CN108489853A - A kind of microwave thermogravimetric response analysis system - Google Patents
A kind of microwave thermogravimetric response analysis system Download PDFInfo
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- CN108489853A CN108489853A CN201810431482.4A CN201810431482A CN108489853A CN 108489853 A CN108489853 A CN 108489853A CN 201810431482 A CN201810431482 A CN 201810431482A CN 108489853 A CN108489853 A CN 108489853A
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- 238000004458 analytical method Methods 0.000 title claims abstract description 27
- 230000004044 response Effects 0.000 title claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 65
- 238000010438 heat treatment Methods 0.000 claims abstract description 59
- 239000000463 material Substances 0.000 claims abstract description 43
- 238000000197 pyrolysis Methods 0.000 claims abstract description 21
- 230000008859 change Effects 0.000 claims abstract description 18
- 230000005484 gravity Effects 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 7
- 230000008569 process Effects 0.000 claims abstract description 6
- 239000003054 catalyst Substances 0.000 claims abstract description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 87
- 239000010453 quartz Substances 0.000 claims description 81
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 22
- 239000003708 ampul Substances 0.000 claims description 15
- 229910052757 nitrogen Inorganic materials 0.000 claims description 11
- 238000010586 diagram Methods 0.000 claims description 10
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- 238000002474 experimental method Methods 0.000 claims description 6
- 238000013461 design Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 238000005979 thermal decomposition reaction Methods 0.000 claims description 5
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- 230000002457 bidirectional effect Effects 0.000 claims description 3
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- 238000012544 monitoring process Methods 0.000 claims description 3
- 238000003199 nucleic acid amplification method Methods 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 238000005259 measurement Methods 0.000 claims description 2
- 230000002093 peripheral effect Effects 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 239000000376 reactant Substances 0.000 claims description 2
- 230000002463 transducing effect Effects 0.000 claims description 2
- 239000000047 product Substances 0.000 claims 3
- 239000007795 chemical reaction product Substances 0.000 claims 1
- 239000004615 ingredient Substances 0.000 claims 1
- 239000004575 stone Substances 0.000 claims 1
- 238000002411 thermogravimetry Methods 0.000 abstract description 4
- 238000012933 kinetic analysis Methods 0.000 abstract description 3
- 230000007246 mechanism Effects 0.000 abstract description 3
- 238000000926 separation method Methods 0.000 abstract description 2
- 230000005494 condensation Effects 0.000 abstract 1
- 238000009833 condensation Methods 0.000 abstract 1
- 239000010815 organic waste Substances 0.000 description 12
- 239000002028 Biomass Substances 0.000 description 3
- 230000004913 activation Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
Abstract
The present invention relates to microwave-heating technical fields, refer in particular to a kind of microwave thermogravimetric response analysis system.The analysis system includes thermocouple temperature sensor, gravity sensor, control circuit, display module, chemical reaction system material pyrolysis section, appendage, magnetron and computer.Microwave power of the present invention is adjustable, reaction temperature and weight change data in high-acruracy survey material microwave pyrolytic process, material microwave-heating is reacted and carries out thermogravimetric analysis and Kinetic analysis, external chemical reaction module can realize product condensation separation, catalyst reforms upgrading, also can external other analytical instrument realize the Analysis on Mechanism to material pyrolytic reaction.
Description
Technical field
The present invention relates to microwave-heating technical fields, more particularly to a kind of microwave-heating organic matter that is used for carry out thermogravimetric analysis
And its kinetics and mechanisms analysis.
