CN110057867A - A kind of suspended state thermal analysis test device and test method - Google Patents

A kind of suspended state thermal analysis test device and test method Download PDF

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CN110057867A
CN110057867A CN201910312286.XA CN201910312286A CN110057867A CN 110057867 A CN110057867 A CN 110057867A CN 201910312286 A CN201910312286 A CN 201910312286A CN 110057867 A CN110057867 A CN 110057867A
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suspended state
sample
reaction furnace
suspension reaction
furnace
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CN110057867B (en
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柏秀奎
曹德光
封广生
方盛南
雷彩霞
陈亚菲
林华
陈春燕
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Guangxi Huaguan Building Materials Co.,Ltd.
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Guangxi University
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    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N25/00Investigating or analyzing materials by the use of thermal means
    • G01N25/20Investigating 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
    • G01N25/48Investigating 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
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E30/00Energy generation of nuclear origin
    • Y02E30/30Nuclear fission reactors

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Abstract

The invention discloses a kind of suspended state thermal analysis test device and test methods comprising vacuum control system, suspension reaction furnace system, automatic feeding system, thermostatic control system and data collection system.Sample is added under temperature constant state, through automatic feeding system in the present apparatus, and sample forms suspended state in reacting furnace therewith, using the thermal change in temperature sensor acquisition suspended state reaction process, to reach to the thermal process reactor analysis under sample suspended state.The present apparatus is reasonable in design, easy to operate, realize quick, accurate, dynamic heat analysis process detection, solves the disadvantage that sample static reaction bring is heated and reaction is uneven during traditional heat analysis, so that thermal process reactor of the analysis result closer to material during actual process.

Description

A kind of suspended state thermal analysis test device and test method
Technical field
The present invention relates to thermal analyzer technical field, specifically a kind of suspended state thermal analysis test device and test side Method.
Background technique
Thermoanalysis technology can rapidly and accurately measure the change such as crystal transfer, melting, distillation, absorption, dehydration, decomposition of substance Change, to inorganic, organic and high molecular material physics and chemical property aspect, is important means of testing.Thermoanalysis technology exists It is used widely in the fields such as physics, chemistry, chemical industry, metallurgy, geology, building materials, fuel, light textile, food, biology.Heat analysis is Study one of the important means of kinetics, researchers at home and abroad in Reaction kinetics research, frequently with DTA/TG, The means such as DSG/TG.But these experimental rigs are static (such as heat analysis balance, differential thermal analyzer) or semi-static mostly (hang sample or tile on web plate, resuspend in air-flow), these static or semi-static devices are reacted in analytic dynamics Often there is sample uneven heating in the process, the problems such as sensor measurement is affected by thickness of sample, limits the type equipment Practicability.
It is directed to the defect of traditional analysis in recent years, domestic and foreign scholars also develop some suspended state apparatus for thermal analysis, Such as the high temperature suspended state gas-solid reaction testing stand that Nanjing University of Technology develops, device passes through gas point using gas cylinder as gas source The physical quantity of analyzer acquisition reaction process.Tianjin Design Inst. of Cement Industry Co., Ltd also develops simulation dore furnace test System, cement kiln coal dust suspension combustion attribute testing furnace etc. of Guangxi University's exploitation.These suspended state reaction units are substantially Realize dynamic analysis process, but this device commonly uses barotropic state mostly, the physical quantity of kinetics process is often with reaction gas Body is as measurement physical quantity, due to sensor and system, tests there are lag issues, needs to correct.
The disclosure of background above technology contents is only used for auxiliary and understands inventive concept and technical solution of the invention, not The prior art for necessarily belonging to present patent application shows above content in the applying date of present patent application in no tangible proof In the case where having disclosed, above-mentioned background technique should not be taken to the novelty and creativeness of evaluation the application.
