CN110057867B - Suspended state thermal analysis test device and test method - Google Patents
Suspended state thermal analysis test device and test method Download PDFInfo
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- 238000012360 testing method Methods 0.000 title claims abstract description 37
- 238000002076 thermal analysis method Methods 0.000 title claims abstract description 28
- 238000010998 test method Methods 0.000 title claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims abstract description 81
- 239000000725 suspension Substances 0.000 claims abstract description 75
- 239000000463 material Substances 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 19
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- 238000003860 storage Methods 0.000 claims description 17
- 230000008859 change Effects 0.000 claims description 14
- 239000012774 insulation material Substances 0.000 claims description 9
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 7
- 229910052710 silicon Inorganic materials 0.000 claims description 7
- 239000010703 silicon Substances 0.000 claims description 7
- 239000011241 protective layer Substances 0.000 claims description 5
- 238000013500 data storage Methods 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 238000003825 pressing Methods 0.000 claims description 3
- 238000005070 sampling Methods 0.000 claims description 2
- 230000008569 process Effects 0.000 abstract description 15
- 238000004458 analytical method Methods 0.000 abstract description 8
- 230000003068 static effect Effects 0.000 abstract description 4
- 230000007547 defect Effects 0.000 abstract description 3
- 238000013461 design Methods 0.000 abstract description 3
- 238000001514 detection method Methods 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 29
- 239000003245 coal Substances 0.000 description 6
- 235000019738 Limestone Nutrition 0.000 description 5
- 239000006028 limestone Substances 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- 238000002485 combustion reaction Methods 0.000 description 4
- 230000001105 regulatory effect Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 239000004568 cement Substances 0.000 description 2
- 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
- 238000009826 distribution Methods 0.000 description 2
- 239000002657 fibrous material Substances 0.000 description 2
- 229910010272 inorganic material Inorganic materials 0.000 description 2
- 239000011147 inorganic material Substances 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229910052863 mullite Inorganic materials 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000003139 buffering effect Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 235000010216 calcium carbonate Nutrition 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
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- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/20—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity
- G01N25/48—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity on solution, sorption, or a chemical reaction not involving combustion or catalytic oxidation
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
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Abstract
The invention discloses a suspended state thermal analysis test device and a test method. The device is in a constant temperature state, samples are added through an automatic feeding system, the samples form a suspension state in the reaction furnace, and a temperature sensor is used for collecting thermal changes in the suspension state reaction process, so that analysis of the thermal reaction process of the samples in the suspension state is achieved. The device has reasonable structural design and simple and convenient operation, realizes rapid, accurate and dynamic thermal analysis process detection, and solves the defects of heating and uneven reaction caused by 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 invention relates to the technical field of thermal analysis equipment, in particular to a suspended state thermal analysis test device and a test method.
Background
The thermal analysis technology can rapidly and accurately measure the changes of the substances such as crystal form transformation, melting, sublimation, adsorption, dehydration, decomposition and the like, and is an important testing means for the physical and chemical properties of inorganic, organic and high polymer materials. Thermal analysis techniques are widely used in the fields of physics, chemistry, chemical industry, metallurgy, geology, building materials, fuels, light spinning, foods, biology, etc. Thermal analysis is one of important means for researching reaction kinetics, and researchers at home and abroad often adopt means such as DTA/TG, DSG/TG and the like in reaction kinetics research. However, most of these test devices are static (such as a thermal analysis balance, a differential thermal analyzer, etc.), or semi-static (the samples are suspended or laid on a screen plate and then suspended in an air flow), and these static or semi-static devices often have the problems that the samples are heated unevenly during the reaction process of analysis dynamics, and the sensor measurement is greatly affected by the thickness of the samples, so that the practicality of the device is limited.
In recent years, aiming at the defects of the traditional analysis method, students 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 industrial university, and the devices use a gas cylinder as a gas source and collect physical quantities in the reaction process through a gas analyzer. The Tianjin cement industry design institute Co., ltd also developed a simulated decomposing furnace test system, a pulverized coal suspension combustion characteristic test furnace for a cement kiln developed by Guangxi university, and the like. The suspended state reaction device basically realizes the dynamic analysis process, but most of the devices are in a positive pressure state, the physical quantity of the reaction dynamic process usually uses the reaction gas as the measurement physical quantity, and the test has a hysteresis problem due to the reasons of a sensor and a system and needs to be corrected.