Background technology
Microwave is a kind of high frequency waves, is that the molecule of heated material occurs in high frequency magnetic field when using microwave heating substance
Vibrations, intermolecular mutual collision rub and generate thermal energy, so that the mass temperature heated is increased, the transmission of heat is by molecule
It transmits from inside to outside, this characteristic based on microwave is more next using technologies such as microwave-heating organic wastes such as biomass, waste plastics
More get more and more people's extensive concerning.Due to fossil energy non-renewable and price it is surging so as to alternatively regenerating combustion
Expect that the demand of resource is more and more stronger.The yield of China's organic waste such as biomass, waste plastics etc. is huge, but its utilization rate
Low, what is utilized after technical finesse is even more fewer and fewer.Compared to traditional electrical heating, microwave-heating organic waste is not only
It can only promote to chemically react, and reaction condition is mild, capacity usage ratio is high.In to material pyrolytic reaction research process not
The real-time change for studying temperature is only needed to also need to the mistake that knowing reaction weight of material varies with temperature to the influence that material is pyrolyzed
Journey.It is reported according to existing research, when using microwave-heating organic waste to its pyrolysis characteristics and Kinetic analysis, institute
The activation energy of acquisition is less than activation energy when traditional electrical heating, this is also indicated that can be with using microwave-heating organic waste
Reduce activation energy.When being pyrolyzed progress thermogravimetric analysis to material, select traditional thermogravimetric analyzer precision height that can meet the requirements, but
Be the material used amount it is few and be not to be carried out under conditions of microwave-heating, so at present in the condition of microwave-heating
Under to organic waste for example biomass carry out thermogravimetric analysis device be not very much.Due to the particularity of microwave, in material heat
The accuracy of its temperature and weight has strict requirements to the selection of sensor in solution preocess, and microwave to be avoided to acquire data
The influence of generation reduces the confidence level that error improves result.Therefore new microwave-heating device is developed, improves the production of target product
Rate reduces influence of the various factors to experimental result in experiment, for research thermal decomposition of organic wastes characteristic and kinetics
It is extremely important.
Currently, being chemically reacted for pyrolysis, the experimental provision function designed by some patents of invention is compared with unification, to reality
Parameter detecting control during testing is not exactly accurate, may be had an impact to experimental result.And major part utilizes microwave
The organic waste microwave-heating reaction that technology carries out all carries out on improved household microwave oven, the pyrolysis of these microwave thermals
Device is primarily present the problem of the following aspects：1. temperature measure and control is inaccurate；2. the excessively middle nothing of thermal decomposition of organic wastes
Method directly measures the real-time change value of reaction mass weight, thermal decomposition behavior point can not be carried out to it in conjunction with measured temperature variation
Analysis and and Kinetic analysis, to influence in-depth analysis to microwave-heating reaction mechanism.In addition, influencing organic waste
, such as material variety, catalyst, the reaction temperature many because being known as of pyrolysis.Emphasis is started in terms of changing above-mentioned two thus,
Design improves the precise requirements for the measurement that microwave-heating device meets in the reaction of microwave-heating organic waste to temperature, improves
Temperature controlled precision, while the weight change of monitoring reaction mass in real time are used in analysis material microwave-heating characteristic and anti-
Answer dynamic (dynamical) device, realize low cost, it is small, have a wide range of application.
Invention content
In order to overcome the problems, such as that some present in existing microwave-heating reaction unit, the present invention provide a kind of microwave thermogravimetric
Response analysis system, preferably realize Temperature Measure Control accuracy and response function it is convenient, simple, fast.System
Reach on the whole using simple, expansion is strong, data are accurate.
The technical solution adopted in the present invention is：
The analysis system includes that thermocouple temperature sensor, gravity sensor, control circuit, display module, chemistry are anti-
Answer system material pyrolysis section, appendage, magnetron and computer；Control circuit includes that A/D is converted, signal amplification circuit,
Microcontroller, D/A conversions；Display module includes touch display screen；Chemical reaction system material pyrolysis section includes that quartz flask is anti-
Answer device, oval quartz ampoule, cylindrical quartz short tube, cylindrical quartz long tube；Appendage includes microwave heating chamber, circle support
Disk, holder；In the upper wall middle holes Kai Liangge of microwave heating chamber, oval trepanning stretches into microwave heating intracavitary for placing
Oval quartz ampoule, thermocouple temperature sensor, thermocouple temperature sensor and quartz flask are inserted into oval quartz ampoule
Pyrolysis material contact in reactor, measures the temperature change value in reaction process, temperature sensor signal is converted by A/D and is passed
It send to microcontroller；Round hole, which stretches into, places cylindrical quartz short tube, and cylindrical quartz short tube is connected to quartz flask reactor,
For being passed through nitrogen；Microwave heating chamber left wall is provided with circular hole, and cylindrical quartz long tube one end is connect with quartz flask reactor, separately
Circular hole is stretched out in one end, is connect with external condensing unit, collects product liquid and pyrolysis gas that reaction mass pyrolysis generates；Quartz
Flask reactor is located on round tray, and be connected with round tray be insulated heat holder under four gravity sensitives
Device, while the changing value of reaction mass weight is monitored, the collected weight transducing signal of gravity sensor amplifies electricity by signal
Microcontroller is sent into road, A/D conversions；Microcontroller is converted by D/A and is connect with magnetron；Microcontroller also respectively with computer and display
Module connects.
