Thermogravimetric analysis and gas analysis system and test method

Abstract

The application provides a thermogravimetric analysis and gas analysis system and a test method. The thermogravimetric analysis and gas analysis system comprises a gas distribution device, a reaction device, a weighing device and an analysis device. The gas distribution device comprises a gas cylinder and a gas pipeline. The reaction device comprises an electric heating furnace, a sleeve, a reaction tube and a sintered plate. The electric heating furnace is arranged on the outer circumferential side of the sleeve. The reaction tube comprises a first tube section and a second tube section which are communicated with each other. The first tube section is located in the sleeve. The sintered plate is used for placing a sample and is located in the first tube section. An air inlet pipe is arranged on the sleeve. The gas cylinder, the gas pipeline and the air inlet pipe are sequentially communicated. The air inlet pipe is communicated with the first tube section through a hose. The weighing device comprises a balance and a cooler. The analysis device comprises a temperature detector, a temperature controller, a gas sampler and a gas analyzer. The thermogravimetric analysis and gas analysis system has the advantages that the thermogravimetric analysis and the gas analysis can be simultaneously performed, and the test data is accurate.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of sample analysis, in particular to a thermogravimetric analysis and gas analysis system and a test method. BACKGROUND

[0002] Thermogravimetric analysis technology is one of the most commonly used methods for studying gas-solid reaction kinetics. It usually places a small amount of solid sample to be tested in a small crucible connected to a weighing mechanism. The solid particles interact with the gas components in the horizontal or vertical gas flow. Under the control of the temperature, the relationship between the solid mass and the temperature or time is measured. In related technologies, the thermogravimetric analyzer is subject to the following problems to varying degrees: (1) The sample to be tested and the crucible are usually suspended in the gas flow and are easily disturbed by the gas buoyancy and convection; (2) Due to the constraints of heat conduction and mass transfer resistance, the sample size for one measurement is usually small (5mg-10mg), which is greatly affected by the uniformity of the material and is difficult to accurately reflect the overall characteristics; (3) The flow field near the crucible is in a state of flow around, and the gas components need to go through processes such as external diffusion and bed internal diffusion to react with the particles accumulated under the crucible. The model description of the flow and mass transfer is very complex, which also brings great uncertainty to the calculation of the corresponding kinetic parameters; (4) Most thermogravimetric analyzers only obtain the mass information of the solid sample. Although there are some thermogravimetric infrared gas chromatography mass spectrometry analysis methods, due to the small sample size, small gas flow, and low tail gas concentration, most gas analyzers cannot meet the measurement requirements in terms of follow-up and accuracy. Therefore, it is usually only possible to obtain qualitative analysis results of the gas components after the reaction, and it is difficult to achieve high-precision online gas measurement and fully understand the progress of the gas-solid reaction. SUMMARY

[0003] The present application aims to at least solve one of the technical problems in the related art. To this end, embodiments of the present application propose a thermogravimetric analysis and gas analysis system and a test method.

[0004] The thermogravimetric analysis and gas analysis system according to an embodiment of the present application comprises:

[0005] A gas distribution device, the gas distribution device comprising a gas cylinder and a gas pipeline;

[0006] A reaction device, the reaction device comprising an electric heating furnace, a sleeve, a reaction tube and a sintered plate, the electric heating furnace being annularly arranged on the outer circumferential side of the sleeve, the reaction tube comprising a first tube segment and a second tube segment which are in communication with each other, the first tube segment being located in the sleeve, the sintered plate being used for placing a sample, the sintered plate being located in the first tube segment, the sleeve being provided with a gas inlet pipe, the gas cylinder, the gas pipeline and the gas inlet pipe being sequentially communicated, the gas inlet pipe being communicated with the first tube segment through a hose;

[0007] a weighing device, the weighing device comprising a balance and a cooler, the cooler having a cooling cavity, the sleeve being in communication with the cooling cavity, the balance being located in the cooling cavity, the second tube segment extending into the cooling cavity and being placed on the balance;

[0008] an analysis device, the analysis device comprising a temperature detector, a temperature controller, a gas sampler and a gas analyzer, each of the temperature detector and the gas sampler extending through the sleeve and the tube wall of the reaction tube and into the first tube segment, the gas temperature controller being located outside the sleeve and connected with the temperature detector, the gas analyzer being located outside the sleeve and connected with the gas sampler.

[0009] Therefore, the thermogravimetric analysis and gas analysis system according to the embodiments of the present application has the advantages of simultaneous thermogravimetric analysis and gas analysis and accurate test data.

[0010] In some embodiments, the reaction tube extends in the up-down direction, the gas inlet tube is located above the reaction tube, and the first tube segment is located above the second tube segment.

