CN104458798B - In-situ test method for high-pressure low-temperature heat conductivity coefficients and heat transfer coefficients - Google Patents
In-situ test method for high-pressure low-temperature heat conductivity coefficients and heat transfer coefficients Download PDFInfo
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- CN104458798B CN104458798B CN201410617225.1A CN201410617225A CN104458798B CN 104458798 B CN104458798 B CN 104458798B CN 201410617225 A CN201410617225 A CN 201410617225A CN 104458798 B CN104458798 B CN 104458798B
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- NMJORVOYSJLJGU-UHFFFAOYSA-N methane clathrate Chemical compound C.C.C.C.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O NMJORVOYSJLJGU-UHFFFAOYSA-N 0.000 description 10
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 8
- 238000002474 experimental method Methods 0.000 description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
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Abstract
The invention discloses an in-situ test method for high-pressure low-temperature heat conductivity coefficients and heat transfer coefficients. The heat conductivity coefficients and the heat transfer coefficients of media are measured based on a point heat source thermistor method. The power of a thermistor is determined, and the heat conductivity coefficient and the heat transfer coefficient of a measured medium are obtained according to the resistance feedback and temperature attenuation data of the thermistor by utilizing a calculation model. The method comprises the following steps: correcting parameters of a thermistor measurement model; slowly extruding a to-be-measured medium by utilizing a piston on the lower part of a reaction kettle, and unifying the standard of to-be-detected samples; introducing reactive gas and controlling the pressure and temperature in a target range; and inputting the determined power value into the thermistor by virtue of a power input control system, acquiring the resistance value and temperature value of the thermistor by utilizing a data acquisition device, and finally, obtaining the heat conductivity coefficient and the heat transfer coefficient by utilizing the calculation model. According to the design of the invention, in-situ synthesis of different media under high pressure and at low temperature can be met, and in-situ measurement of the heat conductivity coefficients and heat transfer coefficients of multi-phase condition substances in different spaces and different time is realized.
Description
Technical field
The present invention relates to a kind of home position testing method for high pressure low temperature heat conductivity, heat transfer coefficient, belong to heat transfer and survey
Examination technical field.
Background technology
It is the relative survey of a kind of measurement different medium heat conductivity, heat transfer coefficient based on critesistor heat point source measuring system
Amount method.The power that critesistor is specified, critesistor and measurement thing sample directly contact are supplied by constant voltage dc source, according to
Critesistor own temperature attenuation data simultaneously calculates heat conductivity and the heat transfer coefficient of testing medium using computation model.This skill
Art method is applicable to measure heat conductivity and heat transfer coefficient under different condition, inside different porous media, by using high pressure
Thermosensitive resistance measurement probe can be inserted in high pressure low temperature reactor by sealing device, and in site measurement multi phase state medium forces down in height
Heat conductivity under the conditions of temperature and heat transfer coefficient.For the medium of the presence multi phase state under cryogenic high pressure, by piston to measurement
Standardization suppressed by thing sample, and the method for multiple spot original position real-time online measuring can obtain different spaces and not heat conduction in the same time
Coefficient, can calculate heat transfer coefficient by heat transfer model simultaneously for the multi phase state medium that there is flowing.Traditional heat-pole method
Measure thing sample heat conductivity with platen surface heat resource method, apply more in atmospheric conditions, but application under the conditions of cryogenic high pressure
Less, under conditions of multi phase state, poor in ease for use and simple operation degree.Further, since traditional heat
Collimation method and platen surface heat resource method caloric value are generally larger, under multi phase state material coexists, easily cause multi phase state material itself
Physical property and the change of state, thus causing larger measurement error, have certain limitation, simultaneously tradition during application
Heat-pole method and platen surface heat resource method on not yet realize the synchro measure of heat conductivity and heat transfer coefficient.Measure high at present in the original location
Force down the heat conductivity under multi phase state under the conditions of temperature and heat transfer coefficient method of testing have not been reported.