Power, temperature, time, the technological parameters such as weight are shown in touch display screen.
Microwave power is controlled using Bang-Bang control algolithms when the error amount of temperature is more than set error amount,
Using maximum power the response speed of system is improved close to the temperature value of setting within the shortest time；When error amount is less than institute
It when the value of setting, uses small-power instead and adjusts temperature, using predictive PID, thermostatic control requirement is realized, substantially without super
It adjusts, and constant temperature is stablized, temperature fluctuation is small；Then the delays time to control pulse signal hardware timer of microcontroller generated acts on
In bidirectional triode thyristor, to accurately control its turn-on time and pwm pulse width, temperature is supervised in real time by being aided with peripheral circuit
It surveys and feeds back to controller to realize the primary voltage virtual value of intelligent control anode of magnetron to change microwave output power,
And then it controls the temperature change in microwave heating chamber and realizes that temperature is measured and automatically controlled.
The changing value of weight of material with result is output to computer after the processing of microcontroller together with temperature change value
Display interface, temperature time history plot during real-time observing response material reaction, weight varies with temperature
Curve graph, and can be shown on host computer after the completion of reaction using software programming according to the experimental data for acquiring and preserving
The TG curve graphs and DTG curve graphs for showing microwave-heating reactive material, seek the matched curve schematic diagram of reaction Kinetics Model
With dependent dynamics parameter.Being organized in using software according to the experimental data for acquiring and preserving after reaction can be on host computer
Show the TG curve graphs and DTG curve graphs of microwave-heating reactive material,
Optionally, TG and DTG are found out according to following formula：
TG=100*m/mT=150 DEG C
Wherein TG indicates that the coefficient values that reactive material quality varies with temperature under temperature programmed control, m indicate reactive material
Mass fraction percentage, mT=150 DEG CIndicate the mass fraction percentage of the reactive material when reaction temperature is 150 DEG C.
DTG=(TGk-TGk+1)/(Tk+1-Tk) (k is positive integer)
The quality that DTG indicates changes with time the functional relation numerical value of rate and temperature (or time), TGkFor the TG at k moment
Value, TGk+1For the TG values at k+1 moment, TkFor the time at k moment, Tk+1For the time at k+1 moment.
Optionally, the kinetics for the reactant being calculated using Arrhenius rate law as reaction Kinetics Model is joined
Number, according to treated, data obtain the conversion ratio η of the reactive material, choose reality when conversion ratio η ranges are respectively 0.1-0.8
The K value of border reaction temperature is reciprocal, is calculated as n=1, n=2 and n=3 according to Arrhenius rate law formula
Numerical value, obtain cutting edge aligned schematic diagram.Its linear fit formula is obtained according to linear schematic diagram.
The conversion ratio η of substance is found out according to following formula：
η=(100-TG)/(100-TGk) (k is positive integer)
TGkTo react the TG values of last moment.
Wherein linear fit formula is as follows：
Y=-ax+b (a is positive number)
Reaction activity E and pre-exponential factor A are found out according to Arrhenius rate law by slope-a.
The a large amount of smog and microwave that material will produce in microwave pyrolytic process are unevenly distributed in heating chamber can be to temperature
Have an impact, thus temperature measure selection is Multi probe thermocouple temperature sensor, according to requirement of experiment design customization
There are four temp probes for temperature sensor tool, wherein three temp probes are distributed at positive triangle, another temp probe designs position
In equilateral triangle center, four temp probes detect the temperature of difference in quartz flask reactor in microwave heating chamber simultaneously
Angle value keeps the temperature value detected more accurate.
