Thermogravimetric analysis equipment as well as use method and application thereof

Abstract

The invention relates to the technical field of thermogravimetric analysis equipment, in particular to thermogravimetric analysis equipment and a using method and application thereof. The thermogravimetric analysis equipment comprises a weighing system, a furnace body system and a driving system, the furnace body system comprises a sealed furnace tube and an air inlet mechanism for supplying air to the sealed furnace tube; an inner cavity of the sealed furnace tube sequentially comprises a first furnace area and a second furnace area which are communicated with each other from front to back, and a bin door is arranged above the first furnace area. A gas inlet pipe of the gas inlet mechanism is communicated with a gas path of the second furnace area; the tail end of a cantilever of the weighing system horizontally penetrates into an inner cavity of the sealed furnace tube from the front end of the sealed furnace tube, and the cantilever is in sliding connection with the sealed furnace tube through a sealed sliding connection mechanism. The thermogravimetric analysis equipment can realize instantaneous heating temperature rise in the furnace chamber from room temperature to set temperature, has good sample weighing accuracy, can effectively adapt to various products and product use scenes, and is high in applicability and universality.

Description

Technical Field

[0001] The present application relates to the technical field of thermogravimetric analysis equipment, and in particular to a thermogravimetric analysis equipment and a method for using and applying the same. Background Art

[0002] Thermogravimetric analysis refers to the determination of the relationship between the mass of a substance and temperature (or time) under programmed temperature control. When the substance being measured sublimates, vaporizes, decomposes gas or loses crystal water during heating, the mass of the substance being measured will change. By analyzing the obtained thermogravimetric curve (TG curve) and its derivative curve (DTG curve), the mass change and rate of change of the substance can be accurately analyzed, and the relevant characteristics of the sample material under study can be obtained.

[0003] Since existing thermogravimetric analyzers use furnace radiation heating, most existing thermogravimetric analyzers measure a small mass of the sample, so the weight sensor has high requirements for measurement accuracy, sensitivity, stability, and anti-interference. At the same time, existing thermogravimetric analyzers cannot provide test conditions such as high heating rates (such as greater than 200℃ / min) and high-temperature oxygen-free environments.

[0004] At present, many existing thermogravimetric analyzers move the weighing device (usually including weighing sensing mechanism, cantilever and container and other components) into the furnace chamber by moving. This container movement method is not conducive to accurate weighing of samples, especially when the mass of the tested sample is small. Such a design affects the accuracy of the test. In order to avoid the movement of the weighing device, a fixed weighing device is used. After the sample is loaded, there is no need to move the weighing device. Instead, the chamber door is directly closed to heat the furnace chamber where the sample is located. The heating method and process of this type of equipment is also from low temperature to high temperature. Some materials (such as ceramic fiber materials) experience instantaneous high temperature or immediate high temperature environment in actual production and use environments. The defects of the above-mentioned thermogravimetric analyzer result in its heating environment and process being unable to accurately simulate the actual application environment of these materials, and thus unable to accurately simulate the mass change and rate of change in the actual application environment of these materials, making it difficult to accurately understand the relevant characteristics of the sample material.

[0005] The Chinese patent application with publication number CN CN112611671A discloses a multifunctional visual thermogravimetric analysis device and method for experiments, in which the moving device and the weighing device still move relative to each other and are hard-linked, which will affect the weighing accuracy.

[0006] The Chinese patent application with publication number CN108007809A discloses a fast-heating wide-range thermogravimetric analyzer, whose heating speed is still from low temperature to high temperature, and cannot achieve a jump from room temperature to high temperature directly. The heating process of the thermogravimetric analyzer from low temperature to high temperature is far from the actual production of ceramic fiber materials, and the immediate high temperature environment in the long tunnel industrial kiln. The heating of the thermogravimetric analyzer cannot simulate the ambient temperature during actual production. Summary of the invention

[0007] In order to solve the deficiencies of the prior art mentioned in the above background technology, the present application provides a thermogravimetric analysis device, and its technical solution is as follows: The thermogravimetric analysis equipment provided in the present application includes a weighing system and a furnace system; the furnace system includes a sealed furnace tube and an air intake mechanism for supplying air to the sealed furnace tube; the inner cavity of the sealed furnace tube includes, from front to back, a first furnace zone and a second furnace zone that are interconnected, and a warehouse door is provided above the first furnace zone; the air intake pipe of the air intake mechanism is connected to the gas path of the second furnace zone, so that the gas enters the second furnace zone through the air intake pipe and is discharged from the exhaust port on the sealed furnace tube; the weighing system includes a weighing sensing mechanism and a sealed sliding connection mechanism; the weighing sensing mechanism includes a cantilever with a sample container at the tail end and a weighing sensing device for sensing the weight of the sample container; the tail end of the cantilever is horizontally inserted into the inner cavity of the sealed furnace tube from the front end thereof, and the cantilever is slidably connected to the sealed furnace tube through the sealed sliding connection mechanism, and the furnace system moves forward and backward so that the weighing sensing mechanism and the furnace system can move forward and backward relative to each other, so that the tail end of the cantilever can be alternately located in the first furnace zone and the second furnace zone back and forth.

[0008] In some embodiments, the sealing sliding connection mechanism includes a sealing flange, a piston, and a connecting piece for connecting the sealing flange and the piston; the cantilever is detachably fixedly connected to the sealing flange; a sealing cavity adapted to the piston is provided on the outer periphery of the sealed furnace tube in the first furnace zone, and the piston is slidingly arranged inside the sealing cavity so that the piston and the furnace body system can move forward and backward relative to each other, thereby driving the tail end of the cantilever and the furnace body system to move forward and backward relative to each other.

