CN210180966U - Suspended state thermal analysis test device - Google Patents
Suspended state thermal analysis test device Download PDFInfo
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- CN210180966U CN210180966U CN201920528316.6U CN201920528316U CN210180966U CN 210180966 U CN210180966 U CN 210180966U CN 201920528316 U CN201920528316 U CN 201920528316U CN 210180966 U CN210180966 U CN 210180966U
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- 238000003860 storage Methods 0.000 claims description 12
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 7
- 229910052710 silicon Inorganic materials 0.000 claims description 7
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- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 4
- 238000002485 combustion reaction Methods 0.000 description 4
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- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 2
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Abstract
The utility model discloses a suspension state thermal analysis test device, it includes negative pressure control system, suspension reaction furnace system, automatic feeding system, constant temperature control system and data acquisition system. The device is in a constant temperature state, a sample is added through an automatic feeding system, the sample forms a suspension state in the reaction furnace, and the temperature sensor is used for collecting thermal change in the suspension state reaction process, so that the thermal reaction process analysis of the sample in the suspension state is realized. The device has reasonable structural design and simple and convenient operation, realizes the rapid, accurate and dynamic detection of the thermal analysis process, and solves the defects of uneven heating and reaction caused by the static reaction of the sample in the traditional thermal analysis process, so that the analysis result is closer to the thermal reaction process of the material in the actual process.
Description
Technical Field
The utility model relates to a thermal analysis equipment technical field specifically is a suspension state thermal analysis test device.
Background
The thermal analysis technology can rapidly and accurately measure the changes of crystal transformation, melting, sublimation, adsorption, dehydration, decomposition and the like of substances, and is an important test means for the aspects of physical and chemical properties of inorganic, organic and high polymer materials. Thermal analysis techniques are widely used in the fields of physics, chemistry, chemical engineering, metallurgy, geology, building materials, fuels, light textiles, foods, biology and the like. Thermal analysis is one of the important means for studying reaction kinetics, and researchers at home and abroad often adopt means such as DTA/TG, DSG/TG and the like in the research of reaction kinetics. However, most of these test devices are static (such as thermal analysis balance, differential thermal analyzer, etc.) or semi-static (the sample is suspended or tiled on a screen plate and then suspended in an air flow), and these static or semi-static devices often have the problems that the sample is heated unevenly, the sensor measurement is greatly influenced by the sample thickness, etc. in the analysis kinetic reaction process, and the practicability of the device is limited.
In recent years, for the defects of the traditional analysis method, scholars at home and abroad also develop some suspended state thermal analysis devices, such as a high-temperature suspended state gas-solid reaction test bed developed by Nanjing industry university, wherein the device utilizes a gas cylinder as a gas source and collects physical quantities in the reaction process through a gas analyzer. The Tianjin cement industry design research institute Co., Ltd also developed a simulated decomposition furnace test system, a pulverized coal suspension combustion characteristic test furnace developed by Guangxi university for cement kilns, and the like. The suspension state reaction devices basically realize a dynamic analysis process, but the devices are mostly in a positive pressure state, the physical quantity in the reaction kinetic process is usually reaction gas as a measurement physical quantity, and due to the sensor and the system, the test has a lag problem and needs to be corrected.
The above background disclosure is only provided to aid understanding of the inventive concepts and solutions of the present invention, and it does not necessarily pertain to the prior art of this patent application, and it should not be used to assess the novelty and inventive aspects of this application without explicit evidence that such contents are disclosed at the filing date of this patent application.
Disclosure of Invention
The utility model discloses to the problem that current thermal analysis appearance exists, provide a suspension state thermal analysis test device. The device realizes the dynamic suspension process of a sample by utilizing a negative pressure principle, quickly measures the thermal physical quantity in the thermal reaction process in real time by utilizing a high-sensitivity thermal sensor, realizes full-automatic measurement, reduces external and artificial experimental errors, and makes the analysis result closer to the thermal reaction process of materials in the actual process.
In order to realize the above purpose, the utility model discloses a technical scheme as follows:
a suspended state thermal analysis test device comprises a negative pressure control system, a suspended reaction furnace system, an automatic feeding system, a constant temperature control system and a data acquisition system;
the negative pressure control system comprises a vacuum pump, a buffer gas storage tank and a three-way electromagnetic valve; gas is pumped by a vacuum pump and is buffered by a buffer gas storage tank, so that a constant-pressure and constant-flow process is realized; the air exhaust end of the vacuum pump is connected with the buffer air storage tank, and the air exhaust port of the vacuum pump is connected with the automatic feeding system through a three-way electromagnetic valve; an air source is provided for the automatic feeding system, and stable feeding of materials is guaranteed.