Its shape is designed to cuboid by the quartz flask reactor of material pyrolysis, and a length of 20cm, wide 15cm are high
15cm is made of the quartz material of high temperature resistant degree.
The upper surface of quartz flask reactor is the oval frosted interface for being inserted into thermocouple temperature sensor, and maximum gauge is
10cm is higher by cuboid quartz flask reactor upper surface 2.5cm and is connected with the oval quartz ampoule of long 20cm；Side simultaneously
It is connected with the cylindrical quartz short tube of long 20cm there are one high 2.5cm frosteds interface at 2cm, it is that reaction is built conveniently to be passed through nitrogen
The environment of anaerobic.Side is connected there are one the outlet frosted interface of 2.5cm with the cylindrical quartz long tube of another segment length 30cm
It connects, and outlet interface tilts down 5-10 °, quartz flask reactor is flowed back into after preventing product liquid from condensing.
For the upper surface of microwave heating chamber there are two hole, thermocouple temperature sensor insert port maximum gauge is 10.8cm, nitrogen
It is passed through a diameter of 3cm of mouth.One a diameter of 3cm of venthole in left side.
The round tray for placing quartz flask reactor is the cylinder of quartz glass material, and a diameter of 28cm, thickness is
0.8cm。
There are one the groove of trapezoidal shape, a length of 21cm in upper surface of the groove of trapezoidal shape, wide 16cm, bottoms at round tray center
The a length of 20.4cn in face, wide 15.4cm, it is 45 °, depth 0.3cm that surrounding inclined-plane, which tilts, facilitates the fixed quartz flask reactor of placement.
The cylindrical quartz long tube other end outside microwave heating chamber can also be connected with catalyst reaction device to be realized to reacting
Product reformate upgrading, or with other detection and analysis instruments (such as FTIR, GC/MS) be connected, realize in real time to thermal decomposition product at
The analysis divided.
The present invention has the following advantages that compared with prior art：
1. accurately measuring the changing value of temperature in reaction process, subtracted by using intelligent control algorithm control temperature-rise period
Small temperature existing error during measuring and controlling.
2. real-time monitoring temperature variation and reaction mass weight change are to analysis organic waste microwave-heating characteristic and instead
Dynamics is answered to provide a convenient.
3. entire microwave-heating system can realize different functional requirements, simple in structure, easy to use, cheap.
The specific implementation mode of the present invention is described in further detail below in conjunction with the accompanying drawings
Description of the drawings
Fig. 1 is microwave-heating apparatus structure schematic diagram
Fig. 2 systematic schematic diagrams in order to control
Fig. 3 is structure of reactor schematic diagram
1 microwave heating chamber, 2 round tray, 3 quartz flask reactor, 4 thermocouple temperature sensor, 5 gravity sensitive in figure
9 cylindrical quartz short tube of the oval quartz ampoule of 6 touch display screen of device, 7 holder 8,10 cylindrical quartz long tube
Specific implementation mode
A kind of microwave thermogravimetric response analysis system, structural schematic diagram are shown in Fig. 1, reactor schematic diagram such as Fig. 3：Response analysis
System is in the upper wall middle holes Kai Liangge of microwave-heating device heating chamber 1, and oval trepanning is for stretching into placement microwave
The quartz ampoule 8 of ellipse in heating chamber 1, oval quartz ampoule 8 is interior to be inserted into thermocouple temperature sensor 4；Round hole is stretched
Enter to place cylindrical quartz short tube 9, the frosted external tapping of oval quartz ampoule 8 and cylindrical quartz short tube 9 respectively with placement
Two interfaces of 3 upper end of quartz flask reactor on round tray 2 are connected.The opening of 1 left side wall of microwave heating chamber
It stretches into cylindrical quartz long tube 10 with quartz flask reactor 3 to be connected, to ensure quartz ampoule 8, the cylindrical quartz of ellipse
Short tube 9, cylindrical quartz long tube 10 are not contacted with microwave heating cavity wall.Circle is placed it in when placing quartz flask reactor 3
In 2 groove of shape pallet, the gap between 2 groove of quartz flask reactor 3 and round tray can add one layer of silica wool and fix
Good quartz flask reactor 3.9 upper end of cylindrical quartz short tube is connected with nitrogen rubber tube is passed through, the purpose for being passed through nitrogen be for
Oxygen-free environment is built in microwave-heating reaction.