Content of the invention
In order to solve the problems, such as that in above high pressure low temperature multi phase state heat conductivity and heat transfer coefficient measurement process, the present invention exists
Develop one kind on the basis of a kind of in-situ measurement device of high pressure low temperature heat conductivity heat transfer coefficient to be used for measuring high pressure low temperature bar
Multi phase state material heat conductivity and heat transfer coefficient method of testing under part, multi phase state material under its mesh online in site measurement high pressure low temperature
Heat conductivity and heat transfer coefficient.
The technical solution used in the present invention is:
A kind of high pressure low temperature heat conductivity, the in-situ testing device of heat transfer coefficient, including thermosensitive resistance measurement probe, high pressure
Low-temp reaction kettle, power input control system and data collecting system etc.；Thermosensitive resistance measurement probe is temperature-sensitive from bottom to top
Resistance, high pressure seal and circuit control panel.The lower end that critesistor is popped one's head in thermosensitive resistance measurement, thermosensitive resistance measurement is visited
Head mid portion is high pressure seal, and the cavity on thermosensitive resistance measurement probe top is connected with circuit control panel；Critesistor
It is inserted directly in high pressure low temperature reactor, middle high pressure seal is connected with high pressure low temperature reactor, thermosensitive resistance measurement
The top of probe is outside high pressure low temperature reactor.
The connecting wire of critesistor, using insulation lacquer coat, prevents circuit from producing after contacting with the medium containing liquid short
Road.The connecting wire of the critesistor after process first passes through rustless steel tubule, is then passed through high pressure seal.Epoxy resin fills
The rustless steel tubule of note is used for parcel protection connecting wire, and critesistor is fixed on the port of rustless steel tubule simultaneously.High pressure
The connecting wire of critesistor is extruded using pressure-resistant plastic, for high pressure sealing is carried out to connecting wire inside sealing device；No
Rust steel tubule is fixed using adhering with epoxy resin with high pressure seal, in order to avoid in environment under high pressure, inside and outside stainless steel tube
Produce huge pressure reduction, uniform punching process is carried out on rustless steel tubule, aperture 1mm, pitch-row 15mm, for eliminating inside and outside pipeline
Pressure reduction, is thus inserted into all elements in autoclave all under pressure balanced environment, work that can be more stable.
Wherein thermosensitive resistance measurement probe is connected with high pressure low temperature reactor using snap joint, is easily installed and dismantles.
Mainly there are change resistance and circuit protecting element on circuit control panel, become resistance and be used for adjusting current value in circuit, circuit protection unit
Part is used for preventing transient current in circuit excessive, protects critesistor and whole circuit.The top electricity of thermosensitive resistance measurement probe
Road delivery outlet is connected with outside direct current of voltage regulation source control system data acquisition system, and constant voltage dc source is used for temperature-sensitive
Resistance is powered, and being capable of curent change in control circuit.In the resistance value of data acquisition system critesistor and circuit
The parameters such as current value.
High pressure low temperature reactor has two Room, is connected by piston between two Room, and measurement thing sample is directly placed into high pressure low temperature reaction
In the upper room of kettle.Piston is promoted in the water filling of high pressure low temperature reactor lower end by constant pressure pump, for suppressing the measurement thing of upper interior
Sample, is standardized suppressing to measurement thing sample using constant pressure.High pressure low temperature reactor top is reserved with temperature sensor and connects
Mouth, pressure sensor interface, thermosensitive resistance measurement probe interface and air intake-exhaust interface；Above-mentioned interface is all connect using snap joint
Mouthful, position all can exchange.Displacement transducer is located at high pressure low temperature reactor lower cover center, can detect piston movement displacement
And determine the volume of high pressure low temperature reactor two Room.Wherein gas and liquid can be inputted to high pressure using constant flow pump, air accumulator
In low-temp reaction kettle, gases at high pressure can also be discharged from air vent with the pressure setting, discharge under the control of counterbalance valve in addition
The gas-liquid discharged can measure its flow velocity and integrated flow by effusion meter.Temperature sensor, pressure transducer and temperature-sensitive electricity
Resistance measuring probe synchronously measures online, and by unified for data output, carries out leading of computation and measurement thing sample using computation model
Hot coefficient and Local Heat Transfer Coefficient.