[0011] In some embodiments, the gas distribution device further comprises a gas mixing chamber, the gas mixing chamber being in communication with the gas inlet tube through the gas conveying pipeline, and the gas cylinders are multiple, the multiple gas cylinders being capable of storing multiple reaction gases, each of the gas cylinders being in communication with the gas mixing chamber through a first pipeline, and each of the first pipelines being provided with a flow meter and a control valve.

[0012] In some embodiments, the cooler comprises

[0013] a water-cooled box, the bottom of the sleeve being in communication with the water-cooled box, a sealing ring being provided between the bottom of the sleeve and the water-cooled box, the water-cooled box comprising a first cavity, a first hole and the cooling cavity, the first cavity being used for containing a cooling liquid, the first cavity being annularly arranged at the periphery of the first hole and the cooling cavity, the sleeve, the first hole and the cooling cavity being sequentially communicated from top to bottom, the first hole extending in the up-down direction, the second tube segment extending through the first hole and into the cooling cavity, and the shape of the first hole being matched with the shape of the reaction tube;

[0014] a mounting plate, the mounting plate being provided at the bottom of the water-cooled box and being used for covering the bottom of the cooling cavity, and the balance being provided on the upper surface of the mounting plate.

[0015] a water chiller, an outlet of the water chiller being in communication with an inlet of the first cavity, and an outlet of the first cavity being in communication with an inlet of the water chiller through a water-cooled pipeline.

[0016] In some embodiments, the weighing device further comprises

[0017] a card seat detachably provided on the balance, the card seat having a card slot with an opening facing upward, the card slot extending in the up-down direction, the second pipe segment being located in the card slot;

[0018] a lifting machine provided at the bottom of the mounting plate.

[0019] In some embodiments, a lower portion of the first pipe segment is provided with a first outlet;

[0020] the sintering plate is located above the first outlet, the sintering plate having a first through hole penetrating therethrough in the up-down direction, the first through hole having a diameter smaller than the particle size of the sample;

[0021] the sleeve pipe includes a pipe body and a top cover, the pipe body extending in the up-down direction, a lower portion of the pipe body being provided with a second outlet, the first outlet and the second outlet being oppositely arranged in the horizontal direction, the top cover being detachably provided on the top of the pipe body, the air inlet pipe being provided on the top cover, a top portion of the hose being connected to the air inlet pipe, and a bottom portion of the hose being in communication with the reaction pipe;

[0022] the temperature measuring device is a thermocouple, the thermocouple sequentially passing through the second outlet and the first outlet and extending into the first pipe segment, the thermocouple being in an L-shaped structure, and a top portion of the thermocouple being adjacent to the sintering plate in the up-down direction;

[0023] the gas sampler is a gas sampling probe, the gas sampling probe sequentially passing through the second outlet and the first outlet and extending into the first pipe segment, the gas sampling probe being in an L-shaped structure, and a top portion of the gas sampling probe being adjacent to the sintering plate in the up-down direction;

[0024] the temperature controller and the gas analyzer are both connected to a computer.

[0025] In some embodiments, each of the sleeve pipe, the reaction pipe and the sintering plate is made of a heat-resistant material with a heat-resistant temperature greater than or equal to 1100℃;

[0026] the hose is made of a silica gel material or a rubber material.

[0027] In some embodiments, an inner wall surface of the top portion of the pipe body has a ground joint matched with the top cover, and the inner wall surface of the top portion of the pipe body is coated with lubricating oil;

[0028] an inner diameter of the reaction pipe is greater than or equal to 8mm and less than or equal to 15mm;

[0029] a ratio of an outer diameter of each of the thermocouple and the gas sampling probe to the inner diameter of the reaction pipe is less than or equal to 1 / 4.

[0030] The present application also provides a test method using the thermal gravimetric and gas analysis system, comprising the following steps:

[0031] Placing the sample on the sintered plate in the reaction tube;

[0032] Extending the reaction tube into the cooling cavity of the cooler and placing it on the balance;

[0033] Covering the outer periphery of the reaction tube with the sleeve and connecting the gas inlet pipe on the sleeve with the inlet of the reaction tube through the hose;

[0034] Extending the temperature measuring device and the gas sampler into the reaction tube;

[0035] Turning on the cooler;

[0036] Delivering the reaction gas with preset concentration and flow rate into the reaction tube through the gas delivery pipeline and discharging it from the reaction tube after passing through the sample on the sintered plate;

[0037] Turning on the temperature controller and the gas analyzer and recording the temperature data, gas concentration data and mass data changing with time synchronously;

[0038] Turning on the heating furnace on the outer periphery of the sleeve to heat the sample on the sintered plate to a preset temperature.

[0039] In some embodiments, the flow rate of the reaction gas into the reaction tube is greater than or equal to 0.1 L / min and less than or equal to 10 L / min;

[0040] The mass of the sample on the sintered plate is greater than or equal to 50 mg. BRIEF DESCRIPTION OF DRAWINGS

[0041] Figure 1 is a schematic diagram of a thermal gravimetric and gas analysis system according to an embodiment of the present application.

