CN112986327A - Rapid heating-atmosphere variable-weight real-time thermal analysis device and application - Google Patents
Rapid heating-atmosphere variable-weight real-time thermal analysis device and application Download PDFInfo
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Abstract
The invention provides a rapid temperature rise-atmosphere variable-weight real-time thermal analysis device and application thereof, comprising a furnace body reaction device, a fixed protection device, a sample weighing device and an electric control device; the sample weighing device utilizes the pressure sensor to replace a traditional thermobalance, is combined with a movable furnace body, realizes the measurement of macroscopic sample amount (g-kg level), avoids mass errors caused by vibration generated by moving a measuring object, and breaks through the limitation caused by easy corrosion of the thermobalance by adopting corrosion-resistant materials; the random combination of various combustion atmospheres and extremely fast temperature rise can be realized, and the application range is greatly improved; the method can accurately measure the thermal burst amount of the sample, and provides an effective way for the research of the later-stage thermal burst behavior.
Description
Technical Field
The invention relates to the field of heating experimental equipment, in particular to a rapid temperature rise-atmosphere variable-weight real-time thermal analysis device and application thereof.
Background
A thermal analyzer is an instrument for performing thermogravimetric analysis and thermogravimetric differential measurement on a sample. The general thermogravimetric analyzers on the market have small volume, high precision requirement and small measured sample amount, the measurement range of the thermogravimetric analyzers is mostly less than or equal to 100mg, and the test requirement of large sample amount cannot be met. At present, thermogravimetric analysis is carried out on a 'large sample' with larger size and mass, the total reaction condition of the large sample can be represented only by the mass difference before and after the heating of a tubular furnace, and the real-time reaction condition of the large sample in the heating process cannot be known, so that the method has certain limitation. Due to the restriction of sample quantity and the limitation of the conventional thermogravimetric analyzer to a severe use environment, the thermogravimetric analyzer can only be used for laboratory research (such as pyrolysis, combustion and gasification) and cannot be used for actual field test of enterprises. In addition, at present, the thermal balance has high requirements on the atmosphere of the sample, mainly uses inert gases (such as nitrogen, argon and the like), oxidizing atmospheres (such as air, oxygen and the like) or other atmospheres (such as carbon dioxide and the like), only few thermal balances can be used for corrosive atmospheres (such as chlorine, sulfur dioxide and water vapor), and have certain limitation on the atmosphere of the sample. And generally adopts the temperature programming, can't realize the constant temperature under various atmospheres and advance the appearance. The existence of these problems greatly affects the efficiency of research, and hinders the progress of research in which this technique simulates actual industrial processes. With higher research requirements, in order to make thermogravimetric analysis conditions closer to reality, thermogravimetric analysis results are more representative, and development of a thermogravimetric analysis device which can realize extremely rapid temperature rise and controllable atmosphere and is oriented to industrialization under large sample quantity (g-kg level) has important practical significance.
The Chinese invention patent CN 101799242A discloses a controllable rapid heating balance reaction furnace. The sample is rapidly introduced into the reaction area of the high-temperature furnace by utilizing the movement of the balance lifter, so that the rapid heating and constant-temperature experiment is realized. However, in the method, the balance cannot be stabilized in a short time due to the fact that the balance lifter is moved, so that great errors are generated, and accurate measurement cannot be achieved. The chinese invention patent CN 107271320 a discloses a thermogravimetric analyzer capable of realizing rapid temperature rise, however, the method for realizing constant temperature sample injection by the apparatus is also to move the balance by the balance elevator, and large errors are also generated. The Chinese invention patent CN 104614272A discloses an application method of a high-temperature pressurizing thermal balance, the thermal balance realizes constant-temperature sample injection by moving a pressure tank, and the problem of large error caused by moving the balance is solved. However, in the present invention patent, all weighing tools used in thermal analysis are balances, and since the analytical balance is easily corroded by gas, which affects the measurement accuracy, a balance chamber needs to be protected by protective gas, which is frequent in maintenance and harsh in use environment, and is not suitable for industrial detection.
