A thermogravimetric analyzer with online feeding sampling

Abstract

The utility model relates to thermogravimetric analyzer technical field discloses a kind of on-line feeding sampling thermogravimetric analyzer.It include shell, heater and reaction cavity being located in shell, reaction crucible, telescopic bellows, feeder, sampler, lifting mechanism, pressure sensor and manual ball valve etc..Telescopic bellows is connected with reaction cavity by vacuum ball valve, feeder and sampler are detachably connected with telescopic bellows via KF clamp interface, lifting mechanism drives reaction cavity to move up and down, double-seal ring shaft seal design ensures system sealing.The thermogravimetric analyzer can realize on-line feeding and sampling without interrupting experiment, avoid atmosphere interference and sample state distortion, realize temperature sudden change by electric lifting mechanism, combine weighing module and thermocouple real-time monitoring analysis, improve experimental continuity and data accuracy, suitable for catalyst performance research, material synthesis and other need dynamic operation scene.

Description

Technical Field

[0001] This utility model relates to the field of thermogravimetric analyzers, and in particular to a thermogravimetric analyzer with online feeding and sampling. Background Technology

[0002] Thermogravimetric analyzers (TGAs), as core instruments that accurately measure the relationship between the mass of a substance and temperature (or time) under programmed temperature control, are widely used in materials science, chemical engineering, food, and pharmaceuticals. With the increasing demand for TGA technology across industries, higher requirements are being placed on the diversification of instrument functions and the precision of performance. Especially in scenarios such as catalyst performance research and material synthesis, online sample feeding or sampling operations are required during TGA. For example, in catalyst activity testing, different reactants need to be added in real time to observe stage-by-stage activity changes; in material synthesis, samples need to be taken out at specific temperature stages to analyze intermediate products in order to optimize the process. However, the design of existing TGAs is insufficient to meet such dynamic operational needs.

[0003] Most existing thermogravimetric analyzers focus on static thermogravimetric analysis of single samples, and their core shortcomings are as follows: The lack of online feeding capability limits the continuity of experiments. Traditional equipment cannot be used to add materials midway through the experiment after the sample is placed. If it is necessary to study multi-component mixed samples or observe the reaction changes after adding new substances, the experiment must be interrupted, the sample must be reloaded, and the equipment must be restarted. This not only prolongs the experimental cycle, but also introduces systematic errors because it is difficult to unify the starting conditions (such as temperature and atmosphere) for each experiment.

[0004] The online sampling function is missing, and the sample status is distorted and the information is incomplete. If existing technology requires obtaining intermediate samples from a reaction, heating must be stopped and the equipment must be allowed to cool down before sampling. During this process, the environmental conditions such as temperature and pressure of the sample change drastically, which can easily trigger secondary reactions (such as passivation of metal oxide intermediates and structural rearrangement of free radicals due to polymer degradation). This results in the sample state after sampling not matching the actual state in the experiment, making it impossible to accurately deduce the reaction mechanism.

[0005] Poor atmosphere control stability can interfere with the accuracy of analytical results. A few devices attempting online operation failed to solve the sealing problem: during the feeding / sampling process, the inside of the device was connected to the outside, causing leakage of inert atmosphere or infiltration of air and moisture, which triggered unexpected reactions in the sample (such as sample oxidation in oxygen-free experiments or moisture absorption by hygroscopic materials), resulting in false weight loss / weight gain peaks in the thermogravimetric curve.

[0006] Based on this, we propose an online feeding and sampling thermogravimetric analyzer. Utility Model Content

[0007] To address the technical problems mentioned in the background section, this utility model provides an online feeding and sampling thermogravimetric analyzer.

[0008] This utility model is achieved using the following technical solution: an online feeding and sampling thermogravimetric analyzer, characterized in that it includes: The housing; and the heater and reaction chamber disposed within the housing, the heater and reaction chamber being connected to the main body of the equipment via a reaction bellows; The reaction crucible is fixed above the weighing module and located inside the heater and reaction chamber. The telescopic bellows has one end connected to the heater and reaction chamber via a vacuum ball valve, and the other end is equipped with a KF clamp interface. The telescopic bellows is made of stainless steel and is telescopic to accommodate the vertical movement of the heater and reaction chamber.

[0009] The feeder and sampler are detachably connected to the telescopic bellows via KF clamp interfaces; The lifting mechanism is linked to the heater and reaction chamber and is used to drive the heater and reaction chamber to move up and down. The lifting mechanism is electrically driven and can realize the rapid lifting and lowering of the heater and reaction chamber.