On above-mentioned rustless steel tubule, the aperture of uniformly punching is 1mm, and pitch-row is 15mm.
Home position testing method is carried out using above-mentioned in-situ testing device, comprises the steps:
The first step, is corrected to thermosensitive resistance measurement model parameter
Using standard substance according to the characteristic of testing medium respectively to β, α, t, the k in formula (1)-(5)bCarry out school with d
Just, carry out survey calculation after correction；
In formula (1)-(5), r: critesistor resistance, ω；β: thermistor temp coefficient；T: critesistor itself temperature
Degree, k；km: testing medium heat conductivity, w/m k；A: critesistor radius, m；δ t: temperature increment on thermal resistor, k；P: critesistor
Heating power, w；kb: thermistor probe heat conductivity, w/m k；nud: average nusselt number, hd/kf；kf: testing medium
Heat conductivity, w/m k；D: critesistor heat transfer model diameter, m；T: critesistor heat transfer model thickness, m；rs: measuring resistance
Resistance, ω；V: thermistor voltage pressure drop, v；vs: measuring resistance voltage drop, v；α: critesistor meter constant, ω；K: heat
Itself heat conductivity of quick Resistance probe, w/m k；bit: biot number；H: mean heat transfer coefficient, w/m2k；
Second step, filling measurement thing sample makes standard testing sample
Open lid on high pressure low temperature reactor, insert solid to be measured and liquid, after covering bonnet, insertion temperature, pressure, heat
Quick resistance measurement probe；The diverse location of multiple thermosensitive resistance measurements probe insertion reaction kettles；Open all terminal valves, profit
Slowly promoted with constant pressure pump and move on piston, extruding measurement thing sample is to setting pressure, and stable a period of time；Inject high after evacuation
Calm the anger body；Using residual gas in vacuum pumped high pressure low temperature reactor, then gases at high pressure are entered to setting using gas injection infusion
Pressure；Thermosensitive resistance measurement probe is connected with DC power system, simultaneously by temperature sensor, pressure transducer wiring and number
Connect according to acquisition module and connect computer；
3rd step, heat conducting coefficient measuring and heat transfer coefficient
Thing sample to be measured starts after reaching setting state to measure, and is first turned on constant voltage dc source, by becoming on circuit board
The power of resistance control input critesistor, the data acquisition system not magnitude of voltage of critesistor and electricity in the same time simultaneously
The current value on road；The temperature of association reaction kettle, pressure parameter, using temperature damping's data of critesistor, bring heat conduction into respectively
Coefficient, heat transfer coefficient computation model formula (1)-(5), calculate not heat conductivity and the heat transfer system with different spaces in the same time
Number；
4th step, Data Integration is analyzed
The measurement of heat conductivity and heat transfer coefficient can real-time monitoring measure thing sample whole phase-state change process, in conjunction with high pressure
Temperature in low-temp reaction kettle, pressure, gas-liquid flow and flow velocity, heat conductivity and heat transfer coefficient data, finally draw multi phase state
Material different spaces, the Heat Transfer Data of different time.
The invention has the beneficial effects as follows: it is applied to multi phase state high pressure low temperature heat conductivity, the in site measurement of heat transfer coefficient, with
When being capable of real-time monitoring different spaces, heat conductivity and heat transfer coefficient change in different time.In measurement process, critesistor
Caloric value less, can be prevented effectively from heat dissipation capacity on measurement thing sample phase-state change impact.High pressure low temperature reactor inner carrier pair
Measurement thing pattern sample standardization compacting, can unified measurement standard, improve data reference value.In addition, thermistor probe
Partly easily change, be easy to life-time service.
Brief description
Fig. 1 is the in-situ test probe structural representation of the in-situ testing device of the present invention.
Fig. 2 is the in-situ testing device system construction drawing of the present invention.
Fig. 3 is the in-situ testing device reactor probe layout of the present invention.
Fig. 4 is the reactor profile of the in-situ testing device of the present invention.
Fig. 5 is methane hydrate heat conductivity and temperature chart in porous media.
Fig. 6 is methane hydrate catabolic process heat transfer coefficient and temperature variation in porous media.
In figure: 1 critesistor；2 epoxy resin；3 punching stainless steel tubes；4 sealing rings；5 snap joints；6 is pressure
Plastics；7 high pressure sealing heads；8 circuit control panels；9 circuit output mouths；10 bolts；11 temperature, pressure, thermosensitive resistance measurement
Probe general-purpose interface；Cap rock on 12；13 o type sealing rings；14 water filling ports；15 displacement transducers；16 sealing rings；17 lower covers
Layer；18 pistons.
Specific embodiment
Below in conjunction with accompanying drawing and technical scheme, further illustrate the specific embodiment of the present invention.
Fig. 1-4 illustrates a kind of high pressure low temperature heat conductivity, heat transfer coefficient in-situ testing device.This device is important two
It is grouped into.Part I is thermosensitive resistance measurement probe, as shown in figure 1, first cleaning up the wire of critesistor, using exhausted
Edge paint is insulated, and is repeated three times, after test insulating properties is good, the wire of critesistor is passed through punching fine steel tube, is used in combination
Epoxy resin fills fine steel tube, wraps up thermal resistor wire simultaneously, stablizes critesistor, then thermal resistor wire is passed through height
Pressure sealing device, fixes by punching fine steel tube insertion high pressure seal leading portion and with epoxy gluing simultaneously.Finally will lead
Line is connected with the circuit board of thermosensitive resistance measurement probe tip, and various pieces are carried out with fastening inspection.Thermosensitive resistance measurement is visited
Head is connected with high pressure low temperature reactor in snap joint mode, is easy to plug and replacing, constant voltage dc source and critesistor
Circuit board connects, for electric current needed for supply circuit.
Part II is high pressure low temperature reactor, is equipped with piston, is noted to room under reactor using constant pressure pump in the middle of reactor
Enter ethylene glycol, by piston suppress measurement thing sample, be easy to unified measurement standard, in addition reactor top be equipped with temperature sensor and
Pressure transducer, can obtain the three-dimensional Temperature Distribution of determinand sample in reactor.Reactor top air inlet respectively
And gas outlet, for gas, the injection of liquid and discharge.High pressure low temperature reactor is placed in calorstat, using calorstat control
Reactor temperature.The vacuum pump being equipped with is used for the air in abstraction reaction kettle.Whole measuring system is as shown in Figure 2.Wherein anti-
Answer arranged probe positions on kettle as shown in figure 3, all of probe positions are standard fast interface, different measuring probe,
Air inlet/outlet can be with transposition.The profile of reactor is as shown in Figure 4.
Embodiment
In porous media, methane hydrate decomposes is the process that multi phase state coexists under the conditions of high pressure low temperature, companion simultaneously
With there being phase-state change process, conventional traditional method is difficult to its different phase heat conductivity, and catabolic process heat transfer coefficient enters
Row measurement, below for test implementation process of the present invention:
First, open on reactor lid, choose methane hydrate and carry out in-situ preparation in porous media:
1. (particle diameter is 0.4mm, and porosity is 0.36, and density is 2.58g/cm to choose 6kg glass sand3) placing response kettle
In, 1kg deionized water is uniformly mixed with glass sand.Close reactor, insertion temperature sensor, thermistor probe, pressure
Sensor, and connect pipeline.
2. open reactor top terminal valve, into reactor piston, slowly inject ethylene glycol solution using constant flow pump
(low temperature resistant), slow extruded sample, to constant pressure 2mpa.
3. evacuation, then enters quantitative methane gas (127 standard liter), wherein pressure in reactor using gas infusion
It is about 7mpa, close all valves afterwards.
4. utilize air bath to freeze, allow reactor generate methane hydrate under the conditions of 3 DEG C of constant temperature, it is to avoid the life of ice
Become.
5. judge whether hydrate generates using temperature-pressure curve, after hydrate generates, stablize 24 hours.According to known
Porous media porosity, each volume components, consume methane molal quantity, calculate generate methane hydrate quantity, Yi Jijia
The saturation (30%) of alkane hydrate.