Temperature controlled processes and weight data gatherer process are shown in Fig. 2, are inserted into the upper wall oval port of microwave-heating device
Oval quartz ampoule 8, lower end are connected with quartz flask reactor 3, upper end be inserted into designed thermocouple temperature sensor 4 with
Pyrolysis material in microwave-heating quartz flask reactor 3 contacts, and the temperature change value in accurately measure reaction process will
Microcontroller is sent to after collected signal processing, microcontroller is judged according to collected data, the practical temperature detected
When angle value and the temperature value error of setting are more than 20 DEG C of given error amount microwave work(is controlled using Bang-Bang control algolithms
Rate improves the response speed of system.When error amount is less than set 20 DEG C, uses small-power instead and adjust temperature, use at this time
Predictive PID realizes thermostatic control requirement.The delays time to control pulse signal effect that the hardware timer of microcontroller generates
In bidirectional triode thyristor, its turn-on time and pwm pulse width are accurately controlled, periphery is aided with display module；Temperature is monitored in real time
And controller is fed back to realize the primary voltage virtual value of intelligent control anode of magnetron, to which the anode for controlling magnetron is high
It presses to change microwave output power, and then controls the temperature change in microwave heating chamber and realize that temperature is measured and automatically controlled.Circle
Four gravity sensors 5 of 2 times installations that are connected with holder 7 of shape pallet monitor the changing value of reaction mass weight simultaneously, and gravity passes
5 collected value of sensor be sent into core processor microcontroller, with together with temperature change value after microcontroller is handled result is defeated
Go out the display interface to computer, observes temperature time history plot during material reaction in real time, weight is with temperature
The curve graph of variation is spent, and after the completion of reaction can be upper using software programming according to the experimental data for acquiring and preserving
The TG curve graphs and DTG curve graphs that microwave-heating reactive material is shown on machine, seek the matched curve of reaction Kinetics Model
Schematic diagram and dependent dynamics parameter.
The operation principle of the present invention：The reaction mass of load weighted certain mass is packed into quartz flask reactor when experiment
It in 3, is put on the round tray 2 of microwave heating chamber 1, the gap between 2 groove of 3 bottom of quartz flask reactor and round tray
The purpose of adding some silica wools is fixed quartz flask reactor 3, prevents mobile pair during the reaction of quartz flask reactor 3
Experiment has an impact, and thermocouple temperature sensor 4 is put into oval quartz ampoule 8 and is connected with quartz flask reactor 3, then
One end of cylindrical quartz short tube 9 is connected with the rubber tube for being passed through nitrogen, the other end is connected to quartz flask reactor 3, then
One end of cylindrical quartz long tube 10 is connected with quartz flask reactor 3, the other end may be coupled to condensing unit, and separation is simultaneously
Product liquid and pyrolysis gas that reaction mass pyrolysis generates are collected, while being connected with computer, finally checks entire reaction system
System avoids accidentalia from causing error to experiment, opens nitrogen bottle valve, nitrogen 15min is passed through into reaction system, for reaction
Build oxygen-free environment.The switch of microwave-heating reaction unit is opened, 500 DEG C of pyrolysis reaction temperature, microwave power 750W are set, instead
20min between seasonable, " operation starts " reaction unit on point touching screen bring into operation, and with the beginning of reaction, touch display
Real-time display goes out the numerical value such as actual temperature, actual power, weight on screen, while it is anti-on the interface of computer to be shown in material
Temperature time history plot during answering, the curve graph that weight varies with temperature, when actual temperature rises to 480 DEG C
When, microwave power quickly becomes 100W from 750W, and small-power adjusts the temperature change in microwave heating chamber 1, until temperature reaches
When set temperature value, " end of run " is clicked after reaction, result and the preservation of data processing are shown on computer interface
It should be as a result, finally closing the device.