[0042] REFERENCE NUMERALS:

[0043] Thermal gravimetric and gas analysis system 100;

[0044] Gas cylinder 1, gas delivery pipeline 11, gas mixing chamber 12, first pipeline 13, flow meter 14, control valve 15;

[0045] Electric heating furnace 2;

[0046] Sleeve 3, pipe body 31, top cover 32, gas inlet pipe 33, second outlet 34, hose 35;

[0047] Reaction tube 4, first pipe section 41, second pipe section 42, first outlet 43;

[0048] Sintered plate 5;

[0049] Balance scale 6, booth 61;

[0050] Water-cooled box 7, first cavity 71, first hole 72, cooling cavity 73, mounting plate 74, water chiller 75, water-cooled pipes 76;

[0051] Temperature sensor 81, temperature controller 82, gas sampler 83, gas analyzer 84, computer 85, elevator 86. Detailed Implementation

[0052] Embodiments of the present invention are described in detail below, examples of which are illustrated in the accompanying drawings. The embodiments described below with reference to the accompanying drawings are exemplary and intended to explain the present invention, and should not be construed as limiting the present invention.

[0053] Thermogravimetric analysis and gas analysis system 100 according to an embodiment of the present invention will now be described with reference to the accompanying drawings. Figure 1 As shown, the thermogravimetric analysis and gas analysis system 100 according to an embodiment of the present invention includes a gas mixing device, a reaction device, a weighing device, and an analysis device.

[0054] The gas distribution device includes a gas cylinder 1 and a gas supply pipeline 11. The reaction device includes an electric heating furnace 2, a sleeve 3, a reaction tube 4, and a sintering plate 5. The electric heating furnace 2 is arranged around the outer periphery of the sleeve 3. The reaction tube 4 includes a first tube section 41 and a second tube section 42 that are interconnected. The first tube section 41 is located inside the sleeve 3. The sintering plate 5 is used to place the sample and is located inside the first tube section 41. The sleeve 3 is provided with an inlet pipe 33. The gas cylinder 1, the gas supply pipeline 11, and the inlet pipe 33 are connected in sequence. The inlet pipe 33 is connected to the first tube section 41 through a flexible hose 35.

[0055] The weighing device includes a balance 6 and a cooler. The cooler has a cooling chamber 73. The sleeve 3 is connected to the cooling chamber 73. The balance 6 is located inside the cooling chamber 73. The second pipe section 42 extends into the cooling chamber 73 and is placed on the balance 6.

[0056] The analytical apparatus includes a thermometer 81, a temperature controller 82, a gas sampler 83, and a gas analyzer 84. Each of the thermometer 81 and the gas sampler 83 passes through the walls of the sleeve 3 and the reaction tube 4 and extends into the first tube section 41. The gas temperature controller 82 is located outside the sleeve 3 and connected to the thermometer 81, and the gas analyzer 84 is located outside the sleeve 3 and connected to the gas sampler 83.

[0057] The thermal gravimetric and gas analysis system 100 according to the embodiment of the present application has the reaction tube 4 arranged in the sleeve 3, and the inlet pipe 33 is communicated with the first pipe section 41 through the hose 35. Thus, when the sample on the sintered plate 5 in the reaction tube 4 reacts with the reaction gas, the reaction is less affected by the outside (air flow or vibration of the sleeve 3). The direct contact between the reaction tube 4 and the outside is minimized, and the accuracy of the mass measurement is improved. The balance 6 is located in the cooling cavity 73 of the cooler, so that the weighing error of the balance 6 to the reaction tube 4 is small, so that the monitoring of the change of the weight of the sample is more accurate.

[0058] The analysis device of the thermal gravimetric and gas analysis system 100 according to the embodiment of the present application includes a temperature detector 81, a temperature controller 82, a gas sampler 83 and a gas analyzer 84. Each of the temperature detector 81 and the gas sampler 83 penetrates the wall of the sleeve 3 and the reaction tube 4 and extends into the first pipe section 41, so that the change of the gas and the change of the temperature in the reaction tube 4 can be monitored. That is, the thermal gravimetric and gas analysis system 100 according to the embodiment of the present application can synchronously and on-line obtain the change of the sample mass and the change of the concentration of the tail gas component in the gas-solid reaction process, so that the progress of the gas-solid reaction is more comprehensively mastered. Thus, the gas analysis can be performed at the same time of the thermal gravimetric analysis, and the test is more comprehensive.

[0059] Therefore, the thermal gravimetric and gas analysis system 100 according to the embodiment of the present application has the advantages that the thermal gravimetric analysis and the gas analysis can be simultaneously performed, and the test data is accurate.

