CN106769606A - One kind is rapidly heated thermogravimetric analyzer - Google Patents
One kind is rapidly heated thermogravimetric analyzer Download PDFInfo
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- CN106769606A CN106769606A CN201710077975.8A CN201710077975A CN106769606A CN 106769606 A CN106769606 A CN 106769606A CN 201710077975 A CN201710077975 A CN 201710077975A CN 106769606 A CN106769606 A CN 106769606A
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 43
- 229910052802 copper Inorganic materials 0.000 claims abstract description 43
- 239000010949 copper Substances 0.000 claims abstract description 43
- NJPPVKZQTLUDBO-UHFFFAOYSA-N novaluron Chemical compound C1=C(Cl)C(OC(F)(F)C(OC(F)(F)F)F)=CC=C1NC(=O)NC(=O)C1=C(F)C=CC=C1F NJPPVKZQTLUDBO-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims description 21
- 230000008859 change Effects 0.000 claims description 7
- 239000002184 metal Substances 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 238000012937 correction Methods 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- 238000004458 analytical method Methods 0.000 claims description 3
- 239000002245 particle Substances 0.000 abstract description 10
- 238000012546 transfer Methods 0.000 abstract description 6
- 230000005855 radiation Effects 0.000 abstract description 3
- 239000000523 sample Substances 0.000 description 17
- 238000006243 chemical reaction Methods 0.000 description 16
- 239000007789 gas Substances 0.000 description 11
- 239000003245 coal Substances 0.000 description 7
- 230000004044 response Effects 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 230000008569 process Effects 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 238000009529 body temperature measurement Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 3
- 238000003556 assay Methods 0.000 description 3
- 230000033228 biological regulation Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000009123 feedback regulation Effects 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 239000013068 control sample Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000007405 data analysis Methods 0.000 description 1
- 238000013480 data collection Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007323 disproportionation reaction Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 125000006850 spacer group Chemical group 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000002411 thermogravimetry Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- 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
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Materials Using Thermal Means (AREA)
Abstract
The invention belongs to measuring instrument field, and disclose one kind and be rapidly heated thermogravimetric analyzer, including pedestal, electronic analytical balance, open support pipe, heater, temperature control system, cloche and equipment data acquisition analyzing, pedestal includes balance room, rebasing adjustment stud and support rim, and electronic analytical balance is arranged in the balance room；Heater includes inverted U copper pipe, wire netting reactor and electrode；Temperature control system includes thermocouple, holding wire and temperature controller；Cloche is accepted by the support rim and covers the open support pipe, wire netting reactor and inverted U copper pipe；The equipment data acquisition analyzing is connected with the electronic analytical balance and the temperature controller respectively.The present invention, as heater, wire netting reactor and particle directly contact, is heated as major way with heat transfer and heat radiation using wire netting reactor to sample particle, and the rate of heat addition can be greatly improved.
Description
Technical field
The invention belongs to measuring instrument field, more particularly, to a kind of thermogravimetric analyzer.
Background technology
Thermogravimetric analyzer is a kind of instrument that material mass-temperature change relation is detected using DTG.Work as measured matter
When having evaporation, pyrolysis, gasification, oxidation etc. to react in heating process, tested material mass will change.DTG
Important feature is quantitative strong, can exactly determine the mass change of material and the speed of change.However, DTG analytical technology
Still suffer from certain limitation.
First, the thermogravimetric analyzer of current use for laboratory, the rate of heat addition only up to reach 100K/min, with actual industrial
During the heating rate of material have larger difference, it is impossible to the need for meeting some researchs.For example, for the boiler of powder coal stove
In, after fuel sprays into boiler furnace, heating rate reaches 1000-10000K/s, and this is far apart with the heating rate of thermogravimetric.Its
Secondary, in thermogravimetric actual moving process, heating rate occurs deviation, and because furnace volume is larger, as temperature is higher, body of heater dissipates
Heat loss is bigger, causes heating rate to reduce, and this is accomplished by carrying out sample temperature feedback regulation correcting sample temperature carrying out instead
Feedback regulation correction, however, thermogravimetric analyzer is all that sample is heated up by radiation of burner hearth and convection heat transfer' heat-transfer by convection at present, by adjusting
The temperature control sample temperature of the big burner hearth of whole body, its regulation process is very slow, it is impossible to ensure the accuracy of heating rate, right
Experimental result has greatly interference.