Summary of the invention
The present invention existing thermal analyzer there are aiming at the problem that, a kind of suspended state thermal analysis test device and test side are provided Method.The present apparatus is to realize the dynamic suspension process of sample using principle of negative pressure, is surveyed quickly, in real time using highly sensitive heat sensor Calorimetric reaction process ermal physics amount, and all automatic measurement is realized, extraneous and artificial experimental error is reduced, so that analysis result is more The thermal process reactor of material during close to actual process.
In order to achieve the goal above, The technical solution adopted by the invention is as follows:
A kind of suspended state thermal analysis test device comprising vacuum control system, suspension reaction furnace system, automatic charging system System, thermostatic control system and data collection system;
The vacuum control system includes vacuum pump, buffering air accumulator and three-way magnetic valve;Gas is extracted by vacuum pump, warp It buffers air accumulator and carries out air-flow buffer, realize constant pressure and flow process;The pumping end of the vacuum pump is connect with buffering air accumulator, very The exhaust outlet of sky pump is connect by three-way magnetic valve with automatic feeding system;Gas source is provided for automatic feeding system, guarantees material Stablize charging.
The suspension reaction furnace system includes suspension reaction furnace, heating electric-oven silk and thermal insulation material;The suspension reaction furnace Surrounding is around heating electric-oven silk, and the surrounding of heating electric-oven silk is around thermal insulation material;The heating electric-oven silk and thermostatic control system It is connected.The thermal insulation material is mullite fiber material.
The automatic feeding system includes loading hopper, conveying tracheae and inlet control valve;The loading hopper respectively with Conveying tracheae and inlet control valve are connected, and the conveying tracheae is controlled to a vacuum pump.After closing inlet control valve when use, sample It is added by loading hopper, when charging, the gas in vacuum pump exhaust port imports conveying tracheae into three-way magnetic valve, at this time charging control Valve processed is synchronous to be opened, and sample enters in suspension reaction furnace via conveying tracheae.When the on-off of three-way magnetic valve and inlet control valve Between controlled by timer, it is ensured that the conveying of sample smoothly and will not bring excessive gas into, excessive to influence gas stream in the stove state.For Reduce feeding gas crushing, the angle between 1 vertical direction of conveying tracheae 2 and loading hopper should be less than 60 °.
The data collection system is mainly by the temperature sensor and data collecting card of insertion suspension reaction furnace sample, temperature Sensor is equipped with more than two thermocouples, and thermocouple is distributed in reacting furnace in a longitudinal fashion, longitudinal in reacting furnace to measure Temperature Distribution, the suspension bed area that the position of general thermocouple should be less comprising the higher fixed bed region of sample concentration and sample Domain.Temperature change on temperature sensor is passed to upper computer software by data collecting card, the data collecting card also with charging Control valve connection.
Suspension reaction furnace roof end is equipped withType opening, longitudinal entrance are inserted into temperature sensor, and lateral entrance connects negative The buffering air accumulator of pressure system, top are simultaneously connect with loading hopper;Feed inlet as sample.
Further, the suspension reaction furnace generally cylindrical structure, the cylindrical portion are suspension region, bottom end For cone structure.
Further, the ratio of the height L1 and cone height L2 in suspension region are 6:3 in the suspension reaction furnace.
Further, the ratio between the cone back cut diameter R and lower port diameter r are 10~7.
Further, the vacuum pump is adjustable speed two-in-parallel negative pressure pump, and the adjustable function of vacuum pump is realized according to material Characteristic carries out the adjusting of negative pressure pressure, guarantees the suspended state of material.
Further, protective layer is equipped at the thermocouple port.Protective layer can be inertia high-temperature metal or inorganic material Material, protective layer can be inertia high-temperature metal or inorganic material.Preferably quartz glass high temperature sticks as protective layer.If needing to survey Determine more multi-zone temperature in suspension region, more multiple thermocouple can be disposed on temperature sensor.