[0060] As shown in Figure 1 The thermal gravimetric and gas analysis system 100 according to the embodiment of the present application includes a gas distribution device, a reaction device, a weighing device and an analysis device.

[0061] The reaction device includes the electric heating furnace 2, the sleeve 3, the reaction tube 4 and the sintered plate 5.

[0062] The reaction tube 4 includes the first pipe section 41 and the second pipe section 42 which are communicated with each other, and the first pipe section 41 is located in the sleeve 3. Specifically, the reaction tube 4 extends in the up-down direction, the first pipe section 41 is located above the second pipe section 42, and the lower part of the first pipe section 41 is provided with the first outlet 43. The up-down direction is shown by the arrow in the figure. The reaction tube 4 extends in the up-down direction, and the inlet of the reaction tube 4 is located at the top thereof, so that the gas flow is in a downward state in the reaction tube 4, the back mixing effect is small, and there is no gas buoyancy effect, which can effectively avoid the distortion of the gas concentration signal and the mass signal. In the reaction process, the flow penetrates the stationary reaction bed layer, the flow structure is simple, the heat and mass transfer law is more clear, and the mature plug flow reactor model can be applied to mathematically describe the reaction process, so that the reaction kinetics parameters can be more accurately calculated.

[0063] In some embodiments, the inner diameter of the reaction tube 4 is greater than or equal to 8 mm and less than or equal to 15 mm. For example, the inner diameter of the reaction tube 4 is 10 mm.

[0064] As shown in FIG. 1, the sintering plate 5 is used to place the sample, and the sintering plate 5 is located in the first tube section 41. Specifically, the thickness direction of the sintering plate 5 is the up-down direction, the sintering plate 5 is located at the upper part of the first tube section 41, and the sintering plate 5 is located above the first outlet 43. The sintering plate 5 has a first through hole penetrating through the sintering plate 5 along the up-down direction, and the diameter of the first through hole is smaller than the particle size of the sample, so as to prevent the sample from being taken away by the reaction gas. Figure 1 As shown in FIG. 1, the sintering plate 5 is used to place the sample, and the sintering plate 5 is located in the first tube section 41. Specifically, the thickness direction of the sintering plate 5 is the up-down direction, the sintering plate 5 is located at the upper part of the first tube section 41, and the sintering plate 5 is located above the first outlet 43. The sintering plate 5 has a first through hole penetrating through the sintering plate 5 along the up-down direction, and the diameter of the first through hole is smaller than the particle size of the sample, so as to prevent the sample from being taken away by the reaction gas.

[0065] Figure 1 As shown in FIG. 1, the sleeve 3 is provided with a gas inlet pipe 33, the gas inlet pipe 33 is located above the reaction tube 4, and the gas inlet pipe 33 is communicated with the first tube section 41 through a hose 35, so as to reduce the influence on the weight of the reaction tube 4. Specifically, the hose 35 is made of silica gel material or rubber material. The hose 35 can be directly sleeved with the gas inlet pipe 33 and the reaction tube 4, or can be connected with the gas inlet pipe 33 and the reaction tube 4 through a clamping sleeve joint.

[0066] In some embodiments, the sleeve 3 includes a tube body 31 and a top cover 32, the tube body 31 extends along the up-down direction, and the lower part of the tube body 31 is provided with a second outlet 34. The first outlet 43 and the second outlet 34 are oppositely arranged in the horizontal direction. The top cover 32 is detachably arranged at the top of the tube body 31, the gas inlet pipe 33 is arranged on the top cover 32, the top of the hose 35 is connected with the gas inlet pipe 33, and the bottom of the hose 35 is communicated with the reaction tube 4. The second outlet 34 can be communicated with a tail gas treatment device, so as to prevent the reaction gas from polluting the environment.

[0067] In some embodiments, the inner wall surface of the top of the tube body 31 has a matching chamfer with the top cover 32 (lower part), and the inner wall surface of the top of the tube body 31 is smeared with lubricating oil. Thus, the tube body 31 and the top cover 32 can be opened and tightly sealed with good sealing effect.

[0068] As shown in FIG. 1, the electric heating furnace 2 is annularly arranged on the outer peripheral side of the sleeve 3, so that the electric heating furnace 2 can heat the sample on the sintering plate 5 in the sleeve 3 (reaction tube 4), and realize program temperature control. Figure 1 In some embodiments, each of the sleeve 3, the reaction tube 4 and the sintering plate 5 is made of a heat-resistant material with a heat-resistant temperature greater than or equal to 1100°C, so that the sleeve 3, the reaction tube 4 and the sintering plate 5 can withstand the high temperature generated by the electric heating furnace 2. For example, the sleeve 3, the reaction tube 4 and the sintering plate 5 can be made of quartz glass material.