The thermal conversion processes such as drying, pyrolysis, combustion, gasification and the like are common processes related to a plurality of industries such as the field of energy chemical industry, the field of energy conservation and environmental protection, and the accurate measurement of the thermal conversion processes has great significance for controlling industrial processes. At present, a thermogravimetric analyzer is a mainstream analyzer for researching the processes in a laboratory, but the analysis from an industrial field to the laboratory has large hysteresis, the operation field condition cannot be reflected in time, and the laboratory thermogravimetric analyzer has limited analysis sample amount and is difficult to analyze massive samples in some industrial processes. In addition, some special industries such as the thermal conversion process of the formed material (briquette pyrolysis, briquette combustion) or the thermal conversion process of the high-moisture material (sludge combustion, coal slurry combustion) are accompanied by a thermal explosion process, and the thermal explosion action directly influences the retention time of the material in a reaction device, so that the thermal conversion efficiency is influenced, but at present, no device and method for accurately measuring the thermal explosion action of the macroscopic material exist.
Disclosure of Invention
In order to solve the defects of the prior art, the rapid temperature rise-atmosphere variable-weight real-time thermal analysis device and the application thereof are provided, so that the problems of mass error caused by vibration generated by moving a measurement object in the using process of the device, easy corrosion of a thermal balance, low applicability caused by incapability of randomly combining a combustion atmosphere and the rapid temperature rise and incapability of accurately measuring the thermal burst quantity of a sample can be solved.
The invention provides a rapid heating-atmosphere variable-weight real-time thermal analysis device which comprises a furnace body reaction device, a fixed protection device, a sample weighing device and an electric control device, wherein the furnace body reaction device comprises a corundum reaction tube and a reaction shell, the corundum reaction tube is embedded in the reaction shell, a first sealing ring is arranged at a radial diminishing position, an exhaust pipe is arranged at the lower part of the corundum reaction tube, a sample cooling area and a sample heating area are arranged in the reaction shell, a water inlet pipe and a water outlet pipe are arranged in the sample cooling area, the fixed protection device comprises a corundum sleeve and a protection shell, the corundum sleeve is arranged in the protection shell, the upper end of the corundum sleeve exceeds the protection shell, a second sealing ring is arranged in the protection shell, an air inlet pipe is arranged on the protection shell, the tail end of the air inlet pipe is inserted into the corundum sleeve, and the sample weighing device comprises a raised ferromagnetic, The electric control device comprises a measuring element closed cavity, an electromagnet and a film pressure sensor, the electromagnet is embedded in the measuring element closed cavity, and the film pressure sensor is tightly attached to the lower surface of the electromagnet.
As a further improvement of the scheme, the raised ferromagnetic material is made of a corrosion-resistant soft magnetic material.
As a further improvement of the scheme, the outer surface of the electromagnet is wrapped with the corrosion-resistant material, and the iron core inside the electromagnet cannot be magnetized.
As a further improvement of the scheme, the outer surface of the thin film pressure sensor is coated with a corrosion-resistant material.