Again, when thermogravimetric GC-MS is needed to use, by coupling during gas analyzer synchro measure gaseous product, due to
Current thermogravimetric analyzer is used mostly crucible as reactor, and the pile up effect of sample is serious (to cause temperature distributing disproportionation, part
Temperature is too high), it is also one of the reason for causing secondary response that gas residence time is long.For some chemical reactions, reaction generation
Gaseous products between or gaseous products and sample between be susceptible to secondary response so that gaseous products concentration changes,
Cause measurement error.
In sum, the thermogravimetric analyzer of current use for laboratory there is problems：
1) rate of heat addition of current thermogravimetric analyzer only up to reach 100K/min, it is impossible to simulate some actual works
Industry process, is unfavorable for further investigated chemical reaction mechanism, there is significant limitation.
2) sample is heated up by Radiative heat transfer in furnace, furnace volume is big, and temperature signal feedback regulation process is slow,
Heating rate cannot be accurately controlled.
3) for some courses of reaction, secondary response significantly, and is difficult control and avoids, when needing that gaseous product is entered
During row Synchronization Analysis, secondary response will cause greatly interference to the accuracy of measurement result.
The content of the invention
For the disadvantages described above or Improvement requirement of prior art, it is rapidly heated thermogravimetric analyzer the invention provides one kind,
Exist in existing thermogravimetric technology that the rate of heat addition is slow, temperature adjustment is slow and secondary response is serious etc. and ask its object is to overcome
Topic, it is fast with heating rate, the advantages of temperature control is precisely and secondary response influence is small.
To achieve the above object, it is proposed, according to the invention, be rapidly heated thermogravimetric analyzer there is provided one kind, it is characterised in that bag
Include pedestal, electronic analytical balance, open support pipe, heater, temperature control system, cloche and data collection and analysis dress
Put, wherein,
The pedestal includes balance room, rebasing adjustment stud and support rim, and the balance room is hollow, the rebasing adjustment
Stud is arranged on the inner bottom surface of balance room, and the support rim is located at balance room top and is held by the platform room
Connect, additionally, being provided with cable tray on the support rim；
The electronic analytical balance is arranged in the balance room and is accepted by the rebasing adjustment stud；
The open support pipe is vertically arranged, and it passes through the electronics after passing through the support rim and the balance room
Assay balance is accepted, and the side wall of the open support pipe has multiple through holes；
The heater includes inverted U copper pipe, wire netting reactor and electrode, two ends of the inverted U copper pipe
It is shelved on the support rim and its inner chamber connects with the cable tray of the support rim, the wire netting reactor leads to
Cross the open support pipe to accept, the electrode is arranged on the inverted U copper pipe and by connecting wire and the gold
The reactor connection of category net, additionally, the electrode also connects the temperature control system by current supply line, for the gold
Category net reactor is powered heating, the current supply line from the cable tray of the support rim through the support rim, and from
Opening on the inner chamber and side wall of the inverted U copper pipe is through the copper pipe of falling inverted U；
The temperature control system includes thermocouple, holding wire and temperature controller, and the thermocouple is fixedly mounted on institute
The top of inverted U copper pipe is stated, it passes through the holding wire and is connected with the temperature controller, and it is described from branch described in holding wire
The cable tray for supportting boss passes through the support rim, and opening from the inner chamber and side wall of the inverted U copper pipe is through institute
The copper pipe of falling inverted U is stated, the temperature controller connects the electrode by the current supply line；
The cloche is accepted by the support rim and covers the open support pipe, wire netting reactor and fall
U-shaped copper pipe, the side wall of the cloche is provided with air inlet and its top is provided with exhaust outlet；
The equipment data acquisition analyzing is connected with the electronic analytical balance and the temperature controller respectively.
Preferably, the wire netting reactor is formed for 2~4 layers of metal net folding.By screw and the open support
Pipe top screw is connected.
Preferably, it is provided with splitting between the wire netting reactor and the open support pipe.