[0069] As shown in FIG. 1, the electric heating furnace 2 is annularly arranged on the outer peripheral side of the sleeve 3, so that the electric heating furnace 2 can heat the sample on the sintering plate 5 in the sleeve 3 (reaction tube 4), and realize program temperature control.

[0070] Figure 1 ​​As shown, the gas distribution device includes gas cylinders 1, a mixing chamber 12 and a gas delivery pipeline 11, the gas cylinders 1 and the gas delivery pipeline 11 are sequentially communicated with the gas inlet pipe 33. Specifically, the mixing chamber 12 is communicated with the gas inlet pipe 33 through the gas delivery pipeline 11. The gas cylinders 1 are multiple, the multiple gas cylinders 1 can store multiple (and multiple concentrations) of reaction gases, each of the gas cylinders 1 is communicated with the mixing chamber 12 through a first pipeline 13, and a flow meter 14 and a control valve 15 are arranged on each of the first pipelines 13. Thus, according to the experimental requirements, the corresponding control valve 15 can be opened to pass different types (or different concentrations) of reaction gases into the mixing chamber 12 according to the proportion, the multiple gases are mixed uniformly in the mixing chamber 12 to obtain reaction gases with specific concentration and specific flow rate, and finally the reaction gases are passed into the gas inlet pipe 33 through the gas delivery pipeline 11. For example, the gas cylinders 1 are three to store inert gas and two different reaction gases respectively. For example, the control valve 15 is a ball valve.

[0071] As shown in Figure 1 , the weighing device includes a balance 6 and a cooler, the cooler has a cooling cavity 73, the sleeve 3 is communicated with the cooling cavity 73, the balance 6 is located in the cooling cavity 73, and the second pipeline segment 42 extends into the cooling cavity 73 and is placed on the balance 6. The cooler can isolate most of the radiant heat emitted by the upper electric heating furnace 2 and reduce the temperature of the reaction tube 4 in the cooling cavity 73, so as to ensure that the balance 6 works at room temperature to prevent the measurement baseline drift and even damage the balance 6. For example, the balance 6 is a high-precision electronic balance. The maximum weighing value of the electronic balance 6 is greater than or equal to 1000g, the readability is less than or equal to 1mg, and the measurement accuracy (repeatability) is less than or equal to 2mg.

[0072] In some embodiments, the cooler includes a water-cooled box 7, a mounting plate 74 and a water-cooled machine 75.

[0073] The bottom of the sleeve 3 (the pipe body 31) is communicated with the water-cooled box 7. Specifically, the bottom of the sleeve 3 (the pipe body 31) and the water-cooled box 7 are connected to each other through flanges, and a sealing ring is arranged between the bottom of the sleeve 3 (the pipe body 31) and the water-cooled box 7. Thus, the unorganized diffusion of part of the toxic and harmful tail gas into the environment can be avoided, and the formation of air flow in the gap between the reaction tube 4 and the first hole 72 can be prevented, and the air flow rubbing against the inner wall of the reaction tube 4 can interfere with the mass measurement.

[0074] As shown in Figure 1 , the water-cooled box 7 includes a first cavity 71, a first hole 72 and a cooling cavity 73, and the first cavity 71 is used to contain a cooling liquid.

[0075] The first cavity 71 is arranged around the first hole 72 and the cooling cavity 73. The sleeve 3, the first hole 72 and the cooling cavity 73 are connected sequentially from top to bottom. The first hole 72 extends in the vertical direction. The second pipe section 42 passes through the first hole 72 and extends into the cooling cavity 73. The shape of the first hole 72 is adapted to the shape of the reaction tube 4 (second pipe section 42). The diameter of the first hole 72 is smaller than the diameter of the cooling cavity 73. The first hole 72 and the reaction tube 4 (second pipe section 42) are spaced apart.

[0076] Mounting plate 74 is located at the bottom of water-cooled box 7 and is used to seal the bottom of cooling cavity 73. Balance 6 is located on the upper surface of mounting plate 74. Specifically, the thickness direction of mounting plate 74 is vertical. A sealing ring is provided between mounting plate 74 and the bottom of water-cooled box 7.

[0077] The outlet of the water chiller 75 is connected to the inlet of the first chamber 71, and the outlet of the first chamber 71 is connected to the inlet of the water chiller 75 through a water-cooling pipe 76. This allows the coolant to circulate within the water chiller 75 and the first chamber 71. Distilled water or deionized water is preferred as the coolant.

[0078] In some embodiments, the weighing device further includes a jack 61 and a lift 86.

[0079] The holder 61 is detachably mounted on the balance 6. The holder 61 has an upward-facing slot that extends vertically, and the second tube section 42 is located within the slot. Specifically, the slot can limit the second tube section 42 to prevent the reaction tube 4 from becoming loose, thereby ensuring that the reaction tube 4 remains vertical and stably placed on the balance 6. For example, the holder 61 is preferably made of PTFE, silicone, or stainless steel.