The foregoing background is only for the purpose of providing an understanding of the inventive concepts and technical aspects of the present invention and is not necessarily prior art to the present application and is not intended to be used to evaluate the novelty and creativity of the present application in the event that no clear evidence indicates that such is already disclosed at the filing date of the present application.
Disclosure of Invention
The invention provides a suspended state thermal analysis test device and a test method aiming at the problems of the existing thermal analyzers. The device utilizes the negative pressure principle to realize the dynamic suspension process of the sample, utilizes the high-sensitivity heat sensor to rapidly measure the thermal physical quantity of the thermal reaction process in real time, realizes full-automatic measurement, reduces the external and artificial experimental errors, and ensures that the analysis result is closer to the thermal reaction process of the material in the actual process.
In order to achieve the above object, the present invention adopts the following technical scheme:
the 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 air storage tank and a three-way electromagnetic valve; the gas is pumped by a vacuum pump, and is buffered by a buffer gas storage tank to realize a constant pressure and constant flow process; 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 ensured.
The suspension reaction furnace system comprises a suspension reaction furnace, heating electric furnace wires and a heat insulation material; the periphery of the suspension reaction furnace is surrounded by a heating electric stove wire, and the periphery of the heating electric stove wire is surrounded by a heat insulation material; the heating wire is connected with a constant temperature control system. The heat insulation material is mullite fiber material.
The automatic feeding system comprises a feeding funnel, a feeding air pipe and a feeding control valve; the feeding funnel is connected with a material conveying air pipe and a feeding control valve respectively, and the material conveying air pipe is connected with a vacuum pump. When the feeding control valve is closed during use, a sample is added from the feeding funnel, and during feeding, gas in the exhaust port of the vacuum pump is introduced into the material conveying air pipe through the three-way electromagnetic valve, and 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 can not be brought in, and the gas flow state in the furnace is influenced excessively. In order to reduce the pressure loss of the feeding gas, the included angle between the feeding gas pipe 2 and the vertical direction of the feeding funnel 1 is smaller than 60 degrees.
The data acquisition system mainly comprises a temperature sensor and a data acquisition card, wherein the temperature sensor is inserted into a sample of a suspension reaction furnace, 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 position of the thermocouples generally comprises a fixed bed region with higher sample concentration and a suspension bed region with fewer samples. The temperature change on the temperature sensor is transmitted into the upper computer software through the 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 withThe longitudinal inlet is inserted into the temperature sensor, the transverse inlet is connected with a buffer air storage tank of the negative pressure system, and the top end of the buffer air storage tank is connected with the feeding funnel; 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 is of a cone structure.
Further, the ratio of the height L1 of the suspension area to the cone height L2 in the suspension reaction furnace is 6:3.
Further, 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.
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 the characteristics of materials, so that the suspension state of the materials is ensured.
Furthermore, a protective layer is arranged at the thermocouple port. The protective layer may be an inert high temperature metal or an inorganic material and the protective layer may be an inert high temperature metal or an inorganic material. Quartz glass height Wen Nianfu is preferred as a protective layer. If more areas of temperature in the suspended area need to be measured, more thermocouples can be arranged on the temperature sensor.
The test device is characterized in that the temperature in the suspension reaction furnace is constant through a constant temperature control system, a constant suspension air pressure source in the suspension reaction furnace is realized through a vacuum pump and a buffer air storage tank, a sample is put into the suspension reaction furnace through an automatic feeding system and is in a suspension state, and at the moment, upper computer software collects the temperature change in the reaction furnace through a temperature sensor.
The constant temperature control system is realized in a constant voltage or constant current mode; the constant voltage is controlled by a controllable silicon.
The invention relates to a testing method of a suspended state thermal analysis testing device, which comprises the following steps:
(1) Turning on the power supply of the negative pressure system and the constant temperature control system, and after 1-2h, reaching the gas flow rate of +/-0.03L/min and the temperature of +/-1 ℃ of the set value;
(2) Accurately weighing 0.05+/-0.001 g of a sample, placing the sample into a feeding funnel, measuring the sample sampling time and a data storage path through upper computer software, and starting data acquisition;
(3) Pressing a feeding button, adding a sample into the suspension reaction furnace through a feeding system, collecting temperature change in the furnace in real time by an upper computer, displaying the temperature change in upper computer software, and automatically storing data by the upper computer when the measured time reaches the set collection time;
(4) After data acquisition is completed, a feeding button is pressed all the time, gas is filled in, the reacted materials are discharged from the bottom end of the suspension reaction furnace, and the next test can be performed after the temperature in the furnace is balanced.