The suspension reaction furnace system comprises a suspension reaction furnace, a heating electric furnace wire and a heat insulation material; the periphery of the suspension reaction furnace is surrounded by heating electric furnace wires, and the periphery of the heating electric furnace wires is surrounded by heat insulation materials; the constant temperature control system is connected with a heating electric furnace wire of the suspension reaction furnace. The heat insulation material is a mullite fiber material.
The automatic feeding system comprises a feeding hopper, a material conveying air pipe and a feeding control valve; the feeding hopper is respectively connected with a material conveying air pipe and a feeding control valve, and the material conveying air pipe is connected with a vacuum pump. When the device is used, after the feeding control valve is closed, a sample is added from the feeding hopper, during feeding, gas in the exhaust port of the vacuum pump enters the three-way electromagnetic valve and is guided into the material conveying air pipe, at the moment, the feeding control valve is synchronously opened, and the sample enters the suspension reaction furnace through the material conveying air pipe. The on-off time of the three-way electromagnetic valve and the feeding control valve is controlled by a timer, so that the smooth conveying of the sample can be ensured, excessive gas cannot be brought in, and the airflow state in the furnace is excessively influenced. In order to reduce the pressure loss of the feeding gas, the included angle between the feeding gas pipe 2 and the feeding hopper 1 in the vertical direction is less than 60 degrees.
The data acquisition system mainly comprises a temperature sensor inserted into a sample of the suspension reaction furnace and a data acquisition card, wherein the temperature sensor is provided with more than two thermocouples, the thermocouples are longitudinally distributed in the reaction furnace to measure the longitudinal temperature distribution in the reaction furnace, and the positions of the thermocouples generally comprise a fixed bed area with higher sample concentration and a suspension bed area with less samples. The temperature change on the temperature sensor is transmitted into the upper computer software through a data acquisition card, and the data acquisition card is also connected with the feeding control valve.
The top end of the suspension reaction furnace is provided with
The vertical inlet of the mould opening is inserted into the temperature sensor, the horizontal inlet is connected with a buffer gas storage tank of the negative pressure system, and the top end of the mould opening is connected with the feeding hopper; as a feed port for the sample.
Furthermore, the whole suspension reaction furnace is of a cylindrical structure, the cylindrical part is a suspension area, and the bottom end of the suspension reaction furnace is of a cone structure.
Further, the ratio of the height L1 of the suspension area in the suspension reaction furnace to the height L2 of the cone is 6: 3.
Furthermore, the ratio of the diameter R of the upper opening of the cone to the diameter R of the lower opening of the cone is 10 to 7.
Furthermore, the vacuum pump is a speed-adjustable double-parallel negative pressure pump, and the adjustable function of the vacuum pump realizes negative pressure adjustment according to material characteristics, so that the suspension state of the material is ensured.
Furthermore, a protection layer is arranged at the port of the thermocouple. The protective layer may be an inert high temperature metal or an inorganic material. Preferably quartz glass, is used as the protective layer. If more zone temperatures in the suspension zone need to be measured, more thermocouples can be placed on the temperature sensor.
The test device is through the temperature in the invariable suspension reacting furnace of constant temperature control system, and the invariable suspension gas pressure source in rethread vacuum pump and the buffering gas holder realization suspension reacting furnace, and the sample drops into the suspension reacting furnace through automatic feeding system to be the suspension state, host computer software passes through the temperature variation in the temperature sensor collection reacting furnace this moment.
The constant temperature control system is realized in a constant pressure or constant current mode; the constant voltage is realized by a silicon controlled rectifier controller.
Compared with the prior art, the utility model discloses an advantage and beneficial effect do:
1. the device of the utility model adds the sample through the automatic feeding system under the constant temperature state, the sample forms the suspension state in the reaction furnace, the temperature sensor is used for collecting the thermal change in the suspension state reaction process, thereby the thermal reaction process analysis under the suspension state of the sample is achieved; the device overcomes the defects of uneven heating and reaction caused by static reaction of the sample in the traditional thermal analysis process, has reasonable structural design and simple and convenient operation, and realizes quick, accurate and dynamic detection of the thermal analysis process; so that the analysis result is closer to the thermal reaction process of the materials in the actual process.
2. This device adopts the negative pressure state at whole test procedure, and the air supply has realized the invariant of system's pressure after through buffering gas holder constant voltage, and adjustable aspiration pump has guaranteed that the system's negative pressure can be adjusted along with the different fineness of material, different proportion, and the device practicality is stronger.
3. The utility model discloses an automatic feeding system utilizes a small amount of gas and control valve to realize material automatic feed, has solved material feeding problem among the airtight negative pressure system, device simple structure, easy to maintain.
4. The device realizes the change of the temperature of the fixed bed and the suspension bed area by utilizing a multi-thermocouple mode, and can increase the distribution of the thermocouples in the longitudinal direction and better reflect the change condition of the whole suspension state temperature field.
Drawings
FIG. 1 is a schematic structural diagram of a suspended thermal analysis test apparatus;
FIG. 2 is a schematic structural view of a suspension reactor;
FIG. 3 is a graph showing the variation of the suspension combustion reaction process of pulverized coal;
FIG. 4 is a graph showing the thermal reaction process of CaCO3 in suspension.
1-feeding hopper, 2-material conveying gas pipe, 3-feeding control valve, 4-control box, 5-temperature sensor, 6-suspension reaction furnace, 7-heat preservation material, 8-heating electric furnace wire, 9-buffer gas storage tank and 10-vacuum pump.
Detailed Description
The present invention will be described in further detail with reference to the following embodiments. It should be emphasized that the following description is merely exemplary in nature and is not intended to limit the scope of the invention or its application.
Example 1
As shown in the attached drawing 1, the suspension state thermal analysis test device of the present invention comprises a negative pressure control system, a suspension reactor system, an automatic feeding system, a constant temperature control system and a data acquisition system;
the negative pressure control system comprises a vacuum pump 10, a buffer gas storage tank 9 and a three-way electromagnetic valve; gas is pumped by a vacuum pump 10 and is buffered by a buffer gas storage tank 9, so that a constant pressure and constant flow process is realized; the air exhaust end of the vacuum pump 10 is connected with the buffer air storage tank 9, and the air exhaust port of the vacuum pump 10 is connected with the automatic feeding system through a three-way electromagnetic valve; an air source is provided for the automatic feeding system, and stable feeding of materials is guaranteed.
The suspension reaction furnace system comprises a suspension reaction furnace 7, a heating electric furnace wire 8 and a heat insulation material 7; the periphery of the suspension reaction furnace is surrounded by a heating electric furnace wire 8, and the periphery of the heating electric furnace wire 8 is surrounded by a heat insulation material 7; and a constant temperature environment is provided for the whole suspension reaction furnace. The heat insulation material is a mullite fiber material.
The automatic feeding system comprises a feeding hopper 1, a material conveying air pipe 2 and a feeding control valve 3; the feeding hopper 1 is respectively connected with a material conveying air pipe 2 and a feeding control valve 3, and the material conveying air pipe 2 is connected with a vacuum pump 10. When the device is used, after the feeding control valve 3 is closed, a sample is added from the feeding hopper 1, during feeding, gas in an exhaust port of the vacuum pump 10 enters the three-way electromagnetic valve and is guided into the material conveying gas pipe 2, at the moment, the feeding control valve is synchronously opened, and the sample enters the suspension reaction furnace 7 through the material conveying gas pipe 2. The on-off time of the three-way electromagnetic valve and the feeding control valve 3 is controlled by a timer, so that the smooth conveying of samples can be ensured, excessive gas cannot be brought in, and the airflow state in the furnace is excessively influenced. In order to reduce the pressure loss of the feeding gas, the included angle between the feeding gas pipe 2 and the feeding hopper 1 in the vertical direction is less than 60 degrees.
The data acquisition system is mainly by inserting temperature sensor 5 and the data acquisition card of suspension reacting furnace sample, and temperature sensor 5 is equipped with two K type thermocouples, and one is located the sensor bottom, and another branch is parallel with cone department on the reacting furnace from sensor bottom 4cm, and the whole temperature sensor bottom is gone up the cone department with the reacting furnace, and the thermocouple of bottom just is in the more fixed bed region of sample concentration this moment, and goes up the thermocouple and be in the suspension bed region that sample concentration is low, and the last temperature variation of temperature sensor passes through data acquisition card and spreads into host computer software into, data acquisition card still is connected with the feeding control valve.
The constant temperature control system is controlled by the controllable silicon at constant voltage, but not limited to constant voltage control, and can also realize constant temperature control in a constant current mode. The constant temperature control system and the data acquisition card are arranged in the control box 4 and are connected with heating electric furnace wires around the suspension reaction furnace.
As shown in the attached figure 2, the whole suspension reaction furnace is of a cylindrical structure, the cylindrical part is a suspension area, and the bottom end of the suspension reaction furnace is of a cone structure; the top end of the suspension reaction furnace is provided with
A profile opening, longitudinal directionThe inlet is inserted with a temperature sensor, the transverse inlet is connected with a buffer gas storage tank 9 of a negative pressure system, and the top end of the transverse inlet is connected with a feeding hopper; as a feed port for the sample. The ratio of the height L1 of the suspension region in the suspension reaction furnace to the height L2 of the cone is 6: 3. The ratio of the diameter R of the upper opening of the cone to the diameter R of the lower opening of the cone is 10-7; at the moment, the sample can be in a continuous suspension state in the suspension furnace.
The test device is through the temperature in the invariable suspension reacting furnace of constant temperature control system, and the invariable suspension gas pressure source in rethread vacuum pump and the buffering gas holder realization suspension reacting furnace, and the sample drops into the suspension reacting furnace through automatic feeding system to be the suspended state, the host computer gathers the temperature variation of sample under the suspended state in real time through the thermocouple of arranging fixed bed and suspended bed in this moment.
Application example 1
The test device of the embodiment 1 is used for measuring the suspension state combustion characteristic of the coal powder, and the specific operation steps are as follows:
(1) controlling a power supply in the box, adjusting the silicon controlled rectifier controller to enable the voltage output to two ends of the electric furnace wire to be about 20v and the voltage to be constant for about 2h, acquiring that the temperature of the lowest end of the temperature sensor is near 650 ℃ by the data acquisition card, and finely adjusting the silicon controlled rectifier to enable the temperature in the furnace to be constant at 650 +/-1 ℃;
(2) closing the feeding control valve, accurately weighing 0.05 +/-0.001 g of pulverized coal, putting the pulverized coal into a feeding funnel, lightly knocking the wall of the funnel to enable the sample to completely fall on the upper end of the control valve, and plugging a rubber plug;
(3) adjusting the vacuum pump to ensure that the gas flow rate at the outlet of the vacuum pump is 0.4 +/-0.03L/min;
(4) when the temperature curve in the reaction furnace tends to be linear, setting a data storage path of an upper computer, wherein the acquisition time is 1min, starting an acquisition program, starting the acquisition program when the suspension furnace is required to be fed, pressing a feeding switch, inputting gas into an automatic feeding system by a vacuum pump through a material conveying gas pipe by a three-way electromagnetic valve, simultaneously opening a feeding control valve, and feeding a sample into the reaction furnace to realize an automatic feeding function;
(5) after the pulverized coal enters the reaction furnace, the computer synchronously acquires a thermoelectric even number value on the temperature sensor and synchronously displays a sample thermal reaction curve, and when the measurement time is up, the upper computer stops acquiring data and stores the data;
(6) after data acquisition is finished, the feeding switch is pressed all the time, gas is filled, the reacted materials are discharged from the lower opening of the reaction furnace, and the next test can be carried out after the temperature in the furnace is balanced. The temperature change curve of the coal powder suspension state combustion reaction process is shown in figure 3, wherein the solid line part in the figure is a fixed bed, and the dotted line is a suspension bed.
Application example 2
The test apparatus of example 1 was used to determine the thermal reaction process of limestone in suspended state, comprising the following steps:
(1) turning on a power supply in the control box, adjusting the silicon controlled rectifier controller to enable the voltage output to two ends of the electric furnace wire to be about 24v and the voltage to be constant for about 2h, acquiring that the temperature of the lowest end of the temperature sensor is near 850 ℃ by the data acquisition card, and finely adjusting the silicon controlled rectifier to enable the temperature in the furnace to be constant at 850 +/-1 ℃;
(2) adjusting the vacuum pump to ensure that the gas flow rate at the outlet of the vacuum pump is 0.5 +/-0.03L/min;
(3) grinding limestone until all the limestone passes through a 80-micron square-hole sieve, accurately weighing 0.05 +/-0.001 g of limestone, putting the limestone into a feeding funnel, lightly knocking the wall of the funnel to enable a sample to completely fall on the upper end of a feeding control valve, and plugging a rubber plug;
(4) when the temperature curve in the reaction furnace tends to be linear, setting a data storage path of an upper computer, wherein the acquisition time is 5min, starting an acquisition program when the suspension furnace is to be fed, pressing a feeding switch, inputting gas into an automatic feeding system by a vacuum pump through a material conveying gas pipe by a three-way electromagnetic valve, simultaneously opening a feeding control valve, and feeding a sample into the reaction furnace to realize an automatic feeding function;
(5) after the sample enters the reaction furnace, the computer synchronously acquires the thermoelectric even number value on the temperature sensor and synchronously displays the thermal reaction curve of the sample, and when the measurement time is up, the upper computer stops acquiring data and stores the data;
(6) after data acquisition is finished, the feeding switch is pressed all the time, gas is filled, the reacted materials are discharged from the lower opening of the reaction furnace, and the next test can be carried out after the temperature in the furnace is balanced. The data collected during the CaCO3 suspension state thermal reaction process are shown in the attached FIG. 4.