Preferably, the temperature signal that the temperature controller is measured according to the thermocouple, the temperature value with setting is carried out
Compare, form feedback signal, so that the electric current on wire netting reactor is controlled, it is to change heating power and then anti-to wire netting
The temperature of device is answered to be adjusted correction.
Preferably, the quantity of the thermocouple is two, wherein a thermometric end for thermocouple is located at wire netting reactor
Overcentre, another thermometric end of thermocouple is located at wire netting reactor edge top.
Preferably, the cloche is provided with sealing ring with the joint of the support rim.
In general, by the contemplated above technical scheme of the present invention compared with prior art, can obtain down and show
Beneficial effect：
1) using wire netting reactor as heater, wire netting reactor and particle directly contact, with heat transfer and
Heat radiation is heated for major way to sample particle, the rate of heat addition can be greatly improved, it is possible to achieve the rate of heat addition is 10-1-103Great-leap-forward regulation between five orders of magnitude of K/s.
2) heating power is controlled by changing the electric current of wire netting, and then adjusts heating rate, shorten regulation
Time, improve the accuracy of temperature control.
3) sample is in individual layer its flat presentation in wire netting reactor, reduces solid particle and directly contacts with each other, together
When, reaction gas flow by conversion zone and takes away gaseous product at a high speed, secondary between significantly reducing admittedly or between gas-solid
Reaction (gas residence time is long, also there is secondary response between gas).
4) sample is in individual layer its flat presentation in wire netting reactor, reduces pile up effect so that sample each several part temperature
Degree is consistent.
5) conversion zone is disposed with two pairs of thermocouples, and is all almost close to reactor surface, and experimental temperature is measured more
Accurately.
Figure explanation
Fig. 1 is structural representation structure chart of the invention；
Fig. 2 (a), Fig. 2 (b) are respectively the sectional view and top view of support rim in the present invention；
Fig. 3 is the structural representation of open support pipe in the present invention；
Fig. 4 is the structural representation of inverted U copper pipe in the present invention；
Fig. 5 is sample on wire netting reactor in the present invention and thermocouple arrangement schematic diagram；
Fig. 6 is cloche structural representation in the present invention.
Specific embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, below in conjunction with figure and embodiment, to this
Invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, not
For limiting the present invention.As long as additionally, technical characteristic involved in invention described below each implementation method that
Conflict is not constituted between this can be just mutually combined.
With reference to each accompanying drawing, one kind is rapidly heated thermogravimetric analyzer, including pedestal 1, electronic analytical balance 2, open support circle
Pipe 3, heater 4, temperature control system 5, cloche 6 and equipment data acquisition analyzing, wherein,
The pedestal 1 includes balance room 1-2, rebasing adjustment stud 1-1 and support rim 1-3, in the balance room 1-2
Sky, the rebasing adjustment stud 1-1 is arranged on the inner bottom surface of balance room 1-2, and the support rim 1-3 is located at the balance room
1-2 tops are simultaneously accepted by the platform room, additionally, being provided with cable tray on the support rim 1-3；
The electronic analytical balance 2 is arranged in the balance room 1-2 and is accepted by the rebasing adjustment stud 1-1；
The open support pipe 3 is vertically arranged, and it passes through after passing through the support rim 1-3 and the balance room 1-2
The electronic analytical balance 2 is accepted, and the side wall of the open support pipe 3 has multiple through holes；
The heater 4 includes inverted U copper pipe 4-1, wire netting reactor 4-4 and electrode, the inverted U copper pipe 4-1
Two ends rests are on the support rim 1-3 and its inner chamber connects with the cable tray of the support rim 1-3, institute
Wire netting reactor 4-4 is stated to be accepted by the open support pipe 3, the electrode be arranged on the inverted U copper pipe on and
It is connected with the wire netting reactor 4-4 by connecting wire, additionally, the electrode also connects described by current supply line 4-2
Temperature control system 5, for heating of being powered to the wire netting reactor 4-4, the current supply line 4-2 is convex from the support
The cable tray of platform 1-3 passes through the support rim 1-3, and opening from the inner chamber and side wall of the inverted U copper pipe 4-1 to wear
Cross the copper pipe of falling inverted U；
The temperature control system 5 includes thermocouple, holding wire 5-4 and temperature controller 5-3, and the thermocouple fixes peace
Mounted in the top of the inverted U copper pipe 4-1, it passes through the holding wire 5-4 and is connected with the temperature controller 5-3, and institute
State from the cable tray of support rim 1-3 described in holding wire 5-4 through the support rim 1-3, and from the inverted U copper pipe 4-
Through the copper pipe of falling inverted U, the temperature controller 5-3 passes through the current supply line 4-2 for opening on 1 inner chamber and side wall
Connect the electrode；
The cloche 6 is accepted by the support rim 1-3 and covers open support pipe 3, the wire netting reaction
Device 4-4 and inverted U copper pipe 4-1, the side wall of the cloche 6 is provided with air inlet and its top is provided with exhaust outlet 6-3；
The equipment data acquisition analyzing 7 is connected with the electronic analytical balance 2 and the temperature controller 5-3 respectively.