Experimental rig of the present invention is then to pass through vacuum by the temperature in the constant suspension reaction furnace of thermostatic control system Pump and buffering air accumulator realize that the constant suspension pneumatic supply in suspension reaction furnace, sample put into suspension reaction through automatic feeding system It in furnace, and is in suspended state, upper computer software acquires the temperature change in reacting furnace by temperature sensor at this time.
The thermostatic control system is realized by constant pressure or constant current form;The constant pressure passes through silicon-controlled realization constant pressure control System.
The test method of suspended state thermal analysis test device of the present invention, includes the following steps:
(1) negative pressure system and thermostatic control system power supply are opened, reach after 1-2h gas flow rate setting value ± 0.03L/min, temperature reaches in setting value ± 1 DEG C;
(2) 0.05 ± 0.001g of accurate weighing sample, is put into loading hopper, measures sample by upper computer software Time and data storing path, and log-on data acquires;
(3) charging button is pressed, sample is added in suspension reaction furnace through feeding system, and host computer acquires in-furnace temperature change in real time Change, and be shown in upper computer software, when time of measuring reaches setting acquisition time, host computer automatically saves data;
(4) after the completion of data acquisition, charging button is pinned always, pours into gas, reacted material is by suspension reaction furnace Bottom end discharge, balances to in-furnace temperature, can be tested next time.
Compared with prior art, it advantages of the present invention and has the beneficial effect that
1, apparatus of the present invention are under temperature constant state, are added sample through automatic feeding system, the sample shape in reacting furnace therewith At suspended state, using the thermal change in temperature sensor acquisition suspended state reaction process, to reach under sample suspended state Thermal process reactor analysis;Solve during traditional heat analysis that sample static reaction bring is heated and reaction is uneven lacks Point, while apparatus structure design is reasonable, easy to operate, realizes quick, accurate, dynamic heat analysis process detection;So that Thermal process reactor of the analysis result closer to material during actual process.
2, the present apparatus uses negative pressure state in entire test process, and gas source is by realizing system after buffering air accumulator constant pressure Pressure it is constant, and adjustable aspiration pump ensure that system negative pressure can be adjusted with material different fineness, different specific weight, and device is real It is stronger with property.
3, the automatic feeding system that the present invention designs realizes material automatic feed using a small amount of gas and control valve, solves Material feed problems in closed negative pressure system, apparatus structure is simple, easy to maintain.
4, the present apparatus realizes the variation of fixed bed and suspension bed regional temperature in the way of multiple thermocouple, while can increase The distribution of thermocouple in the longitudinal direction preferably reflects the situation of change in entire suspended state temperature field.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of suspended state thermal analysis test device;
Fig. 2 is the structural schematic diagram of suspension reaction furnace;
Fig. 3 is the curvilinear motion of coal dust suspended state combustion reaction process;
Fig. 4 is the curvilinear motion of CaCO3 suspended state thermal process reactor.
1- loading hopper, 2- conveying tracheae, 3- inlet control valve, 4- control cabinet, 5- temperature sensor, 6- suspension reaction Furnace, 7- thermal insulation material, 8- electric furnace heating wire, 9- buffer air accumulator, 10- vacuum pump.
Specific embodiment
Invention is further described in detail With reference to embodiment.It is emphasized that following the description is only It is merely exemplary, the range and its application being not intended to be limiting of the invention.
Embodiment 1
As shown in Fig. 1, suspended state thermal analysis test device of the present invention comprising vacuum control system suspends instead Answer furnace system, automatic feeding system, thermostatic control system and data collection system;
The vacuum control system includes vacuum pump 10, buffering air accumulator 9 and three-way magnetic valve;Gas is taken out by vacuum pump 10 It takes, carries out air-flow buffer through buffering air accumulator 9, realize constant pressure and flow process;The pumping end of the vacuum pump 10 and buffering gas storage Tank 9 connects, and the exhaust outlet of vacuum pump 10 is connect by three-way magnetic valve with automatic feeding system;Gas is provided for automatic feeding system Source, guarantee material stablizes charging.