[0080] The lifting platform 86 is located at the bottom of the mounting plate 74. The lifting platform 86 can move the mounting plate 74 in the vertical direction, so that it can be raised and lowered before and after the test, so as to move the balance 6 and the reaction tube 4 in the vertical direction, thereby facilitating test preparation or cleaning.

[0081] like Figure 1 As shown, the analytical apparatus includes a thermometer 81, a temperature controller 82, a gas sampler 83, and a gas analyzer 84. Each of the thermometer 81 and the gas sampler 83 passes through the walls of the sleeve 3 and the reaction tube 4 and extends into the first tube section 41. The thermometer 81 and the gas sampler 83 are spaced apart from the reaction tube 4. The gas temperature controller 82 is located outside the sleeve 3 and connected to the thermometer 81, and the gas analyzer 84 is located outside the sleeve 3 and connected to the gas sampler 83. Both the temperature controller 82 and the gas analyzer 84 are connected to a computer 85. This facilitates the measurement of gas flow and temperature changes within the reaction tube 4 (first tube section 41) and the transmission of the data to the computer for recording and analysis.

[0082] In some embodiments, the temperature detector 81 is a thermocouple, which passes through the second outlet 34 and the first outlet 43 in sequence and extends into the first pipe segment 41. The thermocouple is in an L-shaped structure, and the top of the thermocouple is adjacent to the sintering plate 5 in the up-down direction, so as to facilitate the measurement of the reaction temperature of the sample. For example, the horizontal extension of the L-shaped thermocouple is connected to the pipe body 31 (the second outlet 34) of the sleeve 3, so that the sleeve 3 supports the thermocouple. The thermocouple is preferably a K-type armored thermocouple.

[0083] In some embodiments, the gas sampler 83 is a gas sampling probe, which passes through the second outlet 34 and the first outlet 43 in sequence and extends into the first pipe segment 41. The gas sampling probe is in an L-shaped structure, and the top of the gas sampling probe is adjacent to the sintering plate 5 in the up-down direction, so as to facilitate the measurement of the change of the gas near the sample. For example, the horizontal extension of the L-shaped gas sampling probe is connected to the pipe body 31 (the second outlet 34) of the sleeve 3, so that the sleeve 3 supports the gas sampling probe. The gas sampling probe is preferably made of 316L or 310S stainless steel. The gas analyzer 84 is preferably a fast mass spectrometer.

[0084] In some embodiments, the ratio of the outer diameter of each of the thermocouple and the gas sampling probe to the inner diameter of the reaction tube 4 is less than or equal to 1 / 4. Thus, the influence of the thermocouple and the gas sampling probe on the flow rate of the reaction gas can be reduced. For example, the ratio of the outer diameter of each of the thermocouple and the gas sampling probe to the inner diameter of the reaction tube 4 is equal to 1 / 8.

[0085] The present application also provides a test method using the thermogravimetric analysis and gas analysis system 100 according to the embodiments of the present application. The test method for thermogravimetric analysis and gas analysis according to the embodiments of the present application comprises the following steps:

[0086] Placing the sample on the sintering plate 5 in the reaction tube 4.

[0087] Inserting the second pipe segment 42 into the clamping groove of the clamp seat 61, so that the reaction tube 4 extends in the up-down direction.

[0088] Covering the reaction tube 4 with the sleeve 3, and connecting the gas inlet pipe 33 on the sleeve 3 to the inlet of the reaction tube 4 through the hose 35.

[0089] Inserting the temperature detector 81 and the gas sampler 83 into the reaction tube 4. The temperature detector 81 is connected to the temperature controller 82, and the gas sampler 83 is connected to the gas analyzer 84.

[0090] Turning on the cooler. After the preliminary preparation is completed, close the furnace door, turn on the power of the instruments and equipment, and open the water cooling machine 75 to circulate the cooling liquid.

[0091] The reaction gas with preset concentration and flow rate is delivered into the reaction tube 4 through the gas delivery pipeline 11 and discharged from the reaction tube 4 after passing through the sample on the sintered plate 5. Specifically, the control valves 15 on each first pipeline 13 are opened, the gas flow is adjusted through the flow meter 14 to obtain the reaction gas with preset concentration and flow rate, which enters the reaction tube 4 through the gas mixing chamber 12, the gas delivery pipeline 11, the gas inlet pipeline 33 and the hose 35 in sequence, and the tail gas is discharged through the lower first outlet 43 of the reactor 4 and the second outlet 34 of the lower part of the sleeve 3 after passing through the sample bed and the sintered plate 5.

[0092] The temperature controller 82 and the gas analyzer 84 are turned on, and the temperature data, the gas concentration data and the mass data changing with time are recorded synchronously. Specifically, the temperature-time data, the gas concentration-time data and the mass-time data are recorded synchronously and collected on the computer 85 for recording and processing.

