CN103760190A - Method and device for measuring heat conduction coefficient of natural gas hydrate in porous medium - Google Patents
Method and device for measuring heat conduction coefficient of natural gas hydrate in porous medium Download PDFInfo
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Abstract
The invention discloses a method and a device for measuring the heat conduction coefficient of a natural gas hydrate in a porous medium. The device provided by the invention comprises a pressure stabilizing gas-liquid supplying module, a temperature control module, a heat conduction coefficient measuring module and a data collecting module; the hydrate generation and the heat conduction coefficient determining are carried out in a high-pressure reaction kettle. The axis of the reaction kettle is provided with a resistance wire which can provide stable power so as to continuously heat up a porous medium containing the hydrate; three thermoelectric couples are distributed additionally on the cross section, in which the central point of the resistance wire is positioned, of a kettle body, and are used for analyzing the stable-station transmission characteristics of heat along the cross section in heating. According to the method and the device, a stable-station measurement technique is combined, and can be used for measuring the effective heat conduction coefficient of the porous medium containing the hydrate, comprehensively studying the saturability degrees of different hydrates, heat conduction coefficient models under different temperatures and pressures and different deposition particles, and provides a theory basis for practical exploiting of the natural gas hydrates.
Description
Technical field
The present invention relates to a kind of method and apparatus of measuring gas hydrate coefficient of heat conductivity in porous medium.
Background technology
Gas hydrate, claim again combustible ice, are the natural G&W white crystalline compound that (temperature, pressure, gas saturation, salinity etc.) form under certain condition.Gas hydrate are as a kind of novel potential energy source, and reserves are huge, be considered to have most application prospect can petroleum replacing etc. one of the new forms of energy of fossil energy, and extensively found to be present in marine bottom sediment and land permafrost region.
The exploitation commercial value on the spot of gas hydrate is affected by many geologic conditions, and wherein formation thermal conductivity is one of key factor affecting decomposition of hydrate and gas production rate.Coefficient of heat conductivity has reacted the ability that porous medium heat transmits, and affects in mineral reserve heat to the conduction velocity of hydrate formation region, thereby is retraining decomposition of hydrate gas producing efficiency in recovery process.Numerical simulation result shows, the porous medium that coefficient of heat conductivity is lower, and decomposition of hydrate speed is more limited, causes its extraction value undesirable.In addition, the effective thermal conductivity of porous medium is a function relevant to multi-phase multi-component, and along with the change of the gentle liquid hold-up of decomposition of hydrate, formation thermal conductivity changes thereupon.The principal element that affects formation thermal conductivity comprises factor of porosity, fluid-phase saturation degree, solid phase saturation degree and each phase coefficient of heat conductivity.In solid phase owing to there being the phase transition process such as the decomposition of hydrate and generation, make containing measurement and the research of hydrate Heat Conduction in Porous Media coefficient more complicated, the current research about hydrate formation coefficient of heat conductivity characteristic is also in the theoretical analysis stage, lack enough experimental data support and checking, therefore containing the heat-transfer mechanism of hydrate porous medium, not also very perfect, to actual hydrate exploitation, still can not provide reliable theoretical direction.
The experimental provision of routine measurement material coefficient of heat conductivity and instrument are many to be moved under normal temperature and pressure conditions, and for containing hydrate porous medium, owing to being subject to the impact (low temperature, high pressure) of the stable condition of hydrate own, be difficult to use conventional thermal conductivity measurement instrument to be measured, need the special experimental provision of development.Such experimental provision need meet following requirement: hydrate easily generates, measuring accuracy is high, experimental implementation is simple etc.
Summary of the invention
The object of the present invention is to provide the method and apparatus of gas hydrate coefficient of heat conductivity in a kind of porous medium, the method and device can be for measuring containing hydrate effective thermal conductivity of porous, coefficient of heat conductivity model under the different hydrate concentrations of synthetic study, different temperatures and pressure and porous medium particle, for actual exploitation of gas hydrates provides theoretical foundation.It is simple to operate, measures accurately, and safety is controlled.