[0009] In some embodiments, the thermogravimetric analysis apparatus further comprises a driving system for driving the furnace system to move forward and backward.

[0010] In some embodiments, a liquid inlet and a liquid outlet connected to the sealed cavity are provided on the sealed furnace tube, so that the cooling lubricating liquid can flow into the sealed cavity through the liquid inlet and flow out from the liquid outlet.

[0011] In some embodiments, the connecting member is a connecting rod; a first through hole for inserting a cantilever and a second through hole for inserting a connecting rod are provided at the front end of the sealed furnace tube; the tail end of the cantilever is horizontally inserted into the inner cavity of the sealed furnace tube through the first through hole; the head end of the connecting rod is connected to the sealing flange, and the tail end of the connecting rod is horizontally inserted into the sealed cavity through the second through hole and fixedly connected to the piston; wherein, a leakage-proof sealing structure is provided at the first through hole and the second through hole.

[0012] In some embodiments, the air intake mechanism includes an air intake pipe and a gas heating device for heating the gas; the air inlet of the air intake pipe is connected to the gas circuit of the gas outlet end of the gas heating device, and its air outlet is connected to the gas circuit of the second furnace zone, so that the gas heated by the gas heating device can flow into the second furnace zone through the air intake pipe, and be discharged through the exhaust port on the sealed furnace pipe.

[0013] In some embodiments, the air intake mechanism includes a plurality of air intake pipes, and the air outlets of the plurality of air intake pipes are evenly distributed on the periphery of the second furnace zone; In some embodiments, the furnace system further includes a heat preservation mechanism; the heat preservation mechanism includes a heat preservation layer sleeved outside the sealed furnace tube and a heat preservation heating device for heating the heat preservation layer; In some embodiments, an exhaust pipe is provided on the exhaust port of the sealed furnace tube, and an exhaust gas treatment system is provided at the gas outlet of the exhaust pipe.

[0014] In some embodiments, a control system is also included; the control system includes a controller and a temperature sensing element for sensing the temperature in the second furnace zone; the weighing sensing mechanism, the temperature sensing element, the heat preservation and heating device, and the gas heating device are all electrically connected to the controller.

[0015] In some embodiments, the sample container is a hollow crucible; In some embodiments, the sample container is a crucible made of a high temperature resistant material; In some embodiments, the air inlet pipe and the exhaust pipe are made of high temperature resistant material.

[0016] The present application also provides a method for using the thermogravimetric analysis device as described above, which comprises the following steps: The driving system drives the furnace system as a whole to move backward, so that the sample container is located in the first furnace area in the sealed furnace tube, and then the sample is added into the sample container; The air intake mechanism delivers the heated gas to the second furnace zone in the sealed furnace tube, so that the temperature of the second furnace zone reaches a predetermined value; the drive system drives the furnace system as a whole to move forward, so that the sample container filled with the sample is located in the second furnace zone for detection and analysis; After the test and analysis is completed, the gas in the sealed furnace tube is discharged through the exhaust port to cool the inner cavity of the sealed furnace tube; then the driving system drives the furnace system as a whole to move backward, so that the sample container is located in the first furnace area in the sealed furnace tube, and finally the tested sample is taken out.

[0017] The present application also provides an application of the thermogravimetric analysis device as described above in detecting concrete materials and high-temperature ceramic fiber materials of different gradations.

[0018] Based on the above, compared with the prior art, the thermogravimetric analysis device provided by the present application has the following beneficial effects: The thermogravimetric analysis equipment provided by the present application can realize instantaneous heating and temperature rise from room temperature to a predetermined temperature in the furnace chamber, while having good sample weighing accuracy. Therefore, it can accurately simulate the ambient temperature of the actual industrial production of the product, thereby realizing the actual simulation of the industrial production line, and is particularly suitable for products whose actual application environment is instantaneous high temperature. In summary, the thermogravimetric analysis equipment provided by the present application can adapt to the simulation of a variety of ambient temperature conditions, effectively adapt to a variety of products and product usage scenarios, and has strong applicability and versatility.

[0019] Other features and beneficial effects of the present application will be described in the subsequent description, and partly become apparent from the description, or understood by practicing the present application. The purpose and other beneficial effects of the present application can be realized and obtained by the structures specifically pointed out in the description, claims and drawings. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the following is a brief introduction to the drawings required for use in the embodiments or the description of the prior art. Obviously, the drawings described below are some embodiments of the present application. For ordinary technicians in this field, other drawings can be obtained based on these drawings without creative work. The positional relationships described in the drawings in the following description are based on the directions in which the components are drawn in the diagrams, unless otherwise specified.