[0093] The heating furnace on the outer circumferential side of the sleeve 3 is turned on to heat the sample on the sintered plate 5 to a preset temperature so that the sample starts to react with the gas.

[0094] In some embodiments, the flow rate of the reaction gas introduced into the reaction tube 4 is greater than or equal to 0.1 L / min and less than or equal to 10 L / min, so that the reaction gas is sufficient.

[0095] In some embodiments, the mass of the sample on the sintered plate 5 is greater than or equal to 50 mg. Thus, the sample capacity in the present application can be large, and the mass of solid material in a single experiment can reach kilograms, thereby effectively reducing the interference of sample unevenness on measurement and analysis, and making the quantity measurement more accurate.

[0096] In the description of the present application, it should be understood that the terms "center", "longitudinal", "transverse", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", "axial", "radial", "circumferential" and the like indicate the orientation or positional relationship based on the orientation or positional relationship shown in the drawings, which are only for the convenience of describing the present application and simplifying the description, and do not indicate or imply that the devices or elements referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore cannot be understood as limiting the present application.

[0097] In addition, the terms "first" and "second" are only for descriptive purposes and cannot be understood as indicating or implying relative importance or implicitly indicating the number of the technical features indicated. Therefore, the features defined with "first" and "second" can explicitly or implicitly include at least one of the features. In the description of the present application, the meaning of "a plurality of" is at least two, such as two, three, etc., unless otherwise specifically limited.

[0098] In the present application, unless specifically defined otherwise, the terms "mounting", "connected", "connecting", "fixed", "fixedly connected", "connection", "fixedly connected", "connected", "fixed", and the like should be construed broadly, for example, can be fixed connection, can be detachable connection, or integral; can be mechanical connection, can be electrical connection or communication with each other; can be directly connected, or indirectly connected through an intermediate medium, can be the internal communication of two elements or the interaction relationship between two elements, unless otherwise specifically defined. For those skilled in the art, the specific meaning of the above terms in the present application can be understood according to the specific circumstances.

[0099] In the present application, unless specifically defined otherwise, the first feature is "on" or "under" the second feature. The first and second features can be in direct contact, or the first and second features can be in indirect contact through an intermediate medium. Moreover, the first feature "above", "over" and "on" the second feature can be directly above or obliquely above the first feature, or only indicates that the horizontal height of the first feature is higher than that of the second feature. The first feature "below", "under" and "under" the second feature can be directly below or obliquely below the first feature, or only indicates that the horizontal height of the first feature is less than that of the second feature.

[0100] In the present application, the terms "one embodiment", "some embodiments", "example", "specific example", or "some examples" mean that the specific features, structures, materials or characteristics described in connection with the embodiment or example are included in at least one embodiment or example of the present application. In the present specification, the illustrative description of the above terms does not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in any appropriate manner in any one or more embodiments or examples. In addition, those skilled in the art can combine and combine different embodiments or examples described in the specification and the features of different embodiments or examples without contradiction.

[0101] Although the above embodiments have been shown and described, it is understood that the above embodiments are exemplary and cannot be construed as limiting the present application, and the changes, modifications, replacements and variations of the above embodiments made by those skilled in the art are within the scope of the present application.

Claims

1. A thermogravimetric and gas analysis system, characterized by, The utility model relates to a kind of reaction device and its auxiliary device, including: Gas distribution device, the gas distribution device includes gas cylinder and gas pipeline; Reaction device, the reaction device includes electric heating furnace, sleeve, reaction tube and sintered plate, the electric heating furnace ring is set in the outer circumferential side of the sleeve, the reaction tube extends along up-down direction, including first pipe section and second pipe section that communicate with each other, the first pipe section is located above the second pipe section, the first pipe section is located in the sleeve, the sintered plate is used to place sample, the sintered plate is located in the first pipe section, the sleeve is equipped with inlet pipe, the gas cylinder, the gas pipeline and the inlet pipe are sequentially communicated, the inlet pipe is communicated with the first pipe section by hose; The sleeve includes pipe body and top cover, the pipe body extends along up-down direction, the lower portion of the first pipe section is equipped with first outlet, the lower portion of the pipe body is equipped with second outlet, the first outlet and the second outlet are oppositely arranged in horizontal direction, the top cover is detachably arranged at the top of the pipe body, the inlet pipe is arranged on the top cover, the top of the hose is connected with the inlet pipe, the bottom of the hose is communicated with the first pipe section, the hose is made of silica gel material or rubber material; Weighing device, the weighing device includes balance, cooler and clamping seat, the cooler has cooling cavity, the sleeve is communicated with the cooling cavity, the balance is located in the cooling cavity, the second pipe section is inserted into the cooling cavity and placed on the balance; The clamping seat is detachably arranged on the balance, the clamping seat has clamping groove with opening facing upward, the clamping groove extends along up-down direction, and the second pipe section is located in the clamping groove; Analysis device, the analysis device includes temperature detector, temperature controller, gas sampler and gas analyzer, each of the temperature detector and the gas sampler penetrates the pipe wall of the sleeve and the reaction tube and extends into the first pipe section, the temperature controller is located outside the sleeve and connected with the temperature detector, and the gas analyzer is located outside the sleeve and connected with the gas sampler.