The foregoing is a more detailed description of the invention, taken in conjunction with specific/preferred embodiments, and it is not intended that the invention be limited to the specific embodiments shown and described. For those skilled in the art, without departing from the spirit of the present invention, several alternatives or modifications can be made to the described embodiments, and all such alternatives or modifications should be considered as falling within the scope of the present invention.
Claims (7)
1. The utility model provides a suspended state thermal analysis test device which characterized in that: the system comprises a negative pressure control system, a suspension reaction furnace system, an automatic feeding system, a constant temperature control system and a data acquisition system;
the negative pressure control system comprises a vacuum pump, a buffer gas storage tank and a three-way electromagnetic valve; the air exhaust end of the vacuum pump is connected with the buffer air storage tank, and the air exhaust port of the vacuum pump is connected with the automatic feeding system through a three-way electromagnetic valve;
the suspension reaction furnace system comprises a suspension reaction furnace, a heating electric furnace wire and a heat insulation material; the periphery of the suspension reaction furnace is surrounded by heating electric furnace wires, and the periphery of the heating electric furnace wires is surrounded by heat insulation materials; the constant temperature control system is connected with the heating electric furnace wire;
the automatic feeding system comprises a feeding hopper, a material conveying air pipe and a feeding control valve; the feeding hopper is respectively connected with a material conveying air pipe and a feeding control valve, and the material conveying air pipe is connected with a vacuum pump;
the data acquisition system consists of a temperature sensor inserted into a suspension reaction furnace sample and a data acquisition card, wherein the temperature sensor is provided with more than two thermocouples, and the thermocouples are longitudinally distributed in the suspension reaction furnace; the temperature change on the temperature sensor is transmitted into the upper computer software through a data acquisition card, and the data acquisition card is also connected with a feeding control valve;
the top end of the suspension reaction furnace is provided with
The vertical inlet of the opening is inserted with a temperature sensor, the horizontal inlet is connected with a buffer gas storage tank of a negative pressure control system, and the top end of the opening is connected with a feeding funnel.
2. The suspended state thermal analysis test device according to claim 1, characterized in that: the whole suspension reaction furnace is of a cylindrical structure, the cylindrical part is a suspension area, and the bottom end of the suspension reaction furnace is of a cone structure.
3. The suspended state thermal analysis test device according to claim 2, characterized in that: the ratio of the height L1 of the suspension region in the suspension reaction furnace to the height L2 of the cone is 6: 3.
4. The suspended state thermal analysis test device according to claim 2, characterized in that: the ratio of the diameter R of the upper opening of the cone to the diameter R of the lower opening is 10 to 7.
5. The suspended state thermal analysis test device according to claim 1, characterized in that: the vacuum pump is a speed-adjustable double-parallel negative pressure pump.
6. The suspended state thermal analysis test device according to claim 1, characterized in that: and a protective layer is arranged at the port of the thermocouple.
7. The suspended state thermal analysis test device according to claim 1, characterized in that: the constant temperature control system is a silicon controlled rectifier controller.
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| CN201920528316.6U CN210180966U (en) | 2019-04-18 | 2019-04-18 | Suspended state thermal analysis test device |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110057867A (en) * | 2019-04-18 | 2019-07-26 | 广西大学 | A kind of suspended state thermal analysis test device and test method |
| CN112946013A (en) * | 2021-01-14 | 2021-06-11 | 张贺邦 | Thermal analysis method for cast alloy |
-
2019
- 2019-04-18 CN CN201920528316.6U patent/CN210180966U/en not_active Withdrawn - After Issue
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110057867A (en) * | 2019-04-18 | 2019-07-26 | 广西大学 | A kind of suspended state thermal analysis test device and test method |
| CN110057867B (en) * | 2019-04-18 | 2024-01-12 | 广西大学 | Suspended state thermal analysis test device and test method |
| CN112946013A (en) * | 2021-01-14 | 2021-06-11 | 张贺邦 | Thermal analysis method for cast alloy |
| CN112946013B (en) * | 2021-01-14 | 2022-10-04 | 永嘉工力科技有限公司 | Thermal analysis method for casting alloy |
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Granted publication date: 20200324 Effective date of abandoning: 20240112 |
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| AV01 | Patent right actively abandoned | ||
| AV01 | Patent right actively abandoned |