CN106950252A - A kind of dynamic measurement fine grained sample burning and the device and the method using the measurement device characterisitic parameter of sintering characteristic - Google Patents
A kind of dynamic measurement fine grained sample burning and the device and the method using the measurement device characterisitic parameter of sintering characteristic Download PDFInfo
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- CN106950252A CN106950252A CN201710154016.1A CN201710154016A CN106950252A CN 106950252 A CN106950252 A CN 106950252A CN 201710154016 A CN201710154016 A CN 201710154016A CN 106950252 A CN106950252 A CN 106950252A
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- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/20—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity
- G01N25/22—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity on combustion or catalytic oxidation, e.g. of components of gas mixtures
- G01N25/28—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity on combustion or catalytic oxidation, e.g. of components of gas mixtures the rise in temperature of the gases resulting from combustion being measured directly
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Abstract
A kind of dynamic measurement fine grained sample burning and the device and the method using the measurement device characterisitic parameter of sintering characteristic, are related to the burning of fine grained sample and sintering characteristic parameter measuring technical field.The present invention is to solve existing apparatus in dynamically measurement fuel combustion process, it is impossible to the problem of accurate measurement burning performance parameter.A kind of dynamic measurement fine grained sample burning of the present invention and the device of sintering characteristic, video acquisition device is located at the head end of quartz ampoule, the end of quartz ampoule is tightly connected with seal, sample to be tested is located at quartz ampoule center, the outlet side of gas circuit inside sample to be tested with connecting, gas circuit is provided with flow control valve, the change in size of sample to be tested, centre of sphere temperature and environmental stress are gathered in real time using video acquisition device, temperature collecting device and pressure harvester, obtain the characterisitic parameter of sample to be tested.The present invention is applied to the burning of measurement fine grained sample and sintering characteristic parameter.
Description
Technical field
The invention belongs to the burning of fine grained sample and sintering characteristic parameter measuring technical field.
Background technology
Coal is the main energy sources of China, accounts for more than the 65% of disposable total energy consumption, continuous with coal fired power generation
Increase, all kinds of coal ash that estimation coal-burning power plant is produced every year are more than 500,000,000 tons.The huge discharge of coal ash, a large amount of soils are not only taken up,
Environment is polluted, while also the development of the national economy development to China is exerted heavy pressures on.Wherein greatly have very excellent
Performance, construction material, road backfill are mainly used in, in terms of chemical industry, with boundless application prospect and ring
Support value value.Therefore for the quick and precisely measurement of coal ash sintering characteristic and mechanism, the kinetic parameter of sintering is obtained, can be safety
Stably use and easily stain the theoretical foundation that the inferior fuel of sintering is established and optimized.In addition, some flammable fine particles
Need to be used by shaping, the gasification char that for example gasification furnace is produced, its particle is generally very thin and is difficult to burn.If passing through
The form of shaping burning can extend its residence time, so as to obtain higher efficiency of combustion, recover energy.
University of Newcastle University of Newcastle scholars A.Y.Al-Otoom were sent out in 2000
Proposed first in the article of table using porosity change between pressure decline method measurement fine grained, to determine the sintering initial temperature of coal ash simultaneously
Sintering kinetics parameter is calculated, realizes and Slagging dust stratification is accurately predicted.Under high temperature action, sent out inside coal ash
Raw complicated physical and chemical reaction, makes the reduction of inner surface, and stomata shrinks growth, and interparticle contact face is increased, and improves mechanical strong
Degree.Pressure decline method surveys sintering temperature and its mechanism of kinetic parameter is：With the increase of open pore volume, pass through gray columns gas
Pressure drop decreases, therefore can characterize sintering temperature and kinetic parameter to the test of air-flow pressure drop.Then, lot of domestic and foreign
Research institution and scholar quote to said apparatus to use for reference, such as Tsing-Hua University, Zhejiang University, University of West Australia.But its device exists
Still there is room for improvement in terms of sample size, Pore development response interval and a variety of sintering characteristic parameters of composite measurement.