[0021] Figure 1 A schematic diagram of the structure of a thermogravimetric analysis device provided in one embodiment of the present application Figure 1 ; Figure 2 A schematic diagram of the structure of a thermogravimetric analysis device provided in one embodiment of the present application Figure 2 ; Figure 3 Schematic diagram of the internal structure of a thermogravimetric analysis device provided in one embodiment of the present application Figure 1 ; Figure 4 Schematic diagram of the internal structure of a thermogravimetric analysis device provided in one embodiment of the present application Figure 2 ; Figure 5 Schematic diagram of the internal structure of a thermogravimetric analysis device provided in one embodiment of the present application Figure 3 ; Figure 6 A schematic diagram of the internal structure of a furnace system in a thermogravimetric analysis device provided in one embodiment of the present application; Figure 7 A schematic diagram of the structure of a weighing system in a thermogravimetric analysis device provided in an embodiment of the present application Figure 1 ; Figure 8 A schematic diagram of the structure of a weighing sensing mechanism in a thermogravimetric analysis device provided in one embodiment of the present application; Fig. 9 A schematic diagram of the structure of a sealed sliding connection mechanism in a thermogravimetric analysis device provided in one embodiment of the present application; Fig.10 A schematic diagram of the structure of the front end of the sealed furnace tube in the thermogravimetric analysis device provided in one embodiment of the present application; Fig.11 A schematic diagram of the structure of a weighing system (without a sample container installed) in a thermogravimetric analysis device provided in an embodiment of the present application Figure 2 .

[0022] Reference numerals: 20, cooling lubricant; 100, weighing system; 200, furnace system; 300, drive system; 400, control system; 500, exhaust gas treatment system; 110, weighing sensing mechanism; 120, sealing sliding connection mechanism; 111, weighing sensing device; 112, cantilever; 113, sample container; 121, sealing flange; 122, connector; 123, piston; 210, sealed furnace tube; 220, inlet Gas mechanism; 230, heat preservation mechanism; 240, warehouse door; 211, first furnace zone; 212, second furnace zone; 213, exhaust pipe; 2111, sealed cavity; 2112, first through hole; 2113, second through hole; 2114, liquid inlet; 2115, liquid outlet; 221, gas heating device; 222, air inlet pipe; 231, heat preservation heating device; 232, heat preservation layer; 410, controller; 420, temperature sensing component. DETAILED DESCRIPTION

[0023] In order to make the purpose, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application will be clearly and completely described below in conjunction with the drawings in the embodiments of the present application. Obviously, the described embodiments are part of the embodiments of the present application, not all of the embodiments; the technical features designed in different implementation modes of the present application described below can be combined with each other as long as they do not conflict with each other; based on the embodiments in the present application, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of this application.

[0024] In the description of this application, it should be noted that all terms (including technical terms and scientific terms) used in this application have the same meanings as those generally understood by ordinary technicians in the field to which this application belongs, and cannot be understood as limitations on this application; it should be further understood that the terms used in this application should be understood to have meanings consistent with the meanings of these terms in the context of this specification and in the relevant fields, and should not be understood in an idealized or overly formal sense, unless explicitly defined in this application.

[0025] This application provides Figure 1-11 Thermogravimetric analysis equipment shown in the embodiment: The thermogravimetric analysis device comprises a weighing system 100, a furnace system 200, and a driving system 300; the furnace system 200 comprises a sealed furnace tube 210 and an air intake mechanism 220 for supplying air to the sealed furnace tube 210; the inner cavity of the sealed furnace tube 210 comprises, from front to back, a first furnace zone 211 and a second furnace zone 212 which are interconnected, and a door 240 is arranged above the first furnace zone 211; an air intake pipe 222 of the air intake mechanism 220 is in communication with the gas path of the second furnace zone 212, so that the gas enters the second furnace zone 212 through the air intake pipe 222 and is discharged from the exhaust port on the sealed furnace tube 210; the weighing system 100 comprises a weighing sensing mechanism 1 10. Sealed sliding connection mechanism 120; the weighing sensing mechanism 110 includes a cantilever 112 with a sample container 113 at the tail end, and a weighing sensing device 111 for sensing the weight of the sample container 113; the tail end of the cantilever 112 is horizontally inserted into the inner cavity of the sealed furnace tube 210 from the front end thereof, and the cantilever 112 is slidably connected to the sealed furnace tube 210 through the sealed sliding connection mechanism 120, and the driving system 300 can drive the furnace system 200 to move forward and backward, so that the weighing sensing mechanism 110 and the furnace system 200 can move forward and backward relative to each other, so that the tail end of the cantilever 112 can be alternately located in the first furnace area 211 and the second furnace area 212 back and forth. Among them, the warehouse door 240 is convenient for loading samples in the first furnace area 211.

[0026] When using this device, the process is: (1) If Figure 4 As shown, the driving system 300 drives the furnace system 200 to move backward as a whole, and the positions of the sealed sliding connection mechanism 120 and the sealed furnace tube 210 move relative to each other, thereby driving the cantilever 112 and the sealed furnace tube 210 to move relative to each other, so that the sample container 113 is located in the first furnace area 211 in the sealed furnace tube 210.

[0027] (2) Loading samples: opening the chamber door 240, adding samples to the sample container 113, and closing the chamber door 240; (3) Heating and detection analysis of the inner cavity of the sealed furnace tube 210: like Figure 5As shown, the air intake mechanism 220 delivers the heated gas to the second furnace zone 212 in the sealed furnace tube 210, so that the temperature of the second furnace zone 212 is quickly increased to a predetermined value; the driving system 300 drives the furnace system 200 to move forward as a whole, and similarly, drives the cantilever 112 and the sealed furnace tube 210 to move relative to each other, so that the sample container 113 filled with the sample is located in the second furnace zone 212 for detection and analysis; The weighing sensing mechanism 110 will weigh and record the initial weight of the sample, and will sense and record the sample weight in real time during the detection and analysis process to form analysis data and corresponding curves.