The suspension reaction furnace system includes suspension reaction furnace 7, heating electric-oven silk 8 and thermal insulation material 7;The suspension reaction Furnace surrounding is around heating electric-oven silk 8, and the surrounding of heating electric-oven silk 8 is around thermal insulation material 7;It is provided for entire suspension reaction furnace constant Temperature environment.The thermal insulation material is mullite fiber material.
The automatic feeding system includes loading hopper 1, conveying tracheae 2 and inlet control valve 3;The loading hopper 1 divides It is not connected with conveying tracheae 2 and inlet control valve 3, the conveying tracheae 2 is connect with vacuum pump 10.Charging control is closed when use After valve 3, sample is added by loading hopper 1, and when charging, the gas in 10 exhaust outlet of vacuum pump imports conveying gas into three-way magnetic valve Pipe 2, inlet control valve is synchronous at this time opens, and sample enters in suspension reaction furnace 7 via conveying tracheae 2.Three-way magnetic valve and into The make-and-break time of material control valve 3 is controlled by timer, it is ensured that the conveying of sample is smooth and will not bring excessive gas, excessive shadow into Ring gas stream in the stove state.To reduce feeding gas crushing, the angle between 1 vertical direction of conveying tracheae 2 and loading hopper is answered small In 60 °.
The data collection system is mainly by the temperature sensor 5 and data collecting card of insertion suspension reaction furnace sample, temperature Degree sensor 5 is set there are two K-type thermocouple, and one is located at sensor base, and the place another offset distance sensor base 4cm is entire warm It is parallel at cone mouth on reacting furnace to spend sensor base, at this time the thermocouple of the bottom fixed bed more just at sample concentration Region, and upper thermocouple is in the low suspension bed region of sample concentration, the temperature change on temperature sensor is acquired by data Block incoming upper computer software, the data collecting card is also connect with inlet control valve.
The thermostatic control system is not limited only to Isobarically Control by silicon-controlled Isobarically Control, can also pass through constant current Mode realizes thermostatic control.The thermostatic control system and data collecting card are located in control cabinet 4, and with suspension reaction furnace four The heating electric-oven silk in week is connected.
As shown in Fig. 2, the suspension reaction furnace generally cylindrical structure, the cylindrical portion are suspension region, Bottom end is cone structure;Suspension reaction furnace roof end is equipped withType opening, longitudinal entrance are inserted into temperature sensor, lateral entrance Negative pressure system is connect, top is simultaneously connect with loading hopper;Feed inlet as sample.The height in suspension region in the suspension reaction furnace The ratio for spending L1 and cone height L2 is 6:3.The ratio between the cone back cut diameter R and lower port diameter r are 10~7;Sample at this time It can be in sustained suspension state in shower furnace.
Experimental rig of the present invention is then to pass through vacuum by the temperature in the constant suspension reaction furnace of thermostatic control system Pump and buffering air accumulator realize that the constant suspension pneumatic supply in suspension reaction furnace, sample put into suspension reaction through automatic feeding system It in furnace, and is in suspended state, host computer acquires sample by being placed in the thermocouple of fixed bed and suspension bed in real time and suspending at this time Temperature change under state.