2. The thermogravimetric and gas analysis system of claim 1, wherein, The gas distribution device further includes a gas mixing chamber that is communicated with the inlet pipe through the gas pipeline, the gas cylinder is a plurality of, and the plurality of gas cylinders can store a plurality of reaction gases, each of the gas cylinders is communicated with the gas mixing chamber through a first pipeline, and a flow meter and a control valve are arranged on each of the first pipelines.

3. The thermogravimetric and gas analysis system of claim 1, wherein, The cooler includes: Water-cooled box, the bottom of the sleeve is communicated with the water-cooled box, and a sealing ring is arranged between the bottom of the sleeve and the water-cooled box, the water-cooled box includes a first cavity, a first hole and the cooling cavity, the first cavity is used for containing cooling liquid, the first cavity is ringed around the circumferential side of the first hole and the cooling cavity, the sleeve, the first hole and the cooling cavity are sequentially communicated from top to bottom, the first hole extends along up-down direction, the second pipe section penetrates the first hole and extends into the cooling cavity, and the shape of the first hole is matched with the shape of the reaction tube; Mounting plate, the mounting plate is arranged at the bottom of the water-cooled box and is used for covering the bottom of the cooling cavity, and the balance is arranged on the upper surface of the mounting plate. A water chiller, an outlet of the water chiller being communicated with an inlet of the first cavity, and an outlet of the first cavity being communicated with an inlet of the water chiller through a water cooling pipeline.

4. The thermogravimetric and gas analysis system of claim 3, wherein, The weighing device further comprises a lifter arranged at the bottom of the mounting plate. 5.The thermal gravimetric analysis and gas analysis system according to claim 1, wherein, The sintering plate is located above the first outlet, and the sintering plate has a first through hole penetrating therethrough in the up-down direction, and the diameter of the first through hole is smaller than the particle size of the sample; The temperature detector is a thermocouple, the thermocouple penetrates through the second outlet and the first outlet in sequence and extends into the first pipe segment, the thermocouple has an L-shaped structure, and the top of the thermocouple is adjacent to the sintering plate in the up-down direction; The gas sampler is a gas sampling probe, the gas sampling probe penetrates through the second outlet and the first outlet in sequence and extends into the first pipe segment, the gas sampling probe has an L-shaped structure, and the top of the gas sampling probe is adjacent to the sintering plate in the up-down direction; The temperature controller and the gas analyzer are connected to a computer. 6.The thermal gravimetric analysis and gas analysis system according to claim 5, wherein, Each of the sleeve, the reaction tube and the sintering plate is made of a heat-resistant material with a heat-resistant temperature greater than or equal to 1100℃. 7.The thermal gravimetric analysis and gas analysis system according to claim 5, wherein, The inner wall surface of the top of the pipe body has a matching ground joint with the top cover, and the inner wall surface of the top of the pipe body is coated with lubricating oil; The inner diameter of the reaction tube is greater than or equal to 8mm and less than or equal to 15mm; The ratio of the outer diameter of each of the thermocouple and the gas sampling probe to the inner diameter of the reaction tube is less than or equal to 1 / 4.

8. A test method using the thermogravimetric and gas analysis system according to any one of claims 1 to 7, characterized by, The method comprises the following steps: Placing the sample on the sintering plate in the reaction tube; Extending the reaction tube into the cooling cavity of the cooler and placing it on the balance; Covering the sleeve on the outer periphery of the reaction tube and connecting the gas inlet pipe on the sleeve to the inlet of the reaction tube through a hose; Extending the temperature detector and the gas sampler into the reaction tube; Turning on the cooler; Delivering the reaction gas with a preset concentration and flow rate into the reaction tube through the gas delivery pipeline and discharging the reaction gas after it passes through the sample on the sintering plate; Turning on the temperature controller and the gas analyzer and synchronously recording the temperature data, the gas concentration data and the mass data changing with time; Turning on the heating furnace on the outer periphery of the sleeve so as to heat the sample on the sintering plate to a preset temperature. 9.The thermal gravimetric analysis and gas analysis test method according to claim 8, wherein, The flow rate of the reaction gas delivered into the reaction tube is greater than or equal to 0.1L / min and less than or equal to 10L / min; The mass of the sample on the sintering plate is greater than or equal to 50mg.

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