[0010] Pressure sensor, used to monitor the pressure inside a telescopic bellows; Manual ball valve, located on the side wall of the telescopic bellows, is used to connect to a vacuum pump or reaction gas source.

[0011] The feeder includes a feed tube and a feed rod. The lower part of the feed tube has a through hole, and the lower end of the feed rod is a conical surface. When the feeder extends into the reaction chamber, it pushes the feed rod downward, and the conical surface separates from the inner wall of the feed tube to form an annular gap.

[0012] The sampler includes a sampling rod, a sampling tube, and a connecting rod assembly. The end of the connecting rod assembly is provided with symmetrical sampling slots. When the sampling rod is lifted upward, the clamping plates of the connecting rod assembly close to hold the material.

[0013] As a further optimization of this utility model, when it is necessary to perform feeding or sampling operations, a vacuum pump is connected through a manual ball valve to evacuate the telescopic bellows. Then, the reaction gas source is connected to match the atmosphere inside the furnace. The pressure is monitored by a pressure sensor until the atmosphere inside the bellows matches the atmosphere inside the reaction chamber, thus avoiding interference from the experimental atmosphere by external air.

[0014] As a further optimization of this utility model, the feeder is quickly connected to the telescopic corrugated pipe via a KF clamp interface, and its interior includes a feed pipe and a feed rod. The lower part of the feed pipe has a through hole for pre-loading materials; the lower end of the feed rod is a conical surface, which normally fits and seals against the inner wall of the feed pipe.

[0015] As a further optimization of this utility model, the vacuum ball valve is opened to connect the telescopic bellows to the reaction chamber. The telescopic bellows is manually pressed down to extend the feeder into the reaction chamber. The feed rod is pushed down, and its conical surface separates from the inner wall of the feed tube to form an annular gap. The material falls into the reaction crucible through the gap, completing the quantitative feeding. After feeding, the feed rod is reset, the vacuum ball valve is closed, and the connection between the feeder and the telescopic bellows is disconnected.

[0016] As a further optimization of this utility model, the sampler is quickly connected to the telescopic bellows via a KF clamp interface. Internally, it includes a sampling rod, a sampling tube, and a connecting rod assembly. The end of the connecting rod assembly has symmetrical sampling slots, which are normally open. Open the vacuum ball valve and insert the sampler into the designated position in the reaction chamber. Lift the sampling rod upwards; the clamps of the connecting rod assembly close, holding the material in the reaction crucible within the symmetrical sampling slots. Lift the sampler, close the vacuum ball valve, disconnect the connection, and remove the sample to complete the sampling process.

[0017] As a further optimization of this utility model, the connection between the telescopic corrugated pipe and the heater, reaction chamber, feeder, and sampler is designed with a double-layer sealing ring shaft seal.

[0018] As a further optimization of this utility model, the heater and reaction chamber are connected to the main body of the equipment via a reaction bellows. The connections between the telescopic bellows and the heater, reaction chamber, feeder, and sampler all employ a double-layer sealing ring shaft seal design to ensure the airtightness of the entire system. The shell serves as an external protective structure to maintain internal environmental stability.

[0019] As a further optimization of this invention, a condenser is used to condense the gas discharged from the reaction chamber; a thermocouple is used to monitor the temperature inside the reaction chamber. Initially, the lifting mechanism drives the heater and reaction chamber to rise, placing the material inside the reaction crucible in a heated environment, and the thermocouple monitors the temperature until it stabilizes. The rapidly descending lifting mechanism detaches the heater and reaction chamber from the material, causing a sudden change in the ambient temperature of the material. The weighing module monitors the material's mass change in real time and, combined with temperature data, analyzes the impact of the sudden environmental change on the material's reaction.

[0020] Compared with the prior art, the beneficial effects of this utility model are as follows: 1. This utility model, through the structural design of telescopic bellows, KF clamp interface and vacuum ball valve, realizes online feeding and sampling operations in the thermogravimetric analysis process without interrupting the experiment or reloading samples, avoiding systematic errors caused by inconsistent experimental starting conditions, and effectively improving the continuity of experiments and the efficiency of multi-component sample analysis.

[0021] 2. This utility model adopts a double-layer sealing ring shaft seal design, and the reaction bellows and pressure sensor work together to ensure the system's sealing during feeding / sampling, prevent inert atmosphere leakage or external air infiltration, avoid unexpected reactions such as sample oxidation and moisture absorption, ensure the authenticity and reliability of thermogravimetric curve data, and improve the accuracy of analysis results. 3. This utility model uses an electric lifting mechanism to drive the heater and reaction chamber to rise and fall rapidly, which can cause a sudden change in the temperature of the material's environment. Combined with a weighing module and thermocouples to monitor the mass and temperature changes in real time, it can accurately analyze the impact of sudden temperature changes on the material reaction, providing an effective means for studying dynamic reaction processes.