Claims (10)
1. a kind of microwave thermogravimetric response analysis system, it is characterised in that：The analysis system includes thermocouple temperature sensor, again
Force snesor, control circuit, display module, chemical reaction system material pyrolysis section, appendage, magnetron and computer；
Control circuit includes A/D conversions, signal amplification circuit, microcontroller, D/A conversions；Display module includes touch display screen；It is chemical anti-
It includes quartz flask reactor to answer system material pyrolysis section, oval quartz ampoule, cylindrical quartz short tube, and cylindrical quartz is long
Pipe；Appendage includes microwave heating chamber, round tray, holder；It is oval in the upper wall middle holes Kai Liangge of microwave heating chamber
The trepanning of shape is inserted into electric thermo-couple temperature for placing the oval quartz ampoule for stretching into microwave heating intracavitary, in oval quartz ampoule and is passed
Sensor, thermocouple temperature sensor are contacted with the pyrolysis material in quartz flask reactor, and the temperature measured in reaction process becomes
Temperature sensor signal is sent to microcontroller by change value by A/D conversions；Round hole, which stretches into, places cylindrical quartz short tube, circle
Cylindricality quartz short tube is connected to quartz flask reactor, for being passed through nitrogen；Microwave heating chamber left wall is provided with circular hole, cylindrical stone
English long tube one end is connect with quartz flask reactor, and the other end stretches out circular hole, is connect with external condensing unit, and reactant is collected
The product liquid and pyrolysis gas that material pyrolysis generates；Quartz flask reactor is located on round tray, and is connected with round tray
Be insulated heat holder under four gravity sensors, while monitoring the changing value of reaction mass weight, gravity sensor
Collected weight transducing signal is sent into microcontroller by signal amplification circuit, A/D conversions；Microcontroller is converted by D/A and magnetic
Keyholed back plate connects；Microcontroller is also connect with computer and display module respectively.
2. a kind of microwave thermogravimetric response analysis system as described in claim 1, it is characterised in that：It is shown in touch display screen
Power, temperature, time, weight technological parameter.
3. a kind of microwave thermogravimetric response analysis system as described in claim 1, it is characterised in that：When the error amount of temperature is more than
Microwave power is controlled using Bang-Bang control algolithms when set error amount, using maximum power within the shortest time
Close to the temperature value of setting, the response speed of system is improved；When error amount is less than set value, uses small-power instead and adjust temperature
Degree realizes thermostatic control requirement, basic non-overshoot, and constant temperature is stablized, temperature fluctuation is small using predictive PID；So
The delays time to control pulse signal that the hardware timer of microcontroller generates is acted on into bidirectional triode thyristor afterwards, is led to accurately control it
Logical time and pwm pulse width are monitored temperature by being aided with peripheral circuit and feed back to controller in real time to realize intelligent control
The primary voltage virtual value of anode of magnetron processed controls the temperature in microwave heating chamber and becomes to change microwave output power
Change and realizes that temperature is measured and automatically controlled.
4. a kind of microwave thermogravimetric response analysis system as described in claim 1, it is characterised in that：The changing value of weight of material with
Result is output to the display interface of computer, real-time observing response object by temperature change value after the processing of microcontroller together
Expect temperature time history plot in reaction process, the curve graph that weight varies with temperature, and according to acquiring and preserve
Experimental data can show that the TG of microwave-heating reactive material is bent on host computer after the completion of reaction using software programming
Line chart and DTG curve graphs seek the matched curve schematic diagram and dependent dynamics parameter of reaction Kinetics Model；Simultaneously according to acquisition
The experimental data of preservation is organized in the TG that can show microwave-heating reactive material on host computer after reaction using software
Curve graph and DTG curve graphs.
5. a kind of microwave thermogravimetric response analysis system as described in claim 1, it is characterised in that：Material is in microwave pyrolytic process
The a large amount of smog and microwave that will produce are unevenly distributed in heating chamber to have an impact temperature, so the measurement selection of temperature
Be Multi probe thermocouple temperature sensor, according to the temperature sensor of requirement of experiment design customization tool there are four temp probe,
Wherein three temp probes are distributed at positive triangle, and the design of another temp probe is located at equilateral triangle center, four temperature
Probe while the temperature value for detecting difference in quartz flask reactor in microwave heating chamber, keep the temperature value detected more accurate
Really.