Further, the wire netting reactor 4-4 is formed for 2~4 layers of metal net folding.By screw and the porous branch
The top screw of pipe 3 is held round to be connected.
Further, it is provided with splitting between the wire netting reactor 4-4 and the open support pipe 3.
Further, the temperature signal that the temperature controller 5-3 is measured according to the thermocouple, the temperature value with setting enters
Row compares, and forms feedback signal, so that the electric current on wire netting reactor 4-4 is controlled, to change heating power, and then to metal
The temperature of net reactor 4-4 is adjusted correction.
Further, the quantity of the thermocouple is two, wherein a thermometric end for thermocouple is located at wire netting reactor
4-4 overcentres, another thermometric end of thermocouple is located at wire netting reactor 4-4 edges top.
Further, the cloche 6 is provided with sealing ring 6-1 with the joint of the support rim 1-3.
Reference picture 1, the pedestal includes 4 rebasing adjustment stud 1-1, balance room 1-2 and support rim 1-3.
The rebasing adjustment stud 1-1 is highly 50mm, and surfacing can adjust height so that balance can be not
Level is kept on flat surface.
Referring to Figures 1 and 2, the balance room 1-2 is rectangular structure, and inside is cavity, and balance room top is opened for circle
Mouthful, balance room's lower end side is provided with protection gas import.
The support rim 1-3 includes higher level's boss and subordinate's boss, positioned above balance room 1-2.
Reference picture 2, there is circular support frame passage 1-3-2 in the middle of the support rim 1-3, connect balance room top circle
Shape opening.
Cable tray on the support rim 1-3 is in the first internal wiring passage 1-3-1A and second being arranged symmetrically
Portion line channel 1-3-1B, the one end open of the cable tray is located at the top end face of higher level's boss, and another end opening is located at down
The side of level boss.
Reference picture 1, the open support pipe 3 is cylinder cylinder, and the through hole of many rectangular arrangeds is provided with around it, with
Ensure that the purging air-flow being passed through from both sides the first air inlet 6-2A of cloche 6 and the second air inlet 6-2B in experimentation is uniform.
Circumferentially symmetric design has the first Screw hole structure 3-1 and the second screw at open support pipe top described in reference picture 3
Structure 3-2, for fixing wire netting reactor 4-3 with screw fit.The external diameter of the open support pipe 3 is slightly less than above-mentioned branch
The aperture of the circular support frame passage 1-3-2 in the middle of support boss 1-3.
Reference picture 1 and Fig. 4, the heater 4 include that inverted U copper pipe 4-1, wire 4-2 and electrode and wire netting react
Device 4-4, electrode includes that electrode anode 4-3A and electrode cathode 4-3B, the inverted U copper pipe 4-1 are hollow structure, inverted U copper pipe
First end 4-1A and the second end 4-1B respectively with the first internal wiring passage 1-3-1A and the second internal wiring passage 1-3-
1B is connected and the two ends are fixed on higher level's boss.
The current supply line is entered by the first internal wiring passage 1-3-1A and the second internal wiring passage 1-3-1B
Enter inside inverted U copper pipe 4-1, the first perforate 4-1C and the second perforate 4-1D from the middle part of inverted U copper pipe stretch out, many with being fixed on
The electrode connection of the first screw 3-1 and the second screw 3-2 on the top of hole support pipe 3.
The electrode anode 4-3A and electrode cathode 4-3B is connected to supply by connecting wire with wire netting reactor 4-4
Electricity.