[0028] (4) Exhaust cooling, take out the sample after testing: After the detection and analysis is completed, the gas in the sealed furnace tube 210 is discharged through the exhaust port to cool the inner cavity of the sealed furnace tube 210; then the driving system 300 drives the furnace system 200 to move backward as a whole, so that the sample container 113 is relocated in the first furnace area 211 in the sealed furnace tube 210, and finally the tested sample is taken out.

[0029] Optionally, the sealing sliding connection mechanism 120 includes a sealing flange 121, a piston 123, and a connecting piece 122 for connecting the sealing flange 121 and the piston 123; the cantilever 112 is detachably fixedly connected to the sealing flange 121; the sealed furnace tube 210 is provided with a sealing cavity 2111 adapted to the piston 123 on the outer periphery of the first furnace zone 211, and the piston 123 is slidably arranged inside the sealing cavity 2111, so that the piston 123 and the furnace body system 200 can move forward and backward relative to each other, driving the tail end of the cantilever 112 and the furnace body system 200 to move forward and backward relative to each other.

[0030] Optionally, the connecting member 122 is a connecting rod; a first through hole 2112 for inserting the cantilever 112 and a second through hole 2113 for inserting the connecting rod are provided at the front end of the sealed furnace tube 210; the tail end of the cantilever 112 is horizontally penetrated into the inner cavity of the sealed furnace tube 210 through the first through hole 2112; the head end of the connecting rod is connected to the sealing flange 121, and the tail end of the connecting rod is horizontally penetrated into the sealed cavity 2111 through the second through hole 2113, and is fixedly connected to the piston 123; wherein, a leakage-proof sealing structure is provided at the first through hole 2112 and the second through hole 2113.

[0031] like Figure 4-9 As shown, the sealed sliding connection mechanism 120 and the sealed furnace tube 210 are matched with the above structural design. When in use, the furnace system 200 moves forward and backward, and the inner wall of the sealed cavity 2111 slides forward and backward on the outer periphery of the piston 123, so that the relative position of the piston 123 and the sealed cavity 2111 moves forward and backward, so that the sample container 113 at the tail end of the cantilever 112 is alternately located in the first furnace area 211 and the second furnace area 212 back and forth.

[0032] The sealed sliding connection mechanism 120 and the sealed furnace tube 210 are designed as above, so that the sliding connection between the two has good stability, and the sealed furnace tube 210 has good sealing performance by designing a leak-proof sealing structure (not shown in the figure) at the first through hole 2112 and the second through hole 2113.

[0033] Optionally, when the sample container 113 at the rear end of the cantilever 112 is located in the second furnace zone 212, the sealing flange 121 fits against the end surface of the front end of the sealed furnace tube 210. This design can make the sealing of the sealed furnace tube 210 better during detection and analysis, and the relative stability of the sealed furnace tube 210 and the cantilever 112 is better.

[0034] Optionally, the sealed furnace tube 210 is provided with a liquid inlet 2114 and a liquid outlet 2115 which are in communication with the sealed cavity 2111 , so that the cooling lubricating liquid 20 can flow into the sealed cavity 2111 through the liquid inlet 2114 and flow out from the liquid outlet 2115 .

[0035] With the above design, when in use, the cooling lubricating liquid 20 can circulate from the liquid inlet 2114 into the sealed cavity 2111 and flow out from the liquid outlet 2115, thereby performing circulating cooling on the periphery of the first furnace zone 211, which is beneficial to protecting the weighing sensing mechanism 110 (especially the weighing sensing device 111 and other components therein), and the wall surface of the sealed cavity 2111 moves around the piston 123, and the cooling lubricating liquid 20 can also have a certain lubricating effect on the relative movement of the two.

[0036] Optionally, a transmission rod is provided at the rear end of the sealed furnace tube 210 , and the transmission rod is in transmission connection with the driving system 300 , so that the driving system 300 drives the transmission rod to drive the sealed furnace tube 210 to move forward and backward.

[0037] It should be noted that: The driving system 300 used is a reciprocating linear motion device, including but not limited to a pneumatic cylinder, a hydraulic cylinder, a motor, etc., which can be adaptively selected by those skilled in the art.

[0038] In this embodiment, the piston 123 and the sealing chamber 2111 adapted to the piston 123 adopt the following structural shapes: Figure 10-11 According to the above design concept, the piston 123 and the sealing chamber 2111 are adapted in shape and size so that the piston 123 and the sealing chamber 2111 can slide relative to each other stably, and the shape design is not limited to the embodiment.

[0039] In this embodiment, the sealed furnace tube 210 is a cylindrical structure, and the first furnace zone 211 and the second furnace zone 212 are cylindrical chambers. According to the above design concept, those skilled in the art can adaptively adjust the shapes of the above components.

[0040] Optionally, the air intake mechanism 220 includes an air intake pipe 222 and a gas heating device 221 for heating gas; the air intake of the air intake pipe 222 is connected to the gas path of the gas outlet end of the gas heating device 221, and the air outlet is connected to the gas path of the second furnace zone 212, so that the gas heated by the gas heating device 221 can flow into the second furnace zone 212 through the air intake pipe 222 and be discharged through the exhaust port on the sealed furnace tube 210. Optionally, the air intake mechanism 220 includes a plurality of air intake pipes 222, and the air outlets of the plurality of air intake pipes 222 are evenly distributed on the periphery of the second furnace zone 212.