Compared with the prior art, the invention has the advantages that:
1. under the constant temperature state, the device adds the sample through the automatic feeding system, the sample forms a suspension state in the reaction furnace, and the temperature sensor is used for collecting the thermal change in the suspension state reaction process, so that the analysis of the thermal reaction process of the sample in the suspension state is achieved; the device solves the defects of heating and uneven reaction caused by static reaction of a sample in the traditional thermal analysis process, has reasonable structural design and simple and convenient operation, and realizes rapid, accurate and dynamic thermal analysis process detection; so that the analysis result is more similar to the thermal reaction process of the materials in the actual process.
2. The device adopts a negative pressure state in the whole testing process, the air source realizes the constancy of the system pressure after constant pressure is generated by the buffering air storage tank, and the adjustable air pump ensures that the system negative pressure can be adjusted along with different fineness and different specific gravity of materials, so that the device has stronger practicability.
3. The automatic feeding system designed by the invention realizes automatic feeding of materials by using a small amount of gas and a control valve, solves the problem of material feeding in a closed negative pressure system, and has the advantages of simple structure and easy maintenance.
4. The device realizes the temperature change of the fixed bed and the suspended bed region by utilizing a multi-thermocouple mode, and meanwhile, the distribution of thermocouples in the longitudinal direction can be increased, so that the change condition of the whole suspended state temperature field is better reflected.
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 pulverized coal suspended state combustion reaction process;
FIG. 4 is a graph showing the thermal reaction process in CaCO3 suspension.
The device comprises a 1-feeding funnel, a 2-gas delivery pipe, a 3-feeding control valve, a 4-control box, a 5-temperature sensor, a 6-suspension reaction furnace, a 7-heat insulation material, an 8-electric wire, a 9-buffer gas storage tank and a 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 in no way intended to limit the scope of the invention or its applications.
Example 1
As shown in the attached figure 1, the 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 10, a buffer air storage tank 9 and a three-way electromagnetic valve; the gas is pumped by a vacuum pump 10, and is buffered by a buffer gas storage tank 9 to realize a constant pressure and constant flow process; 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 ensured.
The suspension reaction furnace system comprises a suspension reaction furnace 7, heating electric furnace wires 8 and a heat insulation material 7; the periphery of the suspension reaction furnace is surrounded by a heating electric stove wire 8, and the periphery of the heating electric stove wire 8 is surrounded by a heat insulation material 7; providing a constant temperature environment for the whole suspension reaction furnace. The heat insulation material is mullite fiber material.
The automatic feeding system comprises a feeding funnel 1, a material conveying air pipe 2 and a feeding control valve 3; the feeding funnel 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 feeding control valve 3 is closed during use, a sample is added from the feeding funnel 1, and during feeding, gas in the exhaust port of the vacuum pump 10 is led into the material conveying air pipe 2 through the three-way electromagnetic valve, and at the moment, the feeding control valve is synchronously opened, and the sample enters the suspension reaction furnace 7 through the material conveying air 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 smooth conveying of samples can be ensured, excessive gas can not be brought in, and the gas flow state in the furnace is influenced excessively. In order to reduce the pressure loss of the feeding gas, the included angle between the feeding gas pipe 2 and the vertical direction of the feeding funnel 1 is smaller than 60 degrees.
The data acquisition system mainly comprises a temperature sensor 5 inserted into a sample of a suspension reaction furnace and a data acquisition card, wherein the temperature sensor 5 is provided with two K-type thermocouples, one branch is positioned at the bottom of the sensor, the other branch is positioned at the position 4cm away from the bottom of the sensor, the bottom of the whole temperature sensor is parallel to the upper cone opening of the reaction furnace, the thermocouple at the bottom is just positioned in a fixed bed area with more sample concentration, the upper thermocouple is positioned in a suspension bed area with low sample concentration, the temperature change on the temperature sensor is transmitted into upper computer software through the data acquisition card, and the data acquisition card is also connected with a feed control valve.