Reference picture 1, the wire netting reactor 4-4 is formed for 2 to 4 layers of metal net folding, porous with described by screw
The top of support pipe 3 first screw 3-1 and the second screw 3-2 is connected.
Reference picture 5, wire netting reactor 4-4 marks at middle part the border circular areas of diameter 2-3cm as reaction zone, and reactant is put down
It is laid on this reaction zone.
Reference picture 1, the temperature control system 5 includes the first thermocouple 5-2A and the second thermocouple 5-2B, temperature control
Device 5-3 and holding wire 5-4.
Reference picture 1 and Fig. 4, the first thermocouple 5-2A and the second thermocouple 5-2B are fixed on the curved portions of inverted U copper pipe 4-1
Hole a 4-1E and 4-1F is opened in 5-1, inverted U copper pipe 4-1 top both sides respectively, and inverted U copper pipe 4-1 is hollow structure, logical with circuit
Road is connected, and is fixed on higher level's boss.
The first side opening 4-1E and the second side opening 4-1F, the first thermocouple 5- is opened respectively in thermocouple fix bar top both sides
Thus holes is stretched out for 2A and the second thermocouple 5-2B.
The holding wire passes through line channel, into inside inverted U copper pipe 4-1, from inverted U copper pipe 4-1 tops institute
Open and stretched out at the first side opening 4-1E and the second side opening 4-1F, be connected with the first thermocouple 5-2A and the second thermocouple 5-2B, it is described
The holding wire other end is connected with temperature controller 5-3.
Reference picture 5, the first thermocouple 5-2A and the second thermocouple 5-2B are arranged on the wire netting reactor 4-4
Side, a thermocouple temperature measurement end 5-2C is located at wire netting reactor 4-4 overcentres and measures reaction zone temperature, another thermocouple
Thermometric end 5-2D is located at wire netting reactor 4-4 edges top measurement reaction zone lip temperature.
Reference picture 1, the temperature controller 5-3 is connected with the heater by wire.The temperature controller 5-3
According to the temperature signal that the first thermocouple 5-2A and the second thermocouple 5-2B are measured, the temperature value with setting is compared,
Feedback signal is formed, the electric current of heater 4 is controlled, changes heating power, temperature is adjusted.
Reference picture 1 and Fig. 6, the latter half of the cloche 6 are cylinder, and top is hemispherical.The lower half of the cloche 6
Partial cylinder external diameter is consistent with higher level's boss external diameter of the support rim 1-3, is placed on higher level's boss, contact position arrangement
There is sealing ring 6-1.
Reference picture 6, the cloche side is provided with the first air inlet 6-2A and the second air inlet 6-2B, and top is provided with
One gas outlet 6-3, the gas outlet 6-3 lower ends are set to down infundibulate.
Reference picture 1, the data acquisition and analysis system 7 includes data line and computer 7-1；By the data transfer
Line, the electronic analytical balance 2, the temperature controller 5-3 is connected with the computer 7-1, by the electronic analytical balance 2
Weight signal and the temperature signal of the temperature controller 5-3 be transferred to computer 7-1.
Constant-temperature combustion experiment is carried out to coal particle sample using above-mentioned variable heating speed thermogravimetric analyzer, specific steps are such as
Under：
1) the thermogravimetric analysis instrument apparatus are placed on the experimental bench of surfacing level, adjustment stud in spacer bottom makes
Balance is in horizontality.
2) support bar 3 for taking out cleaning is inserted vertically into the circular support frame passage 1-3-21- of support rim 1-3 from top to bottom
In 3-2, the first screw 3-1 and the 2nd 3-2 of the anti-device 4-4 of fixed wire netting are backed out, choose clean metal mesh sheet (this reality
Test from 200 mesh gauzes, corresponding particle diameter is 100 μm -200 μm) fold after with first screw 3-1 of the top of open support pipe 3
Fixation is tightened with the 2nd 3-2.The thermocouple wire of this experiment preferably 50 μ m diameters.
3) current supply line 4-2 and holding wire 5-4 by the first internal wiring passage 1-3-1A and the second internal wiring passage
1-3-1B is stretched into, and then installs hollow inverted U copper pipe 4-1, by current supply line 4-2 and holding wire 5-4 along inverted U copper pipe 4-1
Stretch into, draw wire at the first middle part perforate 4-1C and the second middle part perforate 4-1D of inverted U copper pipe 4-1, by wire 4-2
It is connected with the electrode for being fixed on the top screw of support bar 3, holding wire 5-4 is drawn by the first side opening 4-1E and the second side opening 4-1F
Go out, then holding wire 5-4 is connected with thermocouple, thermocouple temperature measurement end is arranged in the wire netting reactor 4-4 tops, one
Thermocouple temperature measurement end 5-2C is located at wire netting reactor overcentre and measures reaction zone temperature, another thermocouple temperature measurement end 5-2D
Positioned at wire netting reactor 4-4 edges top measurement reaction zone lip temperature, then inverted U copper pipe 4-1 is fixed.
4) cloche 6 is covered, startup power supply opens electronic analytical balance 2, waits the stable reading of electronic analytical balance 2, clearly
The reading of zero electronic analytical balance 2.
5) reaction heating schedule is write, starts balance, carry out blank assay.
6) the coal sample particle between 100 μm -200 μm of particle diameters of the 30mg by screening is weighed with electronic analytical balance 2.
7) treat that blank assay is completed, after thermogravimetric device is cooled to normal temperature, remove cloche, unclamp the spiral shell of fixed wire netting
Mother, the wire netting reactor 4-4 of folding is spread out, and the coal sample particulate samples 8 for weighing up are laid in wire netting reactor 4-4 middle parts
The reaction zone of diameter 2-3cm.
8) wire netting reactor 4-4 is folded so that wire netting reactor 4-4 compression coal sample particles, tighten fixed wire netting
2 nuts of reactor 4-4.During 2 nuts of fixed wire netting reactor 4-4 are tightened, it should be noted that first twist slightly
Nut makes 2 nuts all press wire netting reactor 4-4, then slowly tightens one by one again, can't by each nut once by
It is individual to tighten.
9) repeat step 3) in arrangement electrode cable and thermocouple process, arrange electrode cable and thermocouple.
10) cloche is covered, each gas piping is connected, the first air inlet 6-2A connects oxygen, and the first air inlet 6-2B connects
Argon gas, first shuts the valve of oxygen, opens argon gas valve, is passed through argon gas.
11) heating schedule is set by computer, is kept for 20 minutes after being heated to 600 DEG C with the speed of 100 DEG C/s.
12) oxygen valve is opened after 600 DEG C after temperature stabilization, being passed through oxygen makes coal sample burn, and flow is 50mL/min.
13) coal sample after-flame is treated, during thermogravimetric curve kept stable, terminates data acquisition, preserve data.
As it will be easily appreciated by one skilled in the art that the foregoing is only presently preferred embodiments of the present invention, it is not used to
The limitation present invention, all any modification, equivalent and improvement made within the spirit and principles in the present invention etc., all should include
Within protection scope of the present invention.
Claims (6)
1. one kind is rapidly heated thermogravimetric analyzer, it is characterised in that including pedestal, electronic analytical balance, open support pipe, plus
Thermal, temperature control system, cloche and equipment data acquisition analyzing, wherein,
The pedestal includes balance room, rebasing adjustment stud and support rim, and the balance room is hollow, the rebasing adjustment stud
It is arranged on the inner bottom surface of balance room, the support rim is located at balance room top and is accepted by the platform room, this
Outward, it is provided with cable tray on the support rim；
The electronic analytical balance is arranged in the balance room and is accepted by the rebasing adjustment stud；
The open support pipe is vertically arranged, and it passes through the electronic analysis after passing through the support rim and the balance room
Balance is accepted, and the side wall of the open support pipe has multiple through holes；
The heater includes inverted U copper pipe, wire netting reactor and electrode, two ends rests of the inverted U copper pipe
On the support rim and its inner chamber connects with the cable tray of the support rim, the wire netting reactor passes through institute
The undertaking of open support pipe is stated, the electrode is arranged on the inverted U copper pipe and by connecting wire and the wire netting
Reactor is connected, additionally, the electrode also connects the temperature control system by current supply line, for the wire netting
Reactor is powered heating, and the current supply line passes through the support rim from the cable tray of the support rim, and from described
Opening on the inner chamber and side wall of inverted U copper pipe is through the copper pipe of falling inverted U；
The temperature control system includes thermocouple, holding wire and temperature controller, and the thermocouple is fixedly mounted on the U
The top of type copper pipe, it passes through the holding wire and is connected with the temperature controller, and described from supporting convex described in holding wire
The cable tray of platform passes through the support rim, and opening from the inner chamber and side wall of the inverted U copper pipe through it is described fall
Inverted U copper pipe, the temperature controller connects the electrode by the current supply line；
The cloche is accepted by the support rim and covers the open support pipe, wire netting reactor and inverted U
Copper pipe, the side wall of the cloche is provided with air inlet and its top is provided with exhaust outlet；
The equipment data acquisition analyzing is connected with the electronic analytical balance and the temperature controller respectively.