In burning inferior coal, oil shale and biomass, the parameter of its combustion characteristics is weighed mainly around fuel particle temperature
Degree changing rule, the index Fi that such as catches fire, ignition temperature Ti, ignition time t, maximum weight-loss ratio temperature Tmax, Burn-out temperature Tb,
And influence factor suffered by inferior fuel burning quality is numerous, component, species, combustion atmosphere, gas flow rate and material as samples
Shape.Domestic and foreign scholars is realize measurement features described above parameter, and phenomenon in observation combustion process simultaneously, and design has been built a variety of
The experimental provision of form, such as by observing Ignition Phenomena, ignition temperature and ignition delay time, research coal slime combustion characteristics and
Fiery characteristic.But central temperature and appearance and size change of the device in existing literature still in dynamically measurement fuel combustion process
Upper existing defects.Therefore, all-sidedly and accurately the form in each stage becomes in measurement combustion characteristic parameter, and record analysis whole process
Change, to full appreciation inferior fuel combustion characteristics, realization is comprehensively utilized to it with deep directive significance.
The content of the invention
The present invention is to solve existing apparatus in dynamically measurement fuel combustion process, it is impossible to which accurate measurement burning is special
Property parameter the problem of, the device of a kind of dynamic measurement fine grained sample burning and sintering characteristic is now provided and the measurement device is utilized
The method of characterisitic parameter.
A kind of dynamic measurement fine grained sample burning and the device of sintering characteristic, including：Video acquisition device 1, heating furnace
2-1, temperature collecting device 5, seal 6, pressure harvester 7 and flowmeter 8；
Heating furnace 2-1 includes heating and thermal insulation layer and quartz ampoule 2-2, and heating and thermal insulation layer is wrapped on the outside of quartz ampoule 2-2,
Video acquisition device 1 is located at quartz ampoule 2-2 head end, and quartz ampoule 2-2 end and seal 6 are tightly connected, treated
Test specimens 3 are located at quartz ampoule 2-2 centers,
The outlet side of gas circuit 10 is connected by seal 6 with the inside of sample to be tested 3, and gas circuit 10 is provided with flow control valve 9,
Video acquisition device 1 is used for the change in size process for gathering sample to be tested 3,
Temperature collecting device 5 is used for the centre of sphere temperature for gathering sample to be tested 3,
Pressure harvester 7 is used to gather the internal pressure of sample to be tested 3,
Flowmeter 8 is used for the gas flow for adjusting and measuring gas circuit 10.
Above-mentioned heating furnace 2-1 is programmable horizontal heating furnace.
Above-mentioned quartz ampoule 2-2 head end is sealed using transparency window.
Above-mentioned quartz ampoule 2-2 head end is in open state.
Above-mentioned seal 6 is the circular cylindrical cavity of inner hollow, the two ends of seal 6 and side wall be equipped with can with it
The opening of chamber connection, and opening and the opening of side-walls at the head end of seal 6 is equipped with connection screw thread 6-3,
Seal 6 can be connected by the connection screw thread 6-3 of its head end with gas circuit 10,
The other end of seal 6 is connected with quartz ampoule 2-2,
Seal 6 can be connected by the connection screw thread 6-3 of its side wall with temperature collecting device 5 so that temperature acquisition is filled
The collection terminal for putting 5 enters inside sample to be tested 3 through seal 6,
Seal 6 is provided with the junction of temperature collecting device 5 and screws gland 6-1,
Sealing gasket ring recess 6-2 is provided with the outside of the screw thread 6-3 of the other end of seal 6 and side wall, for filling seal washer.
The device of a kind of above-mentioned dynamic measurement fine grained sample burning and sintering characteristic also includes sealing flange 4,
Quartz ampoule 2-2 is tightly connected by sealing flange 4 with seal 6.
The device of a kind of above-mentioned dynamic measurement fine grained sample burning and sintering characteristic also includes alundum tube,
Alundum tube is hollow tubular structure, and one end of alundum tube is fixed on seal 6, and alundum tube and seal 6
Inner chamber connection, sample to be tested 3 is fixed on the other end of alundum tube, and the collection terminal of temperature collecting device 5 is worn inside alundum tube
Cross seal 6 and at the centre of sphere of sample to be tested 3.
The device of a kind of above-mentioned dynamic measurement fine grained sample burning and sintering characteristic also includes axial feed device 11,
Axial feed device 11 is used for band dynamic seal 6 and is axially moved along quartz ampoule 2-2.