6. measure under the conditions of equilibrium temperature (3 DEG C), the heat conductivity of methane hydrate.Before experiment, first some are marked
Quasi- material is measured at ambient temperature, the results show, and experimental error is within 5%, and has preferable experiment weight
Renaturation, as shown in table 1.Constant voltage dc source is first opened, control voltage is 15v, connects circuit during experiment, according to formula (1), will
The resistance of critesistor is transformed to temperature value, is made the difference using bulk temperature in critesistor own temperature and reactor, calculates
δ t, calculates p value according to current value in circuit and critesistor self-resistance value, calculates instantaneous heat conduction system according to formula (2)
Number, wherein kbIt is empirical value with a, respectively 0.0411007 and 0.001938666. calculates thermal conductivity value is
0.739w/km, after measurement process data is as shown in figure 5, connect circuit, measurement result is stable when 50 seconds, has preferably
Stable experiment and repeatability.
Table 1. standard substance thermal conductivity measurement and error analyses
7. calculate the heat transfer coefficient of methane hydrate catabolic process, the phase that the catabolic process of methane hydrate is related to becomes
Change, multi phase state coexists, and there is flow process, effective heat transfer coefficient is measured according to critesistor method.It is first turned on constant voltage DC
Power supply, control voltage is 15v, connects circuit, adopts counterbalance valve to control aerogenesis pressure (2mpa) simultaneously, reduces the pressure in reactor
Power, promotes decomposition of hydrate, and decomposition of hydrate is water and methane gas, and methane gas are passed through in effusion meter inflow gas collecting tank.Root
According to formula 1, the resistance of critesistor is transformed to temperature value, using ensemble average temperature in critesistor own temperature and reactor
Degree makes the difference, and calculates δ t, calculates p value according to current value in circuit and critesistor self-resistance value, according to formula 3,4,5
Calculate heat transfer coefficient in methane hydrate catabolic process.Wherein tfFor bulk temperature average in reactor, kf, β, k, d, α, t are equal
For the experiment parameter of this operating condition of test, respectively 0.578w/km, 3336.3,0.002m, 0.0015m, 0.1323m, 0.004m,
Vs is critesistor its voltage, and v is circuit total voltage, rsFor critesistor transient resistance.The heat transfer coefficient asked is in 80-
150w/m2In the range of k, the heat transfer coefficient of measurement process and temperature as shown in fig. 6, empirical tests experiment value in the reasonable scope, with
When experiment there is preferable stability and repeatability.
Claims (2)
1. the home position testing method of a kind of high pressure low temperature heat conductivity, heat transfer coefficient is it is characterised in that the method is forced down using height
Warm heat conductivity, the in-situ testing device of heat transfer coefficient, described in-situ testing device includes thermosensitive resistance measurement probe and height
Force down warm reactor；Thermosensitive resistance measurement probe is critesistor, high pressure seal and circuit control panel from bottom to top；Temperature-sensitive
The lower end that resistance is popped one's head in thermosensitive resistance measurement, thermosensitive resistance measurement probe mid portion is high pressure seal, critesistor
The cavity on measuring probe top is connected with circuit control panel；Critesistor is inserted directly in high pressure low temperature reactor, the height of centre
Pressure sealing device is connected with high pressure low temperature reactor, and the top of thermosensitive resistance measurement probe is outside high pressure low temperature reactor；
The connecting wire of critesistor is first passed through rustless steel tubule, is then passed through high densification using insulation lacquer coat, connecting wire
Seal apparatus；The rustless steel tubule of epoxy resin perfusion is used for parcel protection connecting wire, is fixed on critesistor stainless simultaneously
The port of steel tubule；The connecting wire of critesistor is extruded using pressure-resistant plastic, for leading to connection inside high pressure seal
Line carries out high pressure sealing；Rustless steel tubule and high pressure seal are fixed using adhering with epoxy resin, on rustless steel tubule uniformly
Punching；
Wherein thermosensitive resistance measurement probe is connected with high pressure low temperature reactor using snap joint, and circuit control panel has change resistance
And circuit protecting element, become resistance and be used for adjusting current value in circuit, circuit protecting element is used for preventing transient current in circuit