2. one kind according to claim 1 is rapidly heated thermogravimetric analyzer, it is characterised in that the wire netting reactor is
2~4 layers of metal net folding are formed.It is connected with open support pipe top screw by screw.
3. one kind according to claim 1 is rapidly heated thermogravimetric analyzer, it is characterised in that the wire netting reactor with
Splitting is provided between the open support pipe.
4. one kind according to claim 1 is rapidly heated thermogravimetric analyzer, it is characterised in that the temperature controller according to
The temperature signal that the thermocouple is measured, the temperature value with setting is compared, and feedback signal is formed, so as to control wire netting anti-
The electric current on device is answered, to change heating power, and then temperature to wire netting reactor is adjusted correction.
5. one kind according to claim 1 is rapidly heated thermogravimetric analyzer, it is characterised in that the quantity of the thermocouple is
Two, wherein a thermometric end for thermocouple is located at wire netting reactor overcentre, the thermometric end of another thermocouple is located at
Wire netting reactor edge top.
6. one kind according to claim 1 is rapidly heated thermogravimetric analyzer, it is characterised in that the cloche and the branch
The joint for supportting boss is provided with sealing ring.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710077975.8A CN106769606A (en) | 2017-02-14 | 2017-02-14 | One kind is rapidly heated thermogravimetric analyzer |
| PCT/CN2017/112772 WO2018149208A1 (en) | 2017-02-14 | 2017-11-24 | Thermogravimetric analyser with rapid temperature rise |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710077975.8A CN106769606A (en) | 2017-02-14 | 2017-02-14 | One kind is rapidly heated thermogravimetric analyzer |
Publications (1)
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| CN106769606A true CN106769606A (en) | 2017-05-31 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710077975.8A Pending CN106769606A (en) | 2017-02-14 | 2017-02-14 | One kind is rapidly heated thermogravimetric analyzer |
Country Status (2)
| Country | Link |
|---|---|
| CN (1) | CN106769606A (en) |
| WO (1) | WO2018149208A1 (en) |
Cited By (6)
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| CN108007809A (en) * | 2017-12-08 | 2018-05-08 | 中国科学院广州能源研究所 | One kind is rapidly heated wide-range thermogravimetric analyzer |
| WO2018149208A1 (en) * | 2017-02-14 | 2018-08-23 | 华中科技大学 | Thermogravimetric analyser with rapid temperature rise |
| CN108956361A (en) * | 2018-04-11 | 2018-12-07 | 华中科技大学 | The magnetic suspension thermobalance measurement method being rapidly heated based on photo-thermal |
| CN108956360A (en) * | 2018-04-11 | 2018-12-07 | 华中科技大学 | The magnetic suspension thermobalance being rapidly heated based on photo-thermal |
| CN109541009A (en) * | 2018-11-15 | 2019-03-29 | 中国科学院广州能源研究所 | A kind of silk screen instant heating and quick mass spectrum gas-solid facies analysis instrument |
| CN110470559A (en) * | 2019-05-15 | 2019-11-19 | 华北电力大学（保定） | A kind of solid high-temperature high pressure chemistry reactive kinetics parameters acquisition methods and device |
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| CN115824874B (en) * | 2022-09-26 | 2023-09-29 | 南京航空航天大学 | Direct photothermal heavy high-precision analyzer and working method thereof |
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| Publication number | Publication date |
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| WO2018149208A1 (en) | 2018-08-23 |
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