[0022] 4. The telescopic corrugated pipe of this utility model is made of stainless steel telescopic material and is equipped with KF quick-release interface, which facilitates quick docking and disassembly of the feeder and sampler, improving the convenience of operation; the setting of condenser and thermocouple can condense the reaction gas and accurately monitor the temperature, and combined with the weighing module to realize multi-dimensional data acquisition, enhancing the equipment's functional diversity and experimental adaptability. Attached Figure Description

[0023] Figure 1 This is a front view of the overall structure of this utility model; Figure 2 This is a side view of the present invention; Figure 3 This is a schematic diagram of the connection structure of the feeder of this utility model; Figure 4 This is a schematic diagram of the connection structure of the sampler of this utility model.

[0024] Explanation of key symbols: 101. Shell; 102. Heater and reaction chamber; 1011. Reaction bellows; 1012. Reaction crucible; 1010. Weighing module; 104. Telescopic bellows; 103. Vacuum ball valve; 105. Feeder; 106. Sampler; 1014. Lifting mechanism; 108. Pressure sensor; 107. Manual ball valve; 1051. Feeding pipe; 1052. Feeding rod; 1061. Connecting rod assembly; 1062. Symmetrical sampling groove; 109. Condenser; 1013. Thermocouple. Detailed Implementation

[0025] The present invention will be further described below with reference to the accompanying drawings and specific embodiments. It should be noted that, without conflict, the various embodiments or technical features described below can be arbitrarily combined to form new embodiments.

[0026] Example 1:

[0027] Please combine Figures 1-4This embodiment proposes an online feeding and sampling thermogravimetric analyzer, characterized in that it includes: Housing 101; and heater and reaction chamber 102 disposed within housing 101, the heater and reaction chamber 102 being connected to the main body of the equipment via reaction bellows 1011; The reaction crucible 1012 is fixed above the weighing module 1010 and located inside the heater and reaction chamber 102. The telescopic bellows 104 is connected at one end to the heater and reaction chamber 102 via a vacuum ball valve 103, and at the other end is equipped with a KF clamp interface. The telescopic bellows 104 is made of stainless steel and is telescopic to accommodate the up and down movement of the heater and reaction chamber 102.

[0028] The feeder 105 and the sampler 106 are detachably connected to the telescopic corrugated pipe 104 via KF clamp interfaces. The lifting mechanism 1014 is linked to the heater and reaction chamber 102 and is used to drive the heater and reaction chamber 102 to move up and down. The lifting mechanism 1014 is an electric drive mechanism that can realize the rapid lifting and lowering of the heater and reaction chamber.

[0029] Pressure sensor 108 is used to monitor the pressure inside the telescopic bellows 104; Manual ball valve 107 is located on the side wall of telescopic bellows 104 and is used to connect to a vacuum pump or a reaction gas source.

[0030] In the specific technical solution, when it is necessary to perform feeding or sampling operations, a vacuum pump is connected through a manual ball valve 107 to evacuate the telescopic bellows 104. Then, the reaction gas source is connected to match the atmosphere inside the furnace. The pressure is monitored by a pressure sensor 108 until the atmosphere inside the bellows matches the atmosphere inside the reaction chamber 102, thus avoiding interference from the experimental atmosphere by outside air.

[0031] The feeder 105 includes a feed tube 1051 and a feed rod 1052. The feed tube 1051 has a through hole at the bottom and the lower end of the feed rod 1052 is a conical surface. When the feeder 105 extends into the reaction chamber, it pushes the feed rod 1052 downward, and the conical surface separates from the inner wall of the feed tube 1051 to form an annular gap.

[0032] In the specific technical solution, the feeder 105 is quickly connected to the telescopic corrugated pipe 104 via a KF clamp interface. Its interior includes a feed pipe 1051 and a feed rod 1052. The feed pipe 1051 has a through hole at the bottom for pre-loading materials; the lower end of the feed rod 1052 is a conical surface, which is normally in contact with and sealed to the inner wall of the feed pipe 1051.

[0033] Open the vacuum ball valve 103 to connect the telescopic bellows 104 to the reaction chamber 102. Manually press down the telescopic bellows 104 to extend the feeder 105 into the reaction chamber 102. Push the feed rod 1052 downwards, and its conical surface separates from the inner wall of the feed tube 1051 to form an annular gap. The material falls through the gap into the reaction crucible 1012, completing the quantitative feeding. After feeding, reset the feed rod 1052, close the vacuum ball valve 103, and disconnect the feeder 105 from the telescopic bellows 104.