Excessive, protect critesistor and whole circuit；The top circuit delivery outlet of thermosensitive resistance measurement probe and outside constant voltage DC
Power control system data acquisition system connects, and constant voltage dc source is used for powering to critesistor, and being capable of control circuit
Middle curent change；Current value in the resistance value of data acquisition system critesistor and circuit；
High pressure low temperature reactor has two Room, is connected by piston between two Room, and measurement thing sample is directly placed into high pressure low temperature reactor
In upper room；Piston is promoted in the water filling of high pressure low temperature reactor lower end by constant pressure pump, for suppressing the measurement thing sample of upper interior, profit
With constant pressure, measurement thing sample is standardized suppressing；High pressure low temperature reactor top is reserved with temperature sensor interface, pressure
Force transducer interface, thermosensitive resistance measurement probe interface and air intake-exhaust interface；Above-mentioned interface is all using snap joint interface, position
Put all interchangeable；Displacement transducer is located at high pressure low temperature reactor lower cover center, can detect piston movement displacement and determine
The volume of high pressure low temperature reactor two Room；Wherein gas and liquid are inputted to high pressure low temperature reactor using constant flow pump, air accumulator
In, gases at high pressure, under the control of counterbalance valve, are discharged from air vent with the pressure setting, and the gas-liquid discharging into discharge passes through effusion meter
Measure its flow velocity and integrated flow；Temperature sensor, pressure transducer and thermosensitive resistance measurement probe synchronization are surveyed online
Amount, and by unified for data output, carry out heat conductivity and the Local Heat Transfer Coefficient of computation and measurement thing sample using computation model；
In-situ test is carried out using above-mentioned in-situ testing device, step is as follows:
The first step, is corrected to thermosensitive resistance measurement model parameter
Using standard substance according to the characteristic of testing medium respectively to β, α, t, the k in formula (1)-(5)bIt is corrected with d, school
Just carrying out survey calculation afterwards；
Second step, filling measurement thing sample makes standard testing sample
Open lid on high pressure low temperature reactor, insert solid to be measured and liquid, after covering bonnet, insertion temperature, pressure, temperature-sensitive electricity
Resistance measuring probe；The diverse location of multiple thermosensitive resistance measurements probe insertion reaction kettles；Open all terminal valves, using perseverance
Press pump slowly promotes and moves on piston, and extruding measurement thing sample is to setting pressure, and stable a period of time；High pressure gas are injected after evacuation
Body；Using residual gas in vacuum pumped high pressure low temperature reactor, then gases at high pressure are entered to setting pressure using gas injection infusion；
Thermosensitive resistance measurement probe is connected with DC power system, temperature sensor, pressure transducer wiring and data is adopted simultaneously
Collection module connects and connects computer；
3rd step, heat conducting coefficient measuring and heat transfer coefficient
Thing sample to be measured starts after reaching setting state to measure, and is first turned on constant voltage dc source, by becoming resistance on circuit board
The power of control input critesistor, the data acquisition system not magnitude of voltage of critesistor and circuit in the same time simultaneously
Current value；The temperature of association reaction kettle, pressure parameter, using temperature damping's data of critesistor, bring into respectively heat conductivity,
Heat transfer coefficient computation model formula (1)-(5), try to achieve not heat conductivity and the heat transfer coefficient with different spaces in the same time；
4th step, Data Integration is analyzed
The measurement of heat conductivity and heat transfer coefficient can real-time monitoring measure thing sample whole phase-state change process, in conjunction with high pressure low temperature
Temperature in reactor, pressure, gas-liquid flow and flow velocity, heat conductivity and heat transfer coefficient data, finally draw multi phase state material
Different spaces, the Heat Transfer Data of different time.
2. home position testing method according to claim 1 is it is characterised in that the aperture uniformly punched on rustless steel tubule is
1mm, pitch-row is 15mm.
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| CN201410617225.1A CN104458798B (en) | 2014-11-04 | 2014-11-04 | In-situ test method for high-pressure low-temperature heat conductivity coefficients and heat transfer coefficients |
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