[0041] When in use, the gas heated by the gas heating device 221 can flow into the second furnace zone 212 through the air inlet pipe 222, so that the second furnace zone 212 can be quickly heated up. In addition, the multi-directionally arranged air outlets make the temperatures of various blocks of the second furnace zone 212 more uniform. The above-mentioned air inlet mechanism 220 design can achieve instantaneous heating and heating of the second furnace zone 212 from room temperature to a predetermined temperature, and the heating speed and heating effect are better and more controllable.

[0042] Optionally, the furnace system 200 further includes a heat preservation mechanism 230 ; the heat preservation mechanism 230 includes a heat preservation layer 232 sleeved on the outside of the sealed furnace tube 210 , and a heat preservation heating device 231 for heating the heat preservation layer 232 .

[0043] The sealed furnace tube 210 is insulated by the heat preservation mechanism 230 to improve the temperature stability and controllability of the second furnace zone 212 .

[0044] Optionally, it also includes a control system 400; the control system 400 includes a controller 410 and a temperature sensing component 420 for sensing the temperature in the second furnace zone 212; the weighing sensing mechanism 110, the temperature sensing component 420, the heat preservation and heating device 231, and the gas heating device 221 are all electrically connected to the controller 410.

[0045] The control system 400 can be used to control the detection process more intelligently. For example, the temperature sensing element 420 senses the temperature in the second furnace zone 212 and transmits the signal to the controller 410 for processing. The controller 410 adjusts the power of the heat preservation heating device 231 and the gas heating device 221 according to the temperature information to control the temperature in the second furnace zone 212. Similarly, during the detection and analysis process, the signal sensed by the weighing sensing mechanism 110 is also transmitted to the controller 410 for processing and analysis.

[0046] Optionally, the controller 410 is electrically connected to the driving system 300 to control the operating state of the driving system 300 .

[0047] It should be noted that: The controller 410 is a prior art. For example, a PLC controller 410 can be used. It has a programmable memory for storing programs internally, executing user-oriented instructions such as logical operations, sequential control, timing, counting and arithmetic operations, and controlling various types of machinery or production processes through digital or analog input / output. It is a prior art and the working principle will not be described in detail.

[0048] The weighing sensing mechanism 110, the temperature sensing element 420 (including but not limited to thermocouples, etc.), the heat preservation and heating device 231, the gas heating device 221 and other components are also existing devices. The working principles of the detection, feedback and adjustment processes performed in cooperation with the control system 400 are existing technologies and will not be described again here.

[0049] Optionally, an exhaust pipe 213 is provided on the exhaust port of the sealed furnace tube 210, and an exhaust gas treatment system 500 is provided at the gas outlet of the exhaust pipe 213, so as to perform post-treatment on the exhaust gas.

[0050] Optionally, the sample container 113 is a hollow crucible; The embodiment also optimizes the atmosphere contact scheme for large particle samples, and uses a hollow crucible to cooperate with the above-mentioned air intake mechanism 220, which is suitable for the detection of concrete particle samples with different gradations.

[0051] Optionally, the sample container 113 is a crucible made of a high temperature resistant material.

[0052] It should be noted that: in the specific implementation, a crucible made of high temperature resistant materials including but not limited to graphite, alumina, platinum, etc. can be used. Among them, the graphite crucible has good sealing performance and is the preferred choice.

[0053] Optionally, the air inlet pipe 222 and the exhaust pipe 213 are made of high temperature resistant material.

[0054] It should be noted that: in specific implementation, the air inlet pipe 222 and the exhaust pipe 213 can be made of high-temperature resistant material pipes including but not limited to ceramic pipes, metal pipes, etc., to prevent excessively high gas temperatures from damaging the pipes.

[0055] The present application also provides a method for using the thermogravimetric analysis device as shown in the above embodiment, which comprises the following steps: (1) The lubricating coolant is injected into the sealed cavity 2111. The cooling lubricating liquid 20 flows into the sealed cavity 2111 from the liquid inlet 2114 and flows out from the liquid outlet 2115 for circulation cooling. The driving system 300 drives the furnace system 200 to move backward as a whole, so that the sample container 113 is located in the first furnace zone 211 in the sealed furnace tube 210. The compartment door 240 is opened, and then the sample is added to the sample container 113.

[0056] (2) The control system 400 controls the air intake mechanism 220 so that the air intake mechanism 220 delivers the heated gas to the second furnace zone 212 in the sealed furnace tube 210, so that the temperature of the second furnace zone 212 reaches a predetermined value; the drive system 300 drives the furnace system 200 to move forward as a whole, so that the sample container 113 filled with the sample is located in the second furnace zone 212 for detection and analysis.

[0057] The weighing sensing mechanism 110 will weigh and record the initial weight of the sample, and will sense and record the sample weight in real time during the detection and analysis process to form analysis data and corresponding curves.

[0058] During the detection and analysis process, the temperature of the insulation layer 232 and the atmosphere is controlled by the temperature control design of the control system 400 to adjust the temperature in the second furnace zone 212 .

[0059] (3) After the detection and analysis is completed, the gas in the sealed furnace tube 210 is discharged through the exhaust port to cool the inner cavity of the sealed furnace tube 210; then the driving system 300 drives the furnace system 200 to move backward as a whole, so that the sample container 113 is located in the first furnace area 211 in the sealed furnace tube 210, and finally the tested sample is taken out.