6. a kind of microwave thermogravimetric response analysis system as described in claim 1, it is characterised in that：The quartz flask of material pyrolysis
Its shape is designed to that cuboid, a length of 20cm, wide 15cm, high 15cm are made of the quartz material of high temperature resistant degree by reactor.
7. a kind of microwave thermogravimetric response analysis system as described in claim 1, it is characterised in that：Quartz flask reactor it is upper
Face is the oval frosted interface for being inserted into thermocouple temperature sensor, and it is anti-to be higher by cuboid quartz flask by maximum gauge 10cm
Device upper surface 2.5cm is answered to be connected with the oval quartz ampoule of long 20cm；It is connect simultaneously there are one high 2.5cm frosteds at the 2cm of side
Mouth is connected with the cylindrical quartz short tube of long 20cm, and it is the environment that anaerobic is built in reaction to be conveniently passed through nitrogen；There are one sides
The outlet frosted interface of 2.5cm, is connected, and outlet interface tilts down 5- with the cylindrical quartz long tube of another segment length 30cm
10 °, quartz flask reactor is flowed back into after preventing product liquid from condensing.
8. a kind of microwave thermogravimetric response analysis system as described in claim 1, it is characterised in that：The upper surface of microwave heating chamber has
Two holes, thermocouple temperature sensor insert port maximum gauge are 10.8cm, and nitrogen is passed through a diameter of 3cm of mouth, one of left side
The a diameter of 3cm of venthole.
9. a kind of microwave thermogravimetric response analysis system as described in claim 1, it is characterised in that：Place quartz flask reactor
Round tray be quartz glass material cylinder, a diameter of 28cm, thickness 0.8cm；There are one ladders at round tray center
The groove of shape, a length of 21cm in upper surface of the groove of trapezoidal shape, wide 16cm, a length of 20.4cn in bottom surface, wide 15.4cm, surrounding are oblique
It is 45 °, depth 0.3cm that face, which tilts, facilitates the fixed quartz flask reactor of placement.
10. a kind of microwave thermogravimetric response analysis system as described in claim 1, it is characterised in that：Circle outside microwave heating chamber
The shape quartz long tube other end can also be connected realization to reaction product reformation upgrading with catalyst reaction device, or detect and divide with other
Analyzer device is connected, and realizes the analysis to thermal decomposition product ingredient in real time.
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| CN201810431482.4A CN108489853A (en) | 2018-05-08 | 2018-05-08 | A kind of microwave thermogravimetric response analysis system |
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| CN201810431482.4A CN108489853A (en) | 2018-05-08 | 2018-05-08 | A kind of microwave thermogravimetric response analysis system |
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| CN108489853A true CN108489853A (en) | 2018-09-04 |
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Cited By (3)
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| CN110865000A (en) * | 2019-12-02 | 2020-03-06 | 西安特种设备检验检测院 | System and method for continuously measuring high-temperature corrosion rate of heat-resistant steel |
| CN113083190A (en) * | 2021-03-31 | 2021-07-09 | 西安石油大学 | Microwave thermogravimetric reaction and pyrolysis product staged collection and analysis system and method |
| CN114534770A (en) * | 2022-01-06 | 2022-05-27 | 深圳大学 | Preparation of catalyst with wave-absorbing-catalyzing function and application of microwave pyrolysis of sludge |
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Cited By (4)
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| CN110865000A (en) * | 2019-12-02 | 2020-03-06 | 西安特种设备检验检测院 | System and method for continuously measuring high-temperature corrosion rate of heat-resistant steel |
| CN113083190A (en) * | 2021-03-31 | 2021-07-09 | 西安石油大学 | Microwave thermogravimetric reaction and pyrolysis product staged collection and analysis system and method |
| CN114534770A (en) * | 2022-01-06 | 2022-05-27 | 深圳大学 | Preparation of catalyst with wave-absorbing-catalyzing function and application of microwave pyrolysis of sludge |
| CN114534770B (en) * | 2022-01-06 | 2024-01-30 | 深圳大学 | Catalyst with wave-absorbing-catalytic function and preparation and sludge microwave pyrolysis application thereof |
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