The application of the rapid temperature rise-atmosphere variable-weight real-time thermal analysis device is characterized in that: the method comprises the following steps:
A. and (3) drying at constant temperature: in an initial state, the reaction crucible is in a sample cooling area; introducing air into the corundum reaction tube and the corundum sleeve, starting to heat a sample heating area, moving the corundum reaction tube and the reaction shell upwards after the temperature reaches a set drying temperature until the upper end of the corundum reaction tube is tightly contacted with a second sealing ring in the corundum sleeve, stopping moving, completely placing the reaction crucible in the center of the sample heating area, and starting data acquisition software of a computer to acquire data of the thin film pressure sensor;
B. constant-temperature pyrolysis: in an initial state, the reaction crucible is in a sample cooling area; introducing inert gas or reducing gas into the corundum reaction tube and the corundum sleeve, starting to heat a sample heating area, moving the corundum reaction tube and the reaction shell upwards after the temperature reaches a set pyrolysis temperature until the upper end of the corundum reaction tube is tightly contacted with a second sealing ring in the corundum sleeve, stopping moving, completely placing the reaction crucible in the center of the sample heating area, and starting data acquisition software of a computer to acquire data of the thin-film pressure sensor;
C. constant temperature combustion: in an initial state, the reaction crucible is in a sample cooling area; introducing oxidizing gas into the corundum reaction tube and the corundum sleeve, starting to heat a sample heating area, moving the corundum reaction tube and the reaction shell upwards after the temperature reaches a set combustion temperature until the upper end of the corundum reaction tube is tightly contacted with a second sealing ring in the corundum sleeve, stopping moving, completely placing the reaction crucible in the center of the sample heating area, and starting data acquisition software of a computer to acquire data of the thin film pressure sensor;
D. constant temperature gasification: in an initial state, the reaction crucible is in a sample cooling area; introducing a gasifying agent into the corundum reaction tube and the corundum sleeve, starting to heat a sample heating area, moving the corundum reaction tube and the reaction shell upwards after the temperature reaches a set gasifying temperature until the upper end of the corundum reaction tube is tightly contacted with a second sealing ring in the corundum sleeve, stopping moving, completely placing the reaction crucible in the center of the sample heating area, and starting data acquisition software of a computer to acquire data of the thin-film pressure sensor;
E. constant temperature thermal explosion: in an initial state, the reaction crucible is in a sample cooling area; introducing target gas into the corundum reaction tube and the corundum sleeve, starting to heat a sample heating area, moving the corundum reaction tube and the reaction shell upwards after the temperature reaches a set target temperature until the upper end of the corundum reaction tube is tightly contacted with a second sealing ring in the corundum sleeve, stopping moving, completely placing the reaction crucible in the center of the sample heating area, and starting data acquisition software of a computer to acquire data of the thin-film pressure sensor;
F. temperature programmed pyrolysis: in an initial state, the reaction crucible is in a sample cooling area; introducing inert gas into the corundum reaction tube and the corundum sleeve, moving the corundum reaction tube and the reaction shell upwards until the upper end of the corundum reaction tube is in close contact with a second sealing ring in the corundum sleeve, stopping moving, completely placing the reaction crucible in the center of a sample heating area, starting heating the sample heating area, and simultaneously starting data acquisition software of a computer to acquire data of the thin film pressure sensor;
G. temperature programmed combustion: in an initial state, the reaction crucible is in a sample cooling area; introducing oxidizing gas into the corundum reaction tube and the corundum sleeve, moving the corundum reaction tube and the reaction shell upwards until the upper end of the corundum reaction tube is in close contact with a second sealing ring in the corundum sleeve, stopping moving, completely placing the reaction crucible in the center of a sample heating area, starting heating the sample heating area, and simultaneously starting data acquisition software of a computer to acquire data of the thin film pressure sensor;
and 4, after the experiment is finished, stopping the data acquisition software of the computer, moving the corundum reaction tube and the reaction shell downwards to enable the reaction crucible to be positioned in the sample cooling area for rapid cooling, and after the sample is completely cooled, moving the reaction shell downwards and taking out the reaction crucible.
As a further improvement of the scheme, the sample in the step 2 is in a powdery or blocky shape.
As a further improvement of the above scheme, the target gas in the step 3 is one of an inert gas, an oxidizing gas, a reducing gas, a corrosive gas and water vapor.
As a further improvement of the scheme, the temperature reached after heating in the step 3 is less than or equal to 1600 ℃. The invention has the beneficial effects that:
compared with the prior art, the rapid heating-atmosphere variable-weight real-time thermal analysis device and the application thereof provided by the invention have the following advantages:
(1) the pressure sensor replaces a traditional thermobalance, and is combined with a movable furnace body to realize the measurement of macroscopic sample amount (g-kg level), and the mass error caused by the vibration generated by moving a measurement object is avoided, and meanwhile, the corrosion-resistant material is adopted to break through the limitation caused by the easy corrosion of the thermobalance;
(2) the random combination of various combustion atmospheres and extremely fast temperature rise can be realized, and the application range is greatly improved;
(3) the method can accurately measure the thermal burst amount of the sample, and provides an effective way for the research of the later-stage thermal burst behavior.
Drawings
FIG. 1 is a schematic view of a thermal analysis apparatus according to the present invention;
FIG. 2 is a schematic view of a furnace reaction apparatus in the thermal analysis apparatus according to the present invention;
FIG. 3 is a schematic view of a fixing and protecting device, a sample weighing device and an electric control device in the thermal analysis device according to the present invention;
FIG. 4 is the graph of constant temperature drying weight loss of the sludge for long treatment in example 1;
FIG. 5 is pyrite (FeS) of example 22) Programmed heating thermal decomposition weight loss curve chart;
FIG. 6 is a graph of constant temperature combustion weight loss of large-particle coal gangue in example 3;
FIG. 7 is a graph of the constant temperature thermal decrepitation weight change of the coal slurry/limestone (70%/30%) formed material of example 4.
In the figure: 1-furnace body reaction device, 2-fixed protection device, 3-sample weighing device, 4-electric control device, 5-corundum reaction tube, 6-reaction shell, 7-first sealing ring, 8-sample cooling zone, 9-sample heating zone, 10-water inlet tube, 11-water outlet tube, 12-exhaust tube, 13-corundum sleeve, 14-protection shell, 15-air inlet tube, 16-second sealing ring, 17-raised ferromagnetic material, 18-platinum wire lifting rope, 19-thermocouple, 20-reaction crucible, 21-measuring element closed cavity, 22-electromagnet and 23-film pressure sensor.
Detailed Description
The following detailed description of embodiments of the invention is provided in connection with the accompanying drawings,
as shown in figures 1-3, a thermal analysis device capable of realizing extremely rapid temperature rise of a sample, variable atmosphere and real-time weight comprises a furnace body reaction device (1), a fixed protection device (2), a sample weighing device (3) and an electric control device (4), wherein the furnace body reaction device (1) comprises a corundum reaction tube (5) and a reaction shell (6), the corundum reaction tube (5) is embedded in the reaction shell (6) and is provided with a first sealing ring (7) at a radial diminishing position, the lower part of the corundum reaction tube is provided with an exhaust pipe (12), a sample cooling area (8) and a sample heating area (9) are arranged inside the reaction shell (6), the sample cooling area (8) is provided with a water inlet pipe (10) and a water outlet pipe (11), the fixed protection device (2) comprises a corundum sleeve pipe (13) and a protection shell (14), the corundum sleeve pipe (13) is arranged in the protection shell (14), the upper end of the protective shell (14) is protruded, a second sealing ring (16) is arranged in the protective shell (13), an air inlet pipe (15) is arranged on the protective shell (13), the tail end of the air inlet pipe (15) is inserted into the corundum casing pipe (13), the sample weighing device (3) comprises a convex strong magnetic material (17), a platinum wire lifting rope (18), a thermocouple (19) and a reaction crucible (20), one end of the platinum wire lifting rope (18) is connected with the convex strong magnetic material (17), the other end of the platinum wire lifting rope is connected with the reaction crucible (20), the thermocouple (19) is connected with the platinum wire lifting rope (18) and is in contact with the reaction crucible (20) so as to realize real-time measurement of the temperature of the sample, the electric control device (4) comprises a measuring element closed cavity (21), an electromagnet (22) and a film pressure sensor (23), the electromagnet (22) is embedded in the measuring element closed cavity (21), the thin film pressure sensor (23) is tightly attached to the lower surface of the electromagnet (22), wherein the protruding ferromagnetic material (17) is made of a corrosion-resistant soft magnetic material; the outer surface of the electromagnet (22) is coated with corrosion-resistant materials, and an iron core inside the electromagnet cannot be magnetized; the outer surface of the thin film pressure sensor (23) is coated with a corrosion-resistant material.
The application of the rapid temperature rise-atmosphere variable-weight real-time thermal analysis device comprises the following specific operations:
example 1
The power supply of the thermal analyzer is switched on, air is introduced from the air inlet pipe 15, the reaction shell 6 is disassembled, the reaction crucible 20 is exposed to the environment, the electromagnet 22 is switched on, the raised ferromagnetic material 17 is attracted under the action of magnetic force, the raised position presses the film pressure sensor 23, the current pressure can be obtained through potential difference,
by the formula:
G＝1000mg
wherein G is pressure (N), m is mass (G), and G is gravitational acceleration (N/kg).
And calculating the zeroing mass.
Counting in real time through a computer, and peeling the weight returned to zero; 200g of sludge for growth is then placed into the reaction crucible 20, and the attraction of the electromagnet 22 to the protruding ferromagnetic material 17 is indirectly reduced due to the increase in weight, so that the pressure on the thin film pressure sensor 23 is reduced, and the weight recorded by the computer is the initial weight of the sample.
Setting the constant temperature of the sample heating zone 9 to be 105 ℃, moving the reaction shell 6 upwards until contacting with the first sealing ring 7 on the corundum reaction tube 5, and then placing the reaction crucible 20 in the sample cooling zone 8; after the temperature of the sample heating zone 9 reaches a preset temperature, the corundum reaction tube 5 is pushed upwards by using the reaction shell 6 until the uppermost end of the corundum reaction tube 5 is tightly sealed with the second sealing ring 16 in the corundum sleeve, and at the moment, the reaction crucible 20 is arranged in the sample heating zone 9; at this point the experiment was started and the computer count interval was 1 second. And after the experiment is finished, the reaction shell 6 is moved downwards, so that the sample enters the sample cooling area 8 for cooling, after the sample is cooled, the reaction shell 6 is continuously moved downwards, and the sample is taken out. The experimental data are shown in FIG. 4.
Example 2
The power supply of the thermal analyzer is switched on, air is introduced from the air inlet pipe 15, the reaction shell 6 is disassembled, the reaction crucible 20 is exposed to the environment, the electromagnet 22 is switched on, the raised ferromagnetic material 17 is attracted under the action of magnetic force, the raised position presses the film pressure sensor 23, the current pressure can be obtained through potential difference,
by the formula:
G＝1000mg
wherein G is pressure (N), m is mass (G), and G is gravitational acceleration (N/kg).
And calculating the zeroing mass.
Counting in real time through a computer, and peeling the weight returned to zero; then 50g of pyrite (FeS) was charged into the reaction crucible 202) At this time, the attraction of the electromagnet 22 to the protruding ferromagnetic material 17 is indirectly reduced due to the increase of the weight, so that the compression to the film pressure sensor 23 is reduced, and the weight recorded by the computer is the initial weight of the sample.
And moving the reaction shell 6 upwards until the reaction shell 6 pushes the upper end of the corundum reaction tube 5 to be tightly sealed with the second sealing ring 16 in the corundum sleeve, placing the reaction crucible 20 in the sample heating zone 9, setting the heating rate to be 10 ℃/min, starting the experiment after the target temperature is 900 ℃, and counting the interval by a computer to be 1 second. And after the experiment is finished, the reaction shell 6 is moved downwards, so that the sample enters the sample cooling area 8 to be cooled, after the sample is cooled, the reaction shell 6 is continuously moved downwards, and the sample is taken out. The experimental data are shown in FIG. 5.
Example 3
The power supply of the thermal analyzer is switched on, and the gas distribution (21 percent O) is introduced from the gas inlet pipe 152+79％CO2) The reaction shell 6 is detached, the reaction crucible 20 is exposed to the environment, the electromagnet 22 is turned on, the protruding ferromagnetic material 17 is attracted by the action of the magnetic force, the protruding position of the protruding ferromagnetic material is pressed against the film pressure sensor 23, the current pressure can be obtained by the potential difference,
by the formula:
G＝1000mg
wherein G is pressure (N), m is mass (G), and G is gravitational acceleration (N/kg).
And calculating the zeroing mass.
Counting in real time through a computer, and peeling the weight returned to zero; 200g of large-particle coal gangue is put into the reaction crucible 20, the attraction of the electromagnet 22 to the convex type strong magnetic material 17 is indirectly reduced due to the increase of the weight, so that the compression to the film pressure sensor 23 is reduced, and the weight recorded by a computer is the initial weight of the sample.
Setting the constant temperature of the sample heating zone 9 to 800 ℃, moving the reaction shell 6 upwards until contacting the first sealing ring 7 on the corundum reaction tube 5, and then placing the reaction crucible 20 in the sample cooling zone 8; after the temperature of the sample heating zone 9 reaches a preset temperature, the corundum reaction tube 5 is pushed upwards by using the reaction shell 6 until the uppermost end of the corundum reaction tube 5 is tightly sealed with the second sealing ring 16 in the corundum sleeve, and at the moment, the reaction crucible 20 is arranged in the sample heating zone 9; at this point the experiment was started and the computer count interval was 1 second. And after the experiment is finished, the reaction shell 6 is moved downwards, so that the sample enters the sample cooling area 8 for cooling, after the sample is cooled, the reaction shell 6 is continuously moved downwards, and the sample is taken out. The experimental data are shown in FIG. 6.
Example 4
The power supply of the thermal analyzer is switched on, and inert gas N is introduced from the gas inlet pipe 152The reaction shell 6 is detached, the reaction crucible 20 is exposed to the environment, the electromagnet 22 is turned on, the protruding ferromagnetic material 17 is attracted by the action of the magnetic force, the protruding position of the protruding ferromagnetic material is pressed against the film pressure sensor 23, the current pressure can be obtained by the potential difference,
by the formula:
G＝1000mg
wherein G is pressure (N), m is mass (G), and G is gravitational acceleration (N/kg).
And calculating the zeroing mass.
Counting in real time through a computer, and peeling the weight returned to zero; then 100g of cold-press molding material (70g of coal slurry +30g of limestone) is put into the reaction crucible 20, at this time, the suction force of the electromagnet 22 to the convex type strong magnetic material 17 is indirectly reduced due to the increase of the weight, so that the compression to the film pressure sensor 23 is reduced, and at this time, the weight recorded by the computer is the initial weight of the sample.
Setting the constant temperature of the sample heating zone 9 to 800 ℃, moving the reaction shell 6 upwards until contacting the first sealing ring 7 on the corundum reaction tube 5, and then placing the reaction crucible 20 in the sample cooling zone 8; after the temperature of the sample heating zone 9 reaches a preset temperature, the corundum reaction tube 5 is pushed upwards by using the reaction shell 6 until the uppermost end of the corundum reaction tube 5 is tightly sealed with the second sealing ring 16 in the corundum sleeve, and at the moment, the reaction crucible 20 is arranged in the sample heating zone 9; at this point the experiment was started and the computer count interval was 1 second. And after the experiment is finished, the reaction shell 6 is moved downwards, so that the sample enters the sample cooling area 8 for cooling, after the sample is cooled, the reaction shell 6 is continuously moved downwards, and the sample is taken out. The experimental data are shown in FIG. 7.
The above embodiments are not limited to the technical solutions of the embodiments themselves, and the embodiments may be combined with each other into a new embodiment. The above embodiments are only for illustrating the technical solutions of the present invention and are not limited thereto, and any modification or equivalent replacement without departing from the spirit and scope of the present invention should be covered within the technical solutions of the present invention.