[0034] The sampler 106 includes a sampling rod, a sampling tube, and a connecting rod assembly 1061. The end of the connecting rod assembly is provided with symmetrical sampling grooves 1062. When the sampling rod is lifted upward, the clamping plates of the connecting rod assembly 1061 close to clamp the material.

[0035] Specifically, the sampler 106 is quickly connected to the telescopic bellows 104 via a KF clamp interface. Internally, it includes a sampling rod, a sampling tube, and a connecting rod assembly 1061. The end of the connecting rod assembly 1061 has a symmetrical sampling groove 1062, which is normally open. The vacuum ball valve 103 is opened, and the sampler 106 is inserted into the designated position in the reaction chamber 102. The sampling rod is lifted upwards, closing the clamps of the connecting rod assembly 1061, clamping the material in the reaction crucible 1012 within the symmetrical sampling groove 1062. The sampler 106 is then lifted, the vacuum ball valve 103 is closed, the connection is disconnected, and the sample is removed, completing the sampling process.

[0036] It should be noted that the connection between the telescopic bellows 104 and the heater, reaction chamber 102, feeder 105, and sampler 106 all adopt a double-layer sealing ring shaft seal design.

[0037] In the specific technical solution, the heater and reaction chamber 102 are connected to the main body of the equipment through the reaction bellows 1011. The connection between the telescopic bellows 104 and the heater and reaction chamber 102, the feeder 105, and the sampler 106 all adopt a double-layer sealing ring shaft seal design to ensure the airtightness of the entire system. The shell 101 is an external protective structure to maintain the stability of the internal environment.

[0038] Furthermore, the condenser 109 is used to condense the gas discharged from the reaction chamber; the thermocouple 1013 is used to monitor the temperature inside the reaction chamber. Initially, the lifting mechanism 1014 drives the heater and reaction chamber 102 upwards, placing the material inside the reaction crucible 1012 in a heated environment, and the thermocouple 1013 monitors the temperature until it stabilizes. The lifting mechanism 1014 then rapidly descends, causing the heater and reaction chamber 102 to detach from the material, resulting in a sudden change in the ambient temperature of the material. The weighing module 1010 monitors the material's mass change in real time and, combined with temperature data, analyzes the impact of the sudden environmental change on the material's reaction.

[0039] The working principle of the online feeding and sampling thermogravimetric analyzer described in this patent is as follows: I. Overall Sealing and Atmosphere Control Principle Sealing structure design: The heater and reaction chamber 102 are connected to the main body of the equipment via a reaction bellows 1011. The connections between the telescopic bellows 104 and the heater and reaction chamber 102, the feeder 105, and the sampler 106 all employ a double-layer sealing ring shaft seal design to ensure the airtightness of the entire system. The housing 101 serves as an external protective structure to maintain a stable internal environment.

[0040] Atmosphere replacement process: When feeding or sampling is required, a vacuum pump is connected via manual ball valve 107 to evacuate the telescopic bellows 104. Then, a reaction gas source (consistent with the atmosphere inside the furnace) is connected, and the pressure is monitored by pressure sensor 108 until the atmosphere inside the bellows is consistent with that inside the reaction chamber 102, thus avoiding interference from outside air on the experimental atmosphere.

[0041] II. Working Principle of Online Feeding The feeder 105 is quickly connected to the telescopic corrugated pipe 104 via a KF clamp interface. It contains a feed pipe 1051 and a feed rod 1052. The feed pipe 1051 has a through hole at the bottom for pre-loading materials; the lower end of the feed rod 1052 is a conical surface, which is normally in contact with and sealed to the inner wall of the feed pipe 1051.

[0042] Open the vacuum ball valve 103 to connect the telescopic bellows 104 to the reaction chamber 102. Manually press down the telescopic bellows 104 to extend the feeder 105 into the reaction chamber 102. Push the feed rod 1052 downwards, and its conical surface separates from the inner wall of the feed tube 1051 to form an annular gap. The material falls through the gap into the reaction crucible 1012, completing the quantitative feeding.

[0043] After feeding, reset the feeding rod 1052, close the vacuum ball valve 103, and disconnect the feeder 105 from the telescopic bellows 104.

[0044] III. Working Principle of Online Sampling The sampler 106 is quickly connected to the telescopic bellows 104 via a KF clamp interface. It contains a sampling rod, a sampling tube, and a connecting rod assembly 1061. The end of the connecting rod assembly 1061 is provided with symmetrical sampling slots 1062, which are normally in an open state.