The constant temperature control system is controlled by a constant voltage of a silicon controlled rectifier, but is not limited to constant voltage control, and constant temperature control can be realized by 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 fig. 2, the whole suspension reaction furnace is of a cylindrical structure, the cylindrical part is a suspension area, and the bottom end is of a cone structure; the top end of the suspension reaction furnace is provided withThe longitudinal inlet is inserted into the temperature sensor, the transverse inlet is connected with the negative pressure system, and the top end of the transverse inlet is connected with the feeding funnel; as a feed port for the sample. The ratio of the height L1 of the suspension area to the cone height L2 in the suspension reaction furnace is 6:3. The ratio of the diameter R of the upper opening to the diameter R of the lower opening of the cone is 107; at this time, the sample can be in a continuous suspension state in the suspension furnace.
The test device is characterized in that the temperature in the suspension reaction furnace is constant through a constant temperature control system, a constant suspension air pressure source in the suspension reaction furnace is realized through a vacuum pump and a buffer air storage tank, a sample is put into the suspension reaction furnace through an automatic feeding system and is in a suspension state, and at the moment, an upper computer collects the temperature change of the sample in the suspension state in real time through thermocouples arranged on a fixed bed and a suspension bed.
Application example 1
The test device of example 1 was used to determine the combustion characteristics of pulverized coal in suspension, and the specific operation steps were as follows:
(1) The power supply in the control box regulates the silicon controlled rectifier controller to enable the voltage output to the two ends of the electric stove wire to be about 20v and constant voltage to be about 2 hours, at the moment, the data acquisition card acquires that the temperature of the lowest end of the temperature sensor is near 650 ℃, and the silicon controlled rectifier is finely adjusted to enable the temperature in the stove to be constant at 650+/-1 ℃;
(2) Closing a feeding control valve, accurately weighing 0.05+/-0.001 g of pulverized coal, putting into a feeding funnel, lightly knocking the wall of the funnel to enable a sample to completely fall on the upper end of the control valve, and then plugging a rubber plug;
(3) Regulating the vacuum pump to ensure that the gas flow rate of the vacuum pump is 0.4+/-0.03L/min;
(4) Setting a data storage path of an upper computer when a temperature curve in the reaction furnace tends to be straight, collecting for 1min, starting a collecting program, starting the collecting program when the suspension furnace is to be fed, pressing a feeding switch, at the moment, inputting gas into an automatic feeding system by a vacuum pump through a material conveying air pipe by a three-way electromagnetic valve, opening a feeding control valve at the same time, and enabling a sample to enter the reaction furnace to realize an automatic feeding function;
(5) After the coal powder enters the reaction furnace, synchronously acquiring thermocouple values on the temperature sensor by a computer, synchronously displaying a sample thermal reaction curve, stopping acquiring data by an upper computer after the measurement time is reached, and storing the data;
(6) After the data acquisition is completed, 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 performed when the temperature in the furnace is balanced. The temperature change curve of the pulverized coal suspension state combustion reaction process is shown in figure 3.
Application example 2
The test apparatus of example 1 was used to determine the thermal reaction process of limestone suspension comprising the steps of:
(1) The power supply in the control box is turned on, the silicon controlled rectifier controller is regulated, the voltage output to the two ends of the electric stove wire is about 24v, the constant voltage is about 2 hours, at the moment, the data acquisition card acquires that the temperature of the lowest end of the temperature sensor is near 850 ℃, and the silicon controlled rectifier is finely adjusted, so that the temperature in the stove is constant at 850+/-1 ℃;
(2) Regulating the vacuum pump to ensure that the gas flow rate of the vacuum pump is 0.5+/-0.03L/min;
(3) Grinding limestone until the limestone completely passes through an 80-micrometer square hole sieve, accurately weighing 0.05+/-0.001 g of limestone, putting the limestone into a feed hopper, lightly knocking the wall of the hopper to ensure that a sample completely falls on the upper end of a feed control valve, and then plugging a rubber plug;
(4) When the temperature curve in the reaction furnace tends to be straight, a data storage path of an upper computer is set, the acquisition time is 5min, when the suspension furnace is to be fed, an acquisition program is started, a feeding switch is pressed, at the moment, a vacuum pump inputs gas into an automatic feeding system through a gas transmission pipe by a three-way electromagnetic valve, a feeding control valve is simultaneously opened, and a sample enters the reaction furnace, so that an automatic feeding function is realized;
(5) After the sample enters the reaction furnace, the computer synchronously collects the thermocouple values on the temperature sensor, synchronously displays the thermal reaction curve of the sample, and after the measurement time is reached, the upper computer stops collecting data and stores the data;
(6) After the data acquisition is completed, 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 performed when the temperature in the furnace is balanced. CaCO (CaCO) 3 The data collected during the suspended thermal reaction is shown in figure 4.