[0060] In addition, in order to verify the effect of the present application, the thermogravimetric analysis equipment of the above embodiment is also used to perform sample detection and analysis, and the verification experiment is as follows: The experimental process, experimental conditions and experimental results of the verification experiment (the equipment used is the thermogravimetric analysis equipment provided in the above embodiment) are as follows: Verification experiment 1 Sample: The cement paste flow test method according to the national standard "Test method for homogeneity of concrete admixtures" GB / T 8077-2023 was used to prepare the cement paste. After curing for 1 day, 0.5 g of sample was taken and ground into fine powder.

[0061] Experimental equipment and experimental process: Using the equipment of the aforementioned embodiment and following the method of using the equipment of the aforementioned embodiment, the sealed furnace tube is moved so that the sample container is located in the first furnace zone. After loading the sample and closing the door, the sealed furnace tube (second furnace zone) is slid as a whole to the front, the relative position of the sample container and the sample is placed in the center of the second furnace zone, and then the temperature is raised for testing.

[0062] The experimental conditions are that the heating rate in the second furnace zone is set to 5°C / min, and the heating reaction is carried out under the condition of protective gas nitrogen and no reaction atmosphere. The experimental results are shown in Table 1, No. 1.

[0063] Comparative experiment 1 Samples: The samples of comparative experiment 1 are consistent with those of verification experiment 1.

[0064] Experimental equipment and experimental process: The existing thermogravimetric analyzer is used, and its weighing device and sample container are designed to be mobile. When in use, the weighing device is removed to load the sample, and then the weighing device (usually including weighing sensing mechanism, cantilever and sample container and other components) is moved into the furnace chamber and the chamber door is closed, and then the furnace chamber is heated up for testing.

[0065] The experimental conditions were consistent with those of the verification experiment 1: the heating rate in the second furnace zone was set at 5°C / min, and the heating reaction was carried out under the condition of protective nitrogen gas and no reaction atmosphere. The experimental results are shown in Table 1, No. 2.

[0066] Verification experiment 2 (the only difference from verification experiment 1 is the sample) Sample: The cement mortar water reduction rate test method of the national standard "Test method for homogeneity of concrete admixtures" GB / T 8077-2023 was used to prepare cement mortar. After curing for 1 day, 0.5g of sample was taken and ground into fine powder.

[0067] Experimental equipment and experimental process: consistent with verification experiment 1. The experimental results are shown in Table 1, No. 3.

[0068] Comparative experiment 2 (the only difference from comparative experiment 1 is the sample) Sample: The cement mortar water reduction rate test method of the national standard "Test method for homogeneity of concrete admixtures" GB / T 8077-2023 was used to prepare cement mortar. After curing for 1 day, 0.5g of sample was taken and ground into fine powder.

[0069] Experimental equipment and experimental process: the same as comparative experiment 1. The experimental results are shown in Table 1, No. 4.

[0070] Verification experiment 3 (sample is ceramic fiber) Sample: Polycarboxylate water reducer was used as the precursor dispersant of ceramic fiber material. After pre-calcining the ceramic fiber in a muffle furnace to remove part of the water, 0.5 g of sample was taken.

[0071] Experimental equipment and experimental process: Move the sealed furnace tube so that the sample container is located in the first furnace area. After loading the sample and closing the door, place the sample in the sample container at the end of the cantilever and close the door. At this time, the container uses a graphite crucible; turn on the gas heating device and pass the heated protective atmosphere argon gas into the second furnace area. At this time, the second furnace body is an oxygen-free environment. Turn on the cooling lubricant and turn on the heat preservation heating device until the temperature in the second furnace area reaches 1000℃.

[0072] Slide the second furnace area to the front as a whole, that is, place the relative position of the sample container and the sample in the center of the second furnace area, and the ceramic fiber is instantly heated to 1000°C. At this time, the weight change of the ceramic fiber during the rapid temperature increase can be accurately recorded to simulate the heating effect of an industrial kiln. The experimental results are shown in Table 1, No. 5.

[0073] Verification experiment 4 (sample is calcium oxide (CaO) powder) Sample: Calcium oxide (CaO) powder dried at 300°C in a muffle furnace, 400 mesh, take 0.5g sample and grind into fine powder.

[0074] Using the equipment of the aforementioned embodiment and following the method of using the equipment of the aforementioned embodiment, the sealed furnace tube is moved so that the sample container is located in the first furnace zone. After loading the sample and closing the door, the sealed furnace tube (second furnace zone) is slid as a whole to the front, the relative position of the sample container and the sample is placed in the center of the second furnace zone, and then the temperature is raised for testing.

[0075] The experimental conditions were as follows: the heating rate in the second furnace zone was set to 5°C / min, with nitrogen as the protective gas and CO as the reaction atmosphere. 2 The experimental results are shown in Table 1, No. 6.

[0076] Table 1

[0077] In summary, the thermogravimetric analysis device provided in the embodiment of the present application has the following design concepts and beneficial effects: This application provides a thermogravimetric analysis device with good sealing, synchronous heating of reaction atmosphere and high heating rate. The basic principle is briefly summarized as follows: When in use, the weighing system is fixed (especially the weighing sensing mechanism, cantilever and the sample container on the cantilever are fixed), and the sample container can be alternately located in two different furnace areas by driving the furnace system to move back and forth relative to the weighing system. First, the sample container is placed in the low-temperature first furnace area for sample loading, and then the reaction gas and protective gas are heated by the gas heating device, and the various positions of the second furnace area are quickly raised to the predetermined temperature and the temperature is uniform through the evenly distributed air inlet design and the control system temperature control design, and the sealed furnace tube is moved to place the sample in the second furnace area, and the subsequent temperature control and heating time control are realized through the controller, that is, its built-in software program, to achieve the purpose of detection and analysis.