For realizing above object, the present invention has taked following technical scheme: a kind of device of measuring gas hydrate coefficient of heat conductivity in porous medium, comprise for regulation and control autoclave gas-liquid content, generate the voltage stabilizing gas-liquid supplying module of required arbitrary even hydrate concentration system, be used to device that the temperature control modules of steady temperature is provided, autoclave is placed in water bath with thermostatic control, along described autoclave axle center, place is provided with resistance wire, resistance wire is connected with extraneous stabilized voltage supply, on the autoclave cross section at resistance wire central point place, be distributed with three thermopairs, between thermopair each other 120 degree angles, thermocouple probe radially stretches into the inner diverse location of autoclave, thermocouple probe points to resistance wire, also comprise the thermal conductivity measurement module being connected with resistance wire, and for gathering autoclave, the data acquisition module of thermopair and the pipeline parameter that is connected with autoclave, described thermal conductivity measurement module is connected with data acquisition module, on the pipeline being connected with autoclave, be provided with gas-liquid premixed device, and be provided with high speed agitator in gas-liquid premixed device, described Heat Conduction in Porous Media coefficient k (W/m/K) computing formula is
wherein bath temperature is T
0, unit is ℃, thermopair equilibrium temperature T, and unit is ℃, autoclave internal diameter R, unit is mm, and thermocouple probe and resistance wire distance are r, and unit is mm, resistance wire unit length heating power q, unit is W/m.
Heat stable state transmission characteristic from inside to outside when described three thermopairs are used for analyzing Resistant heating, gas-liquid premixed device and high speed agitator have outstanding role for measurement result accuracy.
The inner active volume V of described autoclave, inside diameter D and length H will strictly control, excessive gas-liquid layering or the bubble coalescence of easily causing of V, D and H, the too small instruments such as internal resistance silk, thermopair that may make itself increase the adverse effect of measurement result, therefore the selection range of V is at 0.4～6.3L, the selection range of D is 50～100mm, H/D >=8.
Described resistance wire sleeve pipe external diameter r
2/ D<4%, resistance wire length h/H>=99%.Resistance wire provides stable heating power by voltage stabilizing for thermoelectric generator.Resistance wire is encapsulated by stainless steel sleeve pipe, does not contact with water with reactor interior media.For guarantee and improve the measuring accuracy of coefficient of heat conductivity as far as possible, resistive heater should meet line heat source requirement, and heat is substantially radially transmitted, and reduces the thermal loss at reactor import and export two ends.
A kind of method of measuring gas hydrate coefficient of heat conductivity in porous medium, measuring method is the radial heat flows method based on steady heat conduction principle, the autoclave level of filling in porous medium is fixed on support, starts water bath with thermostatic control and a steady temperature is set, reactor is vacuumized; Comprise the steps:
Step 1: open gas-liquid premixed device imported valve, injected the pure methane gas of specified pressure by high-pressure air source to gas-liquid premixed device, then close gas-liquid premixed device terminal valve standing half an hour;
Step 2: open the valve between liquid charge pump and gas-liquid premixed device, injected the solution of predetermined quality by liquid charge pump to gas-liquid premixed device;
Step 3: close liquid charge pump outlet valve, open high speed agitator, open the outlet valve between gas-liquid premixed device and reactor, inject the solution after stirring to autoclave;
Step 4: after autoclave and the pressure equilibrium of gas-liquid premixed device, valve-off, stops stirring; After temperature, pressure is stable, according to equation of state of real gas and mass balance equation, calculate the gas-liquid amount of injecting autoclave;
Step 5: close autoclave terminal valve, again reduce water bath with thermostatic control temperature to hydrate and generate temperature, hydrate starts to generate;
Step 6: treat that autoclave pressure decreased is to predetermined value, open stabilized voltage supply, resistance wire starts heating, utilize data acquisition system (DAS) to record temperature temporal evolution curve and the Resistant heating power of thermopair in still, in question response still after the temperature stabilization of three thermopairs, system, in steady heat transfer state, can be calculated different measuring points place containing hydrate effective thermal conductivity of porous according to steady heat conduction principle formula, and described Heat Conduction in Porous Media coefficient k (W/m/K) computing formula is
wherein bath temperature is T0, and unit is ℃, thermopair equilibrium temperature T, and unit is ℃, autoclave (1) internal diameter R, unit is mm, thermopair (3) probe is r with resistance wire (2) distance, unit is mm, resistance wire (2) unit length heating power q, and unit is W/m.