Above-mentioned quartz ampoule 2-2 side wall is provided with branch pipe.
Using a kind of above-mentioned dynamic measurement fine grained sample burning and the method for the measurement device characterisitic parameter of sintering characteristic,
This method is：
Sample to be tested 3 is placed in quartz ampoule 2-2, and the centre of sphere of sample to be tested 3 is adjusted to quartz ampoule 2-2 center
Place,
Heating furnace 2-1 is opened to heat up for the local environment of sample to be tested 3,
Change the gas flow for being passed through the local environment of sample to be tested 3 using flowmeter 8,
Gather the size of sample to be tested 3 in real time using video acquisition device 1, temperature collecting device 5 and pressure harvester 7
Change, centre of sphere temperature and environmental stress, obtain the characterisitic parameter of sample to be tested 3.
Beneficial effects of the present invention：
1 device of the present invention can carry out convenient and reliable installation and removal, overcome sealing property with frequently changing
The contradictory problems of material.During assembling, the mode being bolted connection is adopted between alundum tube and customization seal, and add using packing ring
Strong sealing property.By axial feeding system, push-in and release of the sample in assigned temperature can be realized, experimental implementation spirit is enhanced
Activity and accuracy.
2 devices of the present invention connect quartz ampoule with customization seal when by the way of flange seal, Neng Gouling
Gaseous species and pressure in control quartz ampoule living, fully meet the universality of experimental provision.According to different experimental conditions, it can adjust
Ambiance is oxygen-enriched, flue gas, air or reducing atmosphere, can also realize normal pressure, pressurization or change the conditions such as gas flow rate.
3 by measuring turning for the changing rule of sample internal pressure curve in burning and sintering process, i.e. falloff curve
Point, development trend monitoring that can be to its internal void and sign, more accurately determine initial sintering temperature, so as to calculate burning
Tie kinetic parameter.
4 camera devices can realize that, to the real-time monitoring in Experimental Area, dynamic measures the change in size on radially projecting direction.One
Aspect, in inferior fuel combustion process, can directly judge the critical characteristic parameter such as ignition temperature, and Real Time Observation fired state
And flame characteristic；On the other hand, when measuring sintering parameter, original scheme is substituted using change in size circular on projection plane
The portion size change of middle round platform, excludes the influence that outside out-phase contact surface changes to sample form, realizes to diameter expansion/receipts
Accurately observation and successive image processing, the measurement of contracting and circularity.
Brief description of the drawings
Fig. 1 is a kind of dynamic measurement fine grained sample burning of the present invention and the structural representation of the device of sintering characteristic
Figure；
Fig. 2 is the structural representation of seal.
Embodiment
Embodiment one：Reference picture 1 illustrates present embodiment, one kind dynamic measurement described in present embodiment
The device that fine grained sample burns with sintering characteristic, including：Video acquisition device 1, heating furnace, temperature collecting device 5, seal
6th, pressure harvester 7 and flowmeter 8；
Heating furnace 2-1 includes heating and thermal insulation layer and quartz ampoule 2-2, and heating and thermal insulation layer is wrapped on the outside of quartz ampoule 2-2,
Video acquisition device 1 is located at quartz ampoule 2-2 head end, and quartz ampoule 2-2 end and seal 6 are tightly connected, treated
Test specimens 3 are located at quartz ampoule 2-2 centers,
The outlet side of gas circuit 10 is connected by seal 6 with the inside of sample to be tested 3, and gas circuit 10 is provided with flow control valve 9,
Video acquisition device 1 is used for the change in size process for gathering sample to be tested 3,
Temperature collecting device 5 is used for the centre of sphere temperature for gathering sample to be tested 3,
Pressure harvester 7 is used to gather the internal pressure of sample to be tested 3,
Flowmeter 8 is used for the gas flow for adjusting and measuring gas circuit 10.
In present embodiment, video acquisition device 1 be located at quartz ampoule 2-2 head end, can dynamic acquisition sample to be tested 3 exist
Change in size on quartz ampoule 2-2 radially projectings direction.
The temperature acquisition end of temperature collecting device 5 can directly be inserted into the center of sample to be tested 3, realize to sample to be tested 3
The real-time record of internal temperature.
Gas circuit 10 is provided with flow control valve 9, by the component and flow that adjust gas in gas circuit 10, thus it is possible to vary to be measured
Atmosphere and pressure of the sample 3 in measurement process, can be with the Pore development degree and change procedure of dynamic reflection sample to be tested 3.
Present embodiment is in use, heating furnace assembling thermocouple, is that quartz ampoule 2-2 internal environments are heated, utilizes
Flow control valve 9 adjusts gas flow rate, it becomes possible to the central temperature in whole burning and sintering process of direct measurement sample to be tested 3
With the dynamic change of internal pressure.
Slow down heating rate near critical characteristic temperature, usable high-speed camera replaces high-definition camera, and concentration is put
Big observation sample slight change.
Embodiment two：Present embodiment is to one kind dynamic measurement fine grained examination described in embodiment one
Sample is burnt and the device of sintering characteristic is described further, in present embodiment, and heating furnace is programmable horizontal heating furnace.
Embodiment three：Present embodiment is to one kind dynamic measurement fine grained examination described in embodiment one
Sample is burnt and the device of sintering characteristic is described further, in present embodiment, and quartz ampoule 2-2 head end is close using transparency window
Envelope.
In present embodiment, quartz ampoule 2-2 head end is sealed using transparency window, and now quartz ampoule 2-2 is whole sealing status,
It can be needed to adjust quartz ampoule 2-2 internal gas pressure according to measurement, while video acquisition device 1 can also be adopted by transparency window
Collect the change in size process of sample to be tested 3.
Embodiment four：Present embodiment is to one kind dynamic measurement fine grained examination described in embodiment one
Sample is burnt and the device of sintering characteristic is described further, in present embodiment, and quartz ampoule 2-2 head end is in open state.
In present embodiment, quartz ampoule 2-2 head end is in open state, quartz ampoule 2-2 air pressure insides and ambient pressure phase
Together, it is adaptable to which the style to be measured 3 under room pressure condition is detected.
Embodiment five：Reference picture 2 illustrates present embodiment, and present embodiment is to embodiment one
A kind of described dynamic measurement fine grained sample burning and the device of sintering characteristic are described further, close in present embodiment
Sealing 6 is the circular cylindrical cavity of inner hollow, and the two ends of seal 6 and side wall are equipped with the opening that can be connected with its inner chamber,
And the opening and the opening of side-walls at the head end of seal 6 are equipped with connection screw thread 6-3,
Seal 6 can be connected by the connection screw thread 6-3 of its head end with gas circuit 10,
The other end of seal 6 is connected with quartz ampoule 2-2,
Seal 6 can be connected by the connection screw thread 6-3 of its side wall with temperature collecting device 5 so that temperature acquisition is filled
The collection terminal for putting 5 enters inside sample to be tested 3 through seal 6,
Seal 6 is provided with the junction of temperature collecting device 5 and screws gland 6-1,
Sealing gasket ring recess 6-2 is provided with the outside of the screw thread 6-3 of the other end of seal 6 and side wall, for filling seal washer.
Embodiment six：Present embodiment is to one kind dynamic measurement fine grained examination described in embodiment five
Sample is burnt and the device of sintering characteristic is described further, in present embodiment, and it also includes sealing flange 4, and quartz ampoule 2-2 leads to
Sealing flange 4 is crossed to be tightly connected with seal 6.
Embodiment seven：Present embodiment is to one kind dynamic measurement fine grained examination described in embodiment five
Sample is burnt and the device of sintering characteristic is described further, in present embodiment, and it also includes alundum tube,
Alundum tube is hollow tubular structure, and one end of alundum tube is fixed on seal 6, and alundum tube and seal 6
Inner chamber connection, sample to be tested 3 is fixed on the other end of alundum tube, and the collection terminal of temperature collecting device 5 is worn inside alundum tube
Cross seal 6 and at the centre of sphere of sample to be tested 3.
Embodiment eight：Present embodiment is to one kind dynamic measurement fine grained examination described in embodiment seven
Sample is burnt and the device of sintering characteristic is described further, in present embodiment, and it also includes axial feed device 11,
Axial feed device 11 is used for band dynamic seal 6 and is axially moved along quartz ampoule 2-2.
In present embodiment, axial feed device 11 can be axially moved with dynamic seal 6 along quartz ampoule 2-2, and then band
The alundum tube being fixed on seal 6 has been moved, the purpose of adjustment sample to be tested 3 position is finally reached.
Embodiment nine：Present embodiment is to one kind dynamic measurement fine grained examination described in embodiment one
Sample is burnt and the device of sintering characteristic is described further, in present embodiment, and quartz ampoule 2-2 side wall is provided with branch pipe.
Pass through the branch pipe on quartz ampoule 2-2, thus it is possible to vary ambiance residing for sample to be tested 3 is oxygen-enriched, air, flue gas,
Reducing atmosphere and pressure.
Embodiment ten：Present embodiment is to utilize the dress described in any embodiment of embodiment one to nine
The method for putting measurement characteristicses parameter, this method is：
Sample to be tested 3 is placed in quartz ampoule 2-2, and the centre of sphere of sample to be tested 3 is adjusted to quartz ampoule 2-2 center
Place,
Heating furnace is opened to heat up for the local environment of sample to be tested 3,
Pass through the branch pipe on quartz ampoule 2-2, thus it is possible to vary ambiance residing for sample to be tested 3 is oxygen-enriched, air, flue gas,
Reducing atmosphere and pressure.
Change the gas flow for being passed through sample to be tested 3 using flow control valve 9,
Gather the size of sample to be tested 3 in real time using video acquisition device 1, temperature collecting device 5 and pressure harvester 7
Change, centre of sphere temperature and environmental stress, obtain the characterisitic parameter of sample to be tested 3.
In present embodiment, the temperature program of heating furnace is set according to experimental condition and keeps constant, sample to be tested 3 is straight
Connect push-in quartz ampoule 2-2 centers, combustion process of the simulation sample to be tested 3 in actual device, while starting video acquisition dress
1 is put, the size and pattern in on-line monitoring sample burning each stage change.
Specific embodiment
A kind of dynamic measures the burning of fine grained sample and the method for sintering characteristic parameter, and this method is：
Sample to be tested 3 is fixed on to the front end of alundum tube, the end of alundum tube is fixed in seal 6, and is caused firm
Jade pipe is connected with the inner chamber of seal 6, and sample to be tested 3 is fixed on to quartz ampoule 2-2 center by axial feed device 11,
Quartz ampoule 2-2 and seal 6 are locked using sealing flange 4；
Heating schedule is set to heating furnace, starts video acquisition device 1, temperature collecting device 5 and pressure harvester 7,
Flow control valve 9 is opened, regulation to flowmeter 8 shows test requirements document mass flow, dynamically recording sample relevant feature parameters.
In a heated condition, internal void gradually develops sample to be tested 3, is presented in the real-time change of internal pressure；With
Temperature rise, inner material can volatilize or reunite, and can pass through video acquisition device recording surface pattern and change in size；Directly
The grey ball center's temperature of measurement and surface temperature are connect, is excluded as the influence such as heat transfer resistance caused by the specimen finish that can not ignore.
Claims (10)
1. a kind of dynamic measurement fine grained sample burning and the device of sintering characteristic, it is characterised in that including：Video acquisition device
(1), heating furnace (2-1), temperature collecting device (5), seal (6), pressure harvester (7) and flowmeter (8)；
Heating furnace (2-1) includes heating and thermal insulation layer and quartz ampoule (2-2), and heating and thermal insulation layer is wrapped on the outside of quartz ampoule (2-2),
Video acquisition device (1) is located at the head end of quartz ampoule (2-2), and the end of quartz ampoule (2-2) is sealed with seal (6) to be connected
Connect, sample to be tested (3) is located at quartz ampoule (2-2) center,
The outlet side of gas circuit (10) inside sample to be tested (3) by seal (6) with connecting, and gas circuit (10) is provided with Flow-rate adjustment
Valve (9),
Video acquisition device (1) is used for the change in size process for gathering sample to be tested (3),
Temperature collecting device (5) is used for the centre of sphere temperature for gathering sample to be tested (3),
Pressure harvester (7) is used to gather sample to be tested (3) internal pressure,
Flowmeter (8) is used for the gas flow for adjusting and measuring gas circuit (10).
2. a kind of dynamic measurement fine grained sample burning according to claim 1 and the device of sintering characteristic, its feature exist
In heating furnace (2-1) is programmable horizontal heating furnace.
3. a kind of dynamic measurement fine grained sample burning according to claim 1 and the device of sintering characteristic, its feature exist
In the head end of quartz ampoule (2-2) is sealed using transparency window.
4. a kind of dynamic measurement fine grained sample burning according to claim 1 and the device of sintering characteristic, its feature exist
In the head end of quartz ampoule (2-2) is in open state.
5. a kind of dynamic measurement fine grained sample burning according to claim 1 and the device of sintering characteristic, its feature exist
In seal (6) is the circular cylindrical cavity of inner hollow, and the two ends of seal (6) and side wall are equipped with and can connected with its inner chamber
The opening of opening and side-walls at logical opening, and seal (6) head end is equipped with connection screw thread (6-3),
Seal (6) can be connected by the connection screw thread (6-3) of its head end with gas circuit (10),
The other end of seal (6) is connected with quartz ampoule (2-2),
Seal (6) can be connected by the connection screw thread (6-3) of its side wall with temperature collecting device (5) so that temperature acquisition
The collection terminal of device (5) enters sample to be tested (3) inside through seal (6),
Seal (6) is provided with the junction of temperature collecting device (5) and screws gland (6-1),
Sealing gasket ring recess (6-2) is provided with the outside of the screw thread (6-3) of seal (6) other end and side wall, for filling seal washer.
6. a kind of dynamic measurement fine grained sample burning according to claim 5 and the device of sintering characteristic, its feature exist
In, it also includes sealing flange (4),
Quartz ampoule (2-2) is tightly connected by sealing flange (4) with seal (6).
7. a kind of dynamic measurement fine grained sample burning according to claim 5 and the device of sintering characteristic, its feature exist
In, it also includes alundum tube,
Alundum tube is hollow tubular structure, and one end of alundum tube is fixed on seal (6), and alundum tube and seal (6)
Inner chamber connection, sample to be tested (3) is fixed on the other end of alundum tube, and the collection terminal of temperature collecting device (5) is out of alundum tube
Portion is through seal (6) and at the centre of sphere of sample to be tested (3).
8. a kind of dynamic measurement fine grained sample burning according to claim 7 and the device of sintering characteristic, its feature exist
In, it also includes axial feed device (11),
Axial feed device (11) is used for band dynamic seal (6) and is axially moved along quartz ampoule (2-2).
9. a kind of dynamic measurement fine grained sample burning according to claim 1 and the device of sintering characteristic, its feature exist
In the side wall of quartz ampoule (2-2) is provided with branch pipe.
10. utilize a kind of dynamic measurement fine grained sample burning described in any one of claim 1 to 9 and the device of sintering characteristic
The method of measurement characteristicses parameter, it is characterised in that this method is：
Sample to be tested (3) is placed in quartz ampoule (2-2), and the centre of sphere of sample to be tested (3) is adjusted into quartz ampoule (2-2)
At the heart,
Heating furnace (2-1) is opened to heat up for sample to be tested (3) local environment,
Change the gas flow for being passed through sample to be tested (3) local environment using flowmeter (8),
Sample to be tested (3) is gathered in real time using video acquisition device (1), temperature collecting device (5) and pressure harvester (7)
Change in size, centre of sphere temperature and environmental stress, obtain the characterisitic parameter of sample to be tested (3).
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| CN109490360A (en) * | 2018-12-29 | 2019-03-19 | 中国科学技术大学 | It is a kind of suitable for large sample amount, more atmosphere can be with differential thermal analysis device |
| CN111239183A (en) * | 2020-03-10 | 2020-06-05 | 嘉兴学院 | Device and method for measuring dynamic thermal conductivity coefficient of silver nanoparticle conductive ink in sintering process |
| CN111239183B (en) * | 2020-03-10 | 2022-03-18 | 嘉兴学院 | Device and method for measuring dynamic thermal conductivity coefficient of silver nanoparticle conductive ink in sintering process |
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