The foregoing is a further detailed description of the invention in connection with specific/preferred embodiments, and is not intended to limit the practice of the invention to such description. It will be apparent to those skilled in the art that several alternatives or modifications can be made to the described embodiments without departing from the spirit of the invention, and these alternatives or modifications should be considered to be within the scope of the invention.
Claims (9)
1. The utility model provides a suspended state thermal analysis test device which characterized in that: 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 air 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, heating electric furnace wires and a heat insulation material; the periphery of the suspension reaction furnace is surrounded by a heating electric stove wire, and the periphery of the heating electric stove wire is surrounded by a heat insulation material; the heating electric stove wire is connected with a constant temperature control system;
the automatic feeding system comprises a feeding funnel, a feeding air pipe and a feeding control valve; the feeding funnel 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 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 which are distributed in the reaction furnace in a longitudinal mode; the temperature change on the temperature sensor is transmitted into 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 withThe longitudinal inlet is inserted into the temperature sensor, the transverse inlet is connected with a buffer air storage tank of the negative pressure control system, and the top end of the buffer air storage tank is connected with the feeding funnel.
2. The suspended state thermal analysis test device according to claim 1, wherein: the whole cylinder structure that is of suspension reaction stove, cylinder part is the suspension region, and the bottom is the cone structure.
3. The suspended state thermal analysis test device according to claim 2, wherein: the ratio of the height L1 of the suspension area to the cone height L2 in the suspension reaction furnace is 6:3.
4. The suspended state thermal analysis test device according to claim 2, wherein: the ratio of the diameter R of the upper opening to the diameter R of the lower opening of the cone is 10-7.
5. The suspended state thermal analysis test device according to claim 1, wherein: the vacuum pump is a speed-adjustable double-parallel negative pressure pump.
6. The suspended state thermal analysis test device according to claim 1, wherein: and a protective layer is arranged at the thermocouple port.
7. A method of testing a suspended thermal analysis testing apparatus according to claim 1, wherein: the test device is used for controlling the temperature in the constant suspension reaction furnace through the constant temperature control system, realizing a constant suspension air pressure source in the suspension reaction furnace through the vacuum pump and the buffer air storage tank, and throwing the sample into the suspension reaction furnace through the automatic feeding system and being in a suspension state, wherein the upper computer is used for collecting the temperature change of the sample in the suspension state in real time through the thermocouple.
8. The method for testing a suspended thermal analysis testing apparatus according to claim 7, wherein: the constant temperature control system is realized in a constant voltage or constant current mode; the constant voltage is controlled by a controllable silicon controller.
9. The method for testing a suspended thermal analysis testing apparatus according to claim 7, wherein: the method comprises the following steps:
(1) Turning on the power supply of the negative pressure control system and the constant temperature control system, and after 1-2h, reaching the gas flow rate of the set value +/-0.03L/min, and reaching the temperature of the set value +/-1 ℃;
(2) Accurately weighing 0.05+/-0.001 g of a sample, placing the sample into a feeding funnel, measuring the sample sampling time and a data storage path through upper computer software, and starting data acquisition;
(3) Pressing a feeding button, adding a sample into the suspension reaction furnace through a feeding system, collecting temperature change in the furnace in real time by an upper computer, displaying the temperature change in upper computer software, and automatically storing data by the upper computer when the measured time reaches the set collection time;
(4) After data acquisition is completed, a feeding button is pressed all the time, gas is filled in, the reacted materials are discharged from the bottom end of the suspension reaction furnace, and the next test can be performed after the temperature in the furnace is balanced.
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