Innovation of the present invention is that particular content comprises following several respects by radially steady heat conduction application of principle measurement of gas hydrate coefficient of heat conductivity in porous medium under the yardstick of laboratory:
(1) described voltage stabilizing gas-liquid supplying module, for regulation and control autoclave gas-liquid content, generates required arbitrary even hydrate concentration system; Place, described autoclave axle center is a resistive heater, and resistance wire is by stabilized voltage supply continuous heating, and heating power is controlled; Three the Pt100 thermopairs that distribute on kettle cross section, resistance wire central point place, 120o angle each other between thermopair, thermocouple probe radially stretches into the inner diverse location of kettle, probe external diameter r
1<3mm, while heating for analyzing, heat is along the stable state transmission characteristic in cross section; Thermocouple probe points to resistive heater; Utilize these three electric thermo-couple temperature variation characteristics and the steady heat conduction principle can calculation medium effective thermal conductivity.
(2) whether hydrate distribution is evenly the whether accurate prerequisite of gas hydrate thermal conductivity measurement in porous medium, and before its determinative has hydrate to generate, whether gas, liquid mix, and whether hydrate is present within the scope of suitable physical size.This method and device arrange gas-liquid premixed device and provide well-mixed gas-liquid solution to reactor, can greatly improve the homogeneity that hydrate distributes in reactor.Described gas-liquid premixed device is placed in reactor inflow point, and its inside is provided with a pressure transducer and a Pt100 thermopair, separately has a high speed agitator for uniform mixing gas mixture and solution, so that mixed uniformly gas-liquid solution to be provided to reactor.By temperature, pressure before and after gas-liquid premixed device and reactor gas injection fluid injection, change, utilize equation of state of real gas and mass balance equation can accurate Calculation to inject gas and the solution amount of reactor.In reactor, there is a pressure transducer, for surveying hydrate formation system pressure variation characteristic.Reactor is imported and exported and is provided with compression filtration unit, prevents that solid particle from entering pipeline.Reactor exit is provided with back pressure device, for maintaining kettle top hole pressure.Outlet fluid is discharged through check valve.Reactor and gas-liquid premixed device are all placed in water bath with thermostatic control.
(3) for meeting the radially steady heat conduction principle that in porous medium, gas hydrate thermal conductivity measurement adopts, the inner active volume V of reactor, inside diameter D and length H will strictly control, excessive gas-liquid layering or the bubble coalescence of easily causing of V, D and H, the too small instruments such as internal resistance silk, thermopair that may make itself increase the adverse effect of measurement result, therefore the selection range of V is at 0.4～6.3L, the selection range of D is 50～100mm, H/D >=8.Described resistive heater is encapsulated by stainless steel sleeve pipe, and sleeve pipe external diameter meets r
2/ D<4%, resistance wire length h/H>=99%, to reach line heat source requirement, meets heat in heating process and substantially radially transmits, and reduces the heat waste at reactor import and export two ends.
(4) described autoclave is arranged in water bath with thermostatic control, and temperature controlling range is-15～30 ℃, and control accuracy is ± 0.1 ℃, and withstand voltage scope is 0～50MPa.Described resistance wire is encapsulated by stainless steel sleeve pipe, does not contact with reactor interior media or water-bath, and withstand voltage scope is 0～50MPa, and has good strength, not yielding.For guaranteeing measuring accuracy, described thermocouple temperature measurement precision is ± 0.1 ℃.
(5) described radial heat flows method is a kind of technology of measuring based on steady heat conduction, when cylinder system is during in steady heat transfer, it is stable that kettle internal temperature space distribution can keep, and can determine the coefficient of heat conductivity of medