analyze the composition and concentration of the gas generated at the outlet of the micro-spouted bed 16; after the reaction is finished, storing the data of the rapid online process mass spectrum 24;
during the next group of experiments, the temperature of the electric heating furnace 15 is reset, the steps are repeated, the change relation of the conversion rate of the solid sample with time at different temperatures is measured, and the reaction kinetic parameters can be calculated by an isothermal analysis method according to the obtained array data (generally 4 to 5 groups);
after the experiment is finished, all power supplies are turned off, and after the electric heating furnace 15 is cooled, the rotary stop valve 14 is opened to carry out slag discharge and bed material replacement so as to prepare for other subsequent experiments.
The working processes of the programming logic controller 8, the fast online process mass spectrum 24, the data acquisition unit 25 and the computer 26 belong to the prior art.
Those not described in detail in this specification are well within the skill of the art.
Although the present invention has been described with reference to the above embodiments, it should not be construed as being limited to the scope of the present invention, and any modifications and alterations made by those skilled in the art without departing from the spirit and scope of the present invention should fall within the scope of the present invention.
Claims (3)
1. A micro spouted bed gas-solid reaction kinetic analysis device is characterized by comprising a pulse sample introduction device (10), an isothermal reaction generation device, a gas path device and an online gas analysis testing device;
the pulse sampling device (10) comprises a first pressure sensor (6), an electromagnetic valve (7), a programming logic controller (8) and a feeder (9); the first pressure sensor (6) and the programmed logic controller (8) are both connected with an electromagnetic valve (7), the electromagnetic valve (7) is connected with an inlet of a feeder (9), and an outlet of the feeder (9) extends into the micro-spouted bed (16);
the isothermal reaction generating device comprises a micro spouted bed (16), flowing medium particles (11), a first thermocouple (12), a plug plate (13), a rotary stop valve (14), an electric heating furnace (15), a second thermocouple (17), a temperature display meter (18) and a second pressure sensor (19); the flowing medium particles (11) are arranged in a micro-spouted bed (16), the first thermocouple (12) is inserted into the bed layer of the micro-spouted bed (16), the first thermocouple (12) is positioned above the flowing medium particles (11), the plug plate (13) is arranged above the first thermocouple (12) in the micro-spouted bed (16), the rotary stop valve (14) is tightly close to the lowest part of a U-shaped elbow at the lower part of the micro-spouted bed (16), the electric heating furnace (15) is arranged outside the micro-spouted bed (16), the second thermocouple (17) is arranged outside the micro-spouted bed (16), the temperature display meter (18) is connected with the second thermocouple (17), and the second pressure sensor (19) is connected to the top of the micro-spouted bed (16);
the gas path device comprises a first gas source (1), a second gas source (2), a micro pulse gas inlet gas path and a mixed gas inlet gas path; the first gas source (1) and the second gas source (2) are connected to the micro-spouted bed (16) through a mixed gas inlet gas path, a first flowmeter (3), a second flowmeter (4) and a gas mixing tank (5) are arranged on the mixed gas inlet gas path, the first flowmeter (3) and the second flowmeter (4) are respectively connected with outlets of the first gas source (1) and the second gas source (2), an inlet of the gas mixing tank (5) is respectively connected with the first flowmeter (3) and the second flowmeter (4), and an outlet of the gas mixing tank (5) is connected with an inlet of the micro-spouted bed (16); the second gas source (2) is connected to the pulse sampling device (10) through a micro pulse gas inlet circuit;
the online gas analysis testing device comprises a flow sensor (20), a gas filter (21), a three-way pipe (22), a capillary (23) and a rapid online process mass spectrum (24); the outlet of the micro spouted bed (16) is connected with a flow sensor (20), the flow sensor (20) is connected with the inlet of a gas filter (21), the outlet of the gas filter (21) is connected with the first end of a three-way pipe (22), the second end of the three-way pipe (22) is connected with one end of a capillary tube (23), the third end of the three-way pipe (22) is communicated with the atmosphere, and the other end of the capillary tube (23) is connected with a rapid online process mass spectrum (24); the output ends of the first pressure sensor (6), the second pressure sensor (19), the temperature display meter (18) and the rapid online process mass spectrum (24) are respectively connected with the input end of a data acquisition unit (25), and the output end of the data acquisition unit (25) is connected with a computer (26).
2. The gas-solid reaction kinetic analysis device of the micro-spouted bed according to claim 1, wherein the micro-spouted bed (16) is made of quartz or high temperature resistant alloy material, and has a circular cross section, a diameter of 20mm, and a height of 100-150 mm; reaction samples of the micro spouted bed (16) are sent into the fluidized medium particle (11) layer through the pulse sampling device (10) on the side wall, and a plug plate (13) is arranged above the fluidized layer.
3. A device for analyzing gas-solid reaction kinetics of a micro-spouted bed according to claim 1 or 2, wherein the rotary shut-off valve (14) is connected to the lowest part of the U-bend at the lower part of the micro-spouted bed (16) for controlling the discharge of the flowing medium particles (11) and the reaction products.
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