Application Example 1
Coal dust suspended state combustion characteristics is measured using the experimental rig of embodiment 1, specific steps are as follows:
(1) power supply in control cabinet adjusts controllable silicon controller, so that output is about 20v to the voltage at electric furnace heating wire both ends, Constant pressure about 2h, data collecting card collects temperature sensor bottom temperature near 650 DEG C at this time, and fine tuning is silicon-controlled, makes furnace Interior temperature is constant at 650 ± 1 DEG C;
(2) inlet control valve is closed, accurate weighing 0.05 ± 0.001g of coal dust is put into loading hopper, gently taps leakage Headwall makes sample fall within control valve upper end completely, then rubber stopper beyond the Great Wall;
(3) vacuum pump is adjusted, makes vacuum pump outlet gas flow rate in 0.4 ± 0.03L/min;
(4) tend to straight line to the temperature curve in reacting furnace, the data storing path of host computer is set, acquisition time is 1min starts capture program, when shower furnace to be charging, starts capture program, presses charging switch, vacuum pump is by three at this time Gas is inputted gas to automatic feeding system through conveying tracheae by three-way electromagnetic valve, and inlet control valve opens simultaneously, and sample enters anti- It answers in furnace, realizes automatic feed function;
(5) after coal dust enters reacting furnace, thermoelectricity even number value on computer synchronous acquisition temperature sensor, and simultaneous display Sample thermal response curve, after reaching time of measuring, host computer stops data collection, and saves;
(6) after the completion of data acquisition, charging switch is pinned always, pours into gas, reacted material is by mouth under reacting furnace Discharge is balanced to in-furnace temperature, can be tested next time.The temperature variation curve of coal dust suspended state combustion reaction process is for example attached Shown in Fig. 3.
Application Example 2
Lime stone suspended state thermal process reactor is measured using the experimental rig of embodiment 1, is included the following steps:
(1) power supply in control cabinet is opened, controllable silicon controller is adjusted, making to export to electric furnace heating wire both end voltage is about 24v, Constant pressure about 2h, data collecting card collects temperature sensor bottom temperature near 850 DEG C at this time, and fine tuning is silicon-controlled, makes furnace Interior temperature is constant at 850 ± 1 DEG C;
(2) vacuum pump is adjusted, makes vacuum pump outlet gas flow rate in 0.5 ± 0.03L/min;
(3) agstone is milled to all through 80 microns of square hole screens, accurately weighs 0.05 ± 0.001g lime stone, is put into In loading hopper, hopper walls are gently tapped, sample is made to fall within inlet control valve upper end completely, then rubber stopper beyond the Great Wall;
(4) tend to straight line to the temperature curve in reacting furnace, the data storing path of host computer is set, acquisition time is 5min starts capture program when shower furnace to be charging, presses charging switch, vacuum pump is by three-way magnetic valve by gas at this time Body inputs gas to automatic feeding system through conveying tracheae, and inlet control valve opens simultaneously, and sample enters in reacting furnace, realizes certainly Dynamic material feeding function;
(5) after sample enters reacting furnace, thermoelectricity even number value on computer synchronous acquisition temperature sensor, and simultaneous display Sample thermal response curve, after reaching time of measuring, host computer stops data collection, and saves;
(6) after the completion of data acquisition, charging switch is pinned always, pours into gas, reacted material is by mouth under reacting furnace Discharge is balanced to in-furnace temperature, can be tested next time.CaCO3The collected data of suspended state thermal process reactor such as attached drawing 4 It is shown.
The above content is combine it is specific/further detailed description of the invention for preferred embodiment, cannot Assert that specific implementation of the invention is only limited to these instructions.General technical staff of the technical field of the invention is come It says, without departing from the inventive concept of the premise, some replacements or modifications can also be made to the embodiment that these have been described, And these substitutions or variant are regarded as belonging to the scope of protection of the present invention.