[0045] Open the vacuum ball valve 103 and insert the sampler 106 into the designated position in the reaction chamber 102. Lift the sampling rod upwards; the clamps of the connecting rod assembly 1061 will close, holding the material in the reaction crucible 1012 within the symmetrical sampling groove 1062. Lift the sampler 106, close the vacuum ball valve 103, disconnect the connection, and remove the sample to complete the sampling process.

[0046] IV. Principle of Sudden Temperature Change Experiment The lifting mechanism 1014 is linked to the heater and the reaction chamber 102, and can drive them to move up and down. The reaction chamber 102 is connected to the main body of the equipment through the reaction bellows 1011 to ensure sealing during movement.

[0047] The process of implementing a sudden temperature change: Initially, the lifting mechanism 1014 drives the heater and reaction chamber 102 to rise, placing the material inside the reaction crucible 1012 in a heated environment, with the thermocouple 1013 monitoring the temperature until it stabilizes. The lifting mechanism 1014 then rapidly descends, causing the heater and reaction chamber 102 to detach from the material, resulting in a sudden change in the ambient temperature. The weighing module 1010 monitors the material's mass change in real time and, combined with temperature data, analyzes the impact of the sudden environmental change on the material's reaction.

[0048] The above embodiments are merely preferred embodiments of this utility model and should not be construed as limiting the scope of protection of this utility model. Any non-substantial changes and substitutions made by those skilled in the art based on this utility model shall fall within the scope of protection claimed by this utility model.

Claims

1. A thermogravimetric analyzer with online feeding and sampling, characterized in that, include: The housing (101); and the heater and reaction chamber (102) disposed within the housing (101), the heater and reaction chamber (102) being connected to the main body of the equipment via a reaction bellows (1011); A reaction crucible (1012) is fixed above the weighing module (1010) and located inside the heater and reaction chamber (102); The telescopic bellows (104) has one end connected to the heater and reaction chamber (102) via a vacuum ball valve (103), and the other end is provided with a KF clamp interface; The feeder (105) and sampler (106) are detachably connected to the telescopic corrugated pipe (104) via the KF clamp interface. A lifting mechanism (1014) is linked to the heater and the reaction chamber (102) and is used to drive the heater and the reaction chamber (102) to move up and down. A pressure sensor (108) is used to monitor the pressure inside the telescopic bellows (104); Manual ball valve (107), which is located on the side wall of the telescopic bellows (104), is used to connect the vacuum pump and one of the reaction gas sources.

2. The online feeding and sampling thermogravimetric analyzer according to claim 1, characterized in that, The feeder (105) includes a feed tube (1051) and a feed rod (1052). The feed tube (1051) has a through hole at its lower part, and the lower end of the feed rod (1052) is a conical surface. When the feeder (105) extends into the reaction chamber, it pushes the feed rod (1052) downward, and the conical surface separates from the inner wall of the feed tube (1051) to form an annular gap.

3. The online feeding and sampling thermogravimetric analyzer according to claim 1, characterized in that, The sampler (106) includes a sampling rod, a sampling tube and a connecting rod assembly (1061). The connecting rod assembly (1061) has symmetrical sampling slots (1062) at its end. When the sampling rod is lifted upward, the clamping plates of the connecting rod assembly (1061) close to clamp the material.

4. The online feeding and sampling thermogravimetric analyzer according to claim 1, characterized in that, The connection between the telescopic bellows (104) and the heater and reaction chamber (102), the feeder (105), and the sampler (106) all adopt a double-layer sealing ring shaft seal design.

5. The online feeding and sampling thermogravimetric analyzer according to claim 1, characterized in that, It also includes a condenser (109) and a thermocouple (1013), the condenser (109) being used to condense the gas discharged from the reaction chamber; the thermocouple (1013) being used to monitor the temperature inside the reaction chamber.

6. The online feeding and sampling thermogravimetric analyzer according to claim 1, characterized in that, The telescopic bellows (104) is made of stainless steel and is telescopic to accommodate the up-and-down movement of the heater and reaction chamber (102).

7. The online feeding and sampling thermogravimetric analyzer according to claim 1, characterized in that, The lifting mechanism (1014) is an electrically driven mechanism that enables rapid lifting and lowering of the heater and reaction chamber.

8. The online feeding and sampling thermogravimetric analyzer according to claim 1, characterized in that, The KF clamp interface is a quick-release interface, which enables the rapid docking and disassembly of the feeder (105), sampler (106) and telescopic corrugated pipe (104).

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