Claims (8)
1. A rapid temperature rise-atmosphere variable-weight real-time thermal analysis device is characterized in that: comprises a furnace body reaction device (1), a fixed protection device (2), a sample weighing device (3) and an electric control device (4), wherein the furnace body reaction device (1) comprises a corundum reaction tube (5) and a reaction shell (6), the corundum reaction tube (5) is embedded in the reaction shell (6) and is provided with a first sealing ring (7) at a radial diminishing position, the lower part of the corundum reaction tube is provided with an exhaust pipe (12), a sample cooling area (8) and a sample heating area (9) are arranged inside the reaction shell (6), the sample cooling area (8) is provided with a water inlet pipe (10) and a water outlet pipe (11), the fixed protection device (2) comprises a corundum sleeve (13) and a protection shell (14), the corundum sleeve (13) is arranged in the protection shell (14), the upper end of the corundum sleeve exceeds the protection shell (14), and the inner part of the corundum sleeve is provided with a second, an air inlet pipe (15) is arranged on the protective shell (13), the tail end of the air inlet pipe (15) is inserted into the corundum sleeve (13), the sample weighing device (3) comprises a convex ferromagnetic material (17), a platinum wire lifting rope (18), a thermocouple (19) and a reaction crucible (20), one end of the platinum wire lifting rope (18) is connected with the convex type ferromagnetic material (17), the other end is connected with the reaction crucible (20), the thermocouple (19) is connected with the platinum wire lifting rope (18) and is contacted with the reaction crucible (20), so as to realize the real-time measurement of the temperature of the sample, the electric control device (4) comprises a measuring element closed cavity (21), an electromagnet (22) and a film pressure sensor (23), the electromagnet (22) is embedded in the closed cavity (21) of the measuring element, and the film pressure sensor (23) is tightly attached to the lower surface of the electromagnet (22).
2. The rapid temperature rise-atmosphere variable-weight real-time thermal analysis device according to claim 1, wherein: the protruding type ferromagnetic material (17) is made of corrosion-resistant soft magnetic material.
3. The rapid temperature rise-atmosphere variable-weight real-time thermal analysis device according to claim 1, wherein: the outer surface of the electromagnet (22) is wrapped with corrosion-resistant materials, and the internal iron core cannot be magnetized.
4. The rapid temperature rise-atmosphere variable-weight real-time thermal analysis device according to claim 1, wherein: the outer surface of the thin film pressure sensor (23) is coated with a corrosion-resistant material.
5. The application of the rapid temperature rise-atmosphere variable-weight real-time thermal analysis device is characterized in that: the method comprises the following steps:
step 1, an electromagnet (22) and a film pressure sensor (23) are started, the electromagnet (22) attracts a protruding strong magnetic material (17) to press the film pressure sensor (23), and zero clearing is achieved;
step 2, putting 1 g-1000 g of sample into a reaction crucible (20), moving a reaction shell (6) upwards until the sample contacts a first sealing ring (7) outside a corundum reaction tube (5), and finishing sealing;
step 3, start thermal conversion or thermal decrepitation experiment:
A. and (3) drying at constant temperature: in the initial state, the reaction crucible (20) is in the sample cooling zone (8); introducing air into the corundum reaction tube (5) and the corundum sleeve (13), starting to heat the sample heating zone (9), moving the corundum reaction tube (5) and the reaction shell (6) upwards after the temperature reaches a set drying temperature until the upper end of the corundum reaction tube (5) is tightly contacted with a second sealing ring (16) in the corundum sleeve (13), stopping moving, completely placing the reaction crucible (20) at the center of the sample heating zone (9), and starting data acquisition software of a computer to acquire data of a thin film pressure sensor (23);
B. constant-temperature pyrolysis: in the initial state, the reaction crucible (20) is in the sample cooling zone (8); introducing inert gas or reducing gas into the corundum reaction tube (5) and the corundum sleeve (13), starting to heat the sample heating area (9), moving the corundum reaction tube (5) and the reaction shell (6) upwards after the temperature reaches a set pyrolysis temperature until the upper end of the corundum reaction tube (5) is in close contact with a second sealing ring (16) in the corundum sleeve (13), stopping moving, completely placing the reaction crucible (20) at the center of the sample heating area (9), and starting data acquisition software of a computer to acquire data of a film pressure sensor (23);
C. constant temperature combustion: in the initial state, the reaction crucible (20) is in the sample cooling zone (8); introducing oxidizing gas into the corundum reaction tube (5) and the corundum sleeve (13), starting to heat the sample heating zone (9), moving the corundum reaction tube (5) and the reaction shell (6) upwards after the temperature reaches a set combustion temperature until the upper end of the corundum reaction tube (5) is in close contact with a second sealing ring (16) in the corundum sleeve (13), stopping moving, completely placing the reaction crucible (20) at the center of the sample heating zone (9), and starting data acquisition software of a computer to acquire data of a thin film pressure sensor (23);
D. constant temperature gasification: in the initial state, the reaction crucible (20) is in the sample cooling zone (8); introducing a gasifying agent into the corundum reaction tube (5) and the corundum sleeve (13), starting to heat the sample heating zone (9), moving the corundum reaction tube (5) and the reaction shell (6) upwards after the temperature reaches a set gasifying temperature until the upper end of the corundum reaction tube (5) is tightly contacted with a second sealing ring (16) in the corundum sleeve (13), stopping moving, completely placing the reaction crucible (20) at the center of the sample heating zone (9), and starting data acquisition software of a computer to acquire data of the thin film pressure sensor (23);
E. constant temperature thermal explosion: in the initial state, the reaction crucible (20) is in the sample cooling zone (8); introducing target gas into the corundum reaction tube (5) and the corundum sleeve (13), starting to heat the sample heating zone (9), moving the corundum reaction tube (5) and the reaction shell (6) upwards after the temperature reaches a set target temperature until the upper end of the corundum reaction tube (5) is tightly contacted with a second sealing ring (16) in the corundum sleeve (13), stopping moving, completely placing the reaction crucible (20) at the center of the sample heating zone (9), and starting data acquisition software of a computer to acquire data of a thin film pressure sensor (23);
F. temperature programmed pyrolysis: in the initial state, the reaction crucible (20) is in the sample cooling zone (8); introducing inert gas into the corundum reaction tube (5) and the corundum sleeve (13), moving the corundum reaction tube (5) and the reaction shell (6) upwards until the upper end of the corundum reaction tube (5) is tightly contacted with a second sealing ring (16) in the corundum sleeve (13), stopping moving, completely placing the reaction crucible (20) in the center of the sample heating area (9), starting to heat the sample heating area (9), and simultaneously starting data acquisition software of a computer to acquire data of the thin film pressure sensor (23);
G. temperature programmed combustion: in the initial state, the reaction crucible (20) is in the sample cooling zone (8); introducing oxidizing gas into the corundum reaction tube (5) and the corundum sleeve (13), moving the corundum reaction tube (5) and the reaction shell (6) upwards until the upper end of the corundum reaction tube (5) is tightly contacted with a second sealing ring (16) in the corundum sleeve (13), stopping moving, completely placing the reaction crucible (20) in the center of the sample heating area (9), starting to heat the sample heating area (9), and simultaneously starting data acquisition software of a computer to acquire data of the thin film pressure sensor (23);
and 4, after the experiment is finished, stopping the data acquisition software of the computer, moving the corundum reaction tube (5) and the reaction shell (6) downwards to enable the reaction crucible (20) to be positioned in the sample cooling area (8) for rapid cooling, and after the sample is completely cooled, moving the reaction shell (6) downwards to take out the reaction crucible (20).
6. The use of the rapid temperature rise-atmosphere variable-weight real-time thermal analysis device according to claim 5, wherein: the sample in the step 2 is in a powdery or blocky form.
7. The use of the rapid temperature rise-atmosphere variable-weight real-time thermal analysis device according to claim 5, wherein: the target gas in step 3 is one of inert gas, oxidizing gas, reducing gas, corrosive gas and water vapor.
8. The use of the rapid temperature rise-atmosphere variable-weight real-time thermal analysis device according to claim 5, wherein: the temperature reached after heating in the step 3 is less than or equal to 1600 ℃.
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