Claims (9)

1. a kind of suspended state thermal analysis test device, it is characterised in that: including vacuum control system, suspension reaction furnace system, from Dynamic feeding system, thermostatic control system and data collection system;
The vacuum control system includes vacuum pump, buffering air accumulator and three-way magnetic valve;The pumping end of the vacuum pump and slow Air accumulator connection is rushed, the exhaust outlet of vacuum pump is connect by three-way magnetic valve with automatic feeding system;
The suspension reaction furnace system includes suspension reaction furnace, heating electric-oven silk and thermal insulation material;The suspension reaction furnace surrounding Around heating electric-oven silk, the surrounding of heating circuit silk is around thermal insulation material;The heating electric-oven silk is connected with thermostatic control system;
The automatic feeding system includes loading hopper, conveying tracheae and inlet control valve;The loading hopper respectively with conveying Tracheae and inlet control valve are connected, and the conveying tracheae is controlled to a vacuum pump;
The data collection system is mainly by the temperature sensor and data collecting card of insertion suspension reaction furnace sample, temperature sensing Device is equipped with more than two thermocouples, and thermocouple is distributed in reacting furnace in a longitudinal fashion;Temperature change on temperature sensor It is passed to upper computer software by data collecting card, the data collecting card is also connect with inlet control valve;
Suspension reaction furnace roof end is equipped withType opening, longitudinal entrance are inserted into temperature sensor, and lateral entrance meets negative pressure system The buffering air accumulator of system, top are simultaneously connect with loading hopper.
2. suspended state thermal analysis test device according to claim 1, it is characterised in that: the suspension reaction furnace is generally round Column structure, the cylindrical portion are suspension region, and bottom end is cone structure.
3. suspended state thermal analysis test device according to claim 2, it is characterised in that: floating zone in the suspension reaction furnace The ratio of the height L1 and cone height L2 in domain are 6:3.
4. suspended state thermal analysis test device according to claim 2, it is characterised in that: the cone back cut diameter R is under The ratio between mouth diameter r is 10~7.
5. suspended state thermal analysis test device according to claim 1, it is characterised in that: the vacuum pump is that adjustable speed is double simultaneously Join negative pressure pump.
6. suspended state thermal analysis test device according to claim 1, it is characterised in that: be equipped with and protect at the thermocouple port Sheath.
7. a kind of test method of suspended state thermal analysis test device as described in claim 1, it is characterised in that: experimental rig is logical The temperature in the constant suspension reaction furnace of thermostatic control system is crossed, then is realized in suspension reaction furnace by vacuum pump and buffering air accumulator Constant suspension pneumatic supply, sample is in suspended state through in automatic feeding system investment suspension reaction furnace, and host computer is logical at this time It crosses thermocouple and acquires temperature change of the sample under suspended state in real time.
8. the test method of suspended state thermal analysis test device according to claim 7, it is characterised in that: the thermostatic control System is realized by constant pressure or constant current form;The constant pressure realizes Isobarically Control by controllable silicon controller.
9. the test method of suspended state thermal analysis test device according to claim 7, it is characterised in that: including walking as follows It is rapid:
(1) negative pressure system and thermostatic control system power supply are opened, gas flow rate is reached after 1-2h in setting value ± 0.03L/ Min, temperature reach setting value ± 1 DEG C;
(2) 0.05 ± 0.001g of accurate weighing sample, is put into loading hopper, measures the sample time by upper computer software With data storing path, and log-on data acquire;
(3) charging button is pressed, sample is added in suspension reaction furnace through feeding system, and host computer acquires in-furnace temperature variation in real time, And be shown in upper computer software, when time of measuring reaches setting acquisition time, host computer automatically saves data;
(4) after the completion of data acquisition, charging button is pinned always, pours into gas, reacted material is by suspension reaction furnace bottom end Discharge is balanced to in-furnace temperature, can be tested next time.
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JPH05346427A (en) * 1992-02-27 1993-12-27 Nippon Steel Corp Method and apparatus for analyzing constituent of metal
CN1776421A (en) * 2005-12-01 2006-05-24 武汉理工大学 Device for measuring reaction rateof flash magnetized calcination for refractory iron oxide ore
CN104458805A (en) * 2014-12-18 2015-03-25 广西大学 Pulverized coal suspension combustion characteristic trial furnace for cement kiln
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110514009A (en) * 2019-08-30 2019-11-29 西安建筑科技大学 A kind of shower furnace of achievable constant temperature

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