[0078] The thermogravimetric analysis device provided in the embodiment of the present application has the following innovative features and beneficial effects: 1. The thermogravimetric analysis equipment is flexible in sample heating scenarios and can adapt to a variety of ambient temperature conditions. It can be used to detect and analyze concrete particles of different gradations and high-temperature ceramic fibers and other products. There is no need to purchase a variety of thermogravimetric analyzers, saving costs; 2. The weighing sensing mechanism of the thermogravimetric analysis equipment is fixed and does not need to be moved during use and is not affected by movement, so the weighing accuracy of the sample is good.

[0079] 3. The air intake mechanism of the thermogravimetric analysis equipment adopts a gas heating device to prevent the cold gas from affecting the main body temperature. It can heat the internal temperature of the furnace body and the protective atmosphere and reaction atmosphere to a predetermined temperature at the same time to avoid the influence of gas temperature difference on the symmetry.

[0080] 4. The thermogravimetric analysis equipment can heat the second furnace zone to a predetermined temperature and achieve instantaneous heating through the air intake mechanism and the temperature control mechanism of the control system. The detection process is not affected by the heating rate.

[0081] 5. The multiple air outlets in the second furnace area of ​​the thermogravimetric analysis equipment are evenly distributed, and a control system temperature control mechanism is provided to achieve uniform and stable air intake to the core heating area, so as to heat the sample evenly and controllably, effectively increase the reaction area of ​​the sample in the furnace area, and make the reaction more uniform.

[0082] In addition, changing different crucibles can adapt to product particles of different sizes (concrete particles, etc.), achieve uniform and rapid sample heating, and effectively eliminate interference. For example, the atmosphere contact scheme for large particle samples is optimized, and the hollow crucible is used to cooperate with the above-mentioned air intake mechanism, which is suitable for the detection of concrete particle samples of different sizes.

[0083] 6. The thermogravimetric analysis equipment uses cooling lubrication medium for circulating cooling in the first furnace area, which can protect the weighing sensing mechanism (such as a balance) and achieve a certain lubrication effect on the movement of the sealed furnace tube.

[0084] 7. The thermogravimetric analysis equipment has a good sealing effect and can realize positive pressure protection and reaction atmosphere reaction condition simulation.

[0085] 8. The thermogravimetric analysis equipment can simulate the existing fiber sintering furnace.

[0086] The thermogravimetric analysis equipment provided by the present application can realize instantaneous heating and temperature rise from room temperature to a predetermined temperature in the furnace chamber, which can more accurately control the reaction temperature and has good sample weighing accuracy. Therefore, it can accurately simulate the ambient temperature of the actual industrial production of the product, thereby realizing the actual simulation of the industrial production line, and is particularly suitable for products whose actual application environment is instantaneous high temperature, such as the detection of ceramic fiber materials. The thermogravimetric analysis equipment provided by the present application can adapt to the simulation of a variety of ambient temperature conditions, effectively adapt to a variety of products and product usage scenarios, and has strong applicability and versatility.

[0087] It should be noted that: Although the present application states that the thermogravimetric analysis equipment provided by the present application is suitable for detecting concrete materials and high-temperature ceramic fiber materials of different gradations, it is not limited to this. It not only has an instantaneous heating function, but can also perform more different heating curves and temperature changes, and the sample heating scenario is flexible.

[0088] In addition, those skilled in the art should understand that, although there are many problems in the prior art, each embodiment or technical solution of the present application can be improved in only one or several aspects, without having to solve all the technical problems listed in the prior art or background technology at the same time. Those skilled in the art should understand that the content not mentioned in a claim should not be used as a limitation on the claim.

[0089] Although the terms such as weighing system, furnace system, drive system, control system, exhaust gas treatment system, etc. are used more frequently in this article, the possibility of using other terms is not excluded. These terms are used only to more conveniently describe and explain the essence of this application; interpreting them as any additional restrictions is contrary to the spirit of this application; the terms "first", "second", etc. (if any) in the description and claims of the embodiments of this application and the above-mentioned drawings are used to distinguish similar objects, and are not necessarily used to describe a specific order or sequence.

[0090] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present application, rather than to limit it. Although the present application has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or replace some or all of the technical features therein with equivalents. However, these modifications or replacements do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present application.

Claims

1. A thermogravimetric analysis device, characterized in that: It comprises a weighing system (100) and a furnace system (200); The furnace system (200) comprises a sealed furnace tube (210) and an air intake mechanism (220) for supplying air to the sealed furnace tube (210); The inner cavity of the sealed furnace tube (210) comprises, from front to back, a first furnace zone (211) and a second furnace zone (212) which are connected to each other, and a door (240) is provided above the first furnace zone (211); the air intake pipe (222) of the air intake mechanism (220) is connected to the gas path of the second furnace zone (212), so that gas enters the second furnace zone (212) through the air intake pipe (222) and is discharged from the exhaust port on the sealed furnace tube (210); The weighing system (100) comprises a weighing sensing mechanism (110) and a sealed sliding connection mechanism (120); the weighing sensing mechanism (110) comprises a cantilever (112) with a sample container (113) at the rear end, and a weighing sensing device (111) for sensing the weight of the sample container (113); The tail end of the cantilever (112) is horizontally inserted into the inner cavity of the sealed furnace tube (210) from the front end thereof, and the cantilever (112) is slidably connected to the sealed furnace tube (210) via a sealed sliding connection mechanism (120). The furnace body system (200) moves forward and backward so that the weighing sensing mechanism (110) and the furnace body system (200) can move forward and backward relative to each other, so that the tail end of the cantilever (112) can be alternately located back and forth in the first furnace area (211) and the second furnace area (212).

2. The thermogravimetric analysis device according to claim 1, characterized in that: The sealing sliding connection mechanism (120) comprises a sealing flange (121), a piston (123), and a connecting piece (122) for connecting the sealing flange (121) and the piston (123); The cantilever (112) is detachably fixedly connected to the sealing flange (121); the sealed furnace tube (210) is provided with a sealing cavity (2111) adapted to the piston (123) on the outer periphery of the first furnace zone (211); the piston (123) is slidably arranged inside the sealing cavity (2111), so that the piston (123) and the furnace body system (200) can move forward and backward relative to each other, thereby driving the rear end of the cantilever (112) and the furnace body system (200) to move forward and backward relative to each other.

3. The thermogravimetric analysis device according to claim 2, characterized in that: The thermogravimetric analysis device further comprises a driving system (300) for driving the furnace system (200) to move forward and backward; And / or, the sealed furnace tube (210) is provided with a liquid inlet (2114) and a liquid outlet (2115) which are in communication with the sealed cavity (2111), so that the cooling lubricating liquid (20) can flow into the sealed cavity (2111) through the liquid inlet (2114) and flow out from the liquid outlet (2115).

4. The thermogravimetric analysis device according to claim 2, characterized in that: The connecting piece (122) is a connecting rod; the front end of the sealed furnace tube (210) is provided with a first through hole (2112) for inserting the cantilever (112) and a second through hole (2113) for inserting the connecting rod; The tail end of the cantilever (112) is horizontally inserted into the inner cavity of the sealed furnace tube (210) through the first through hole (2112); the head end of the connecting rod is connected to the sealing flange (121), and the tail end of the connecting rod is horizontally inserted into the sealed cavity (2111) through the second through hole (2113) and is fixedly connected to the piston (123); Wherein, the first through hole (2112) and the second through hole (2113) are provided with a leakage-proof sealing structure.

5. The thermogravimetric analysis device according to claim 1, characterized in that: The air intake mechanism (220) comprises an air intake pipe (222) and a gas heating device (221) for heating gas; The air inlet of the air inlet pipe (222) is in communication with the air path of the air outlet of the gas heating device (221), and the air outlet is in communication with the air path of the second furnace zone (212), so that the gas heated by the gas heating device (221) can flow into the second furnace zone (212) through the air inlet pipe (222) and be discharged through the exhaust port on the sealed furnace tube (210).

6. The thermogravimetric analysis device according to claim 5, characterized in that: The air intake mechanism (220) comprises a plurality of air intake pipes (222), and the air outlets of the plurality of air intake pipes (222) are evenly distributed on the periphery of the second furnace zone (212); And / or, the furnace system (200) further comprises a heat preservation mechanism (230); the heat preservation mechanism (230) comprises a heat preservation layer (232) sleeved outside the sealed furnace tube (210), and a heat preservation heating device (231) for heating the heat preservation layer (232); And / or, an exhaust pipe (213) is provided on the exhaust port of the sealed furnace tube (210), and an exhaust gas treatment system (500) is provided at the gas outlet of the exhaust pipe (213).

7. The thermogravimetric analysis device according to claim 6, characterized in that: It also includes a control system (400); the control system (400) includes a controller (410) and a temperature sensing element (420) for sensing the temperature in the second furnace zone (212); The weighing sensing mechanism (110), the temperature sensing element (420), the heat preservation and heating device (231), and the gas heating device (221) are all electrically connected to the controller (410).

8. The thermogravimetric analysis device according to claim 6, characterized in that: The sample container (113) is a hollow crucible; And / or, the sample container (113) is a crucible made of a high temperature resistant material; And / or, the air intake pipe (222) and the exhaust pipe (213) are made of high temperature resistant material.

9. A method for using the thermogravimetric analysis device according to any one of claims 1 to 8, characterized in that: The following steps are involved: The driving system (300) drives the furnace system (200) to move backward as a whole, so that the sample container (113) is located in the first furnace zone (211) in the sealed furnace tube (210), and then the sample is added into the sample container (113); The air intake mechanism (220) delivers the heated gas to the second furnace zone (212) in the sealed furnace tube (210), so that the temperature of the second furnace zone (212) reaches a predetermined value; the drive system (300) drives the furnace system (200) to move forward as a whole, so that the sample container (113) filled with the sample is located in the second furnace zone (212) for detection and analysis; After the detection and analysis is completed, the gas in the sealed furnace tube (210) is discharged through the exhaust port to cool the inner cavity of the sealed furnace tube (210); then the drive system (300) drives the furnace system (200) to move backward as a whole, so that the sample container (113) is located in the first furnace area (211) in the sealed furnace tube (210), and finally the detected sample is taken out.

10. Use of the thermogravimetric analysis device according to any one of claims 1 to 8 in detecting concrete materials and high-temperature ceramic fiber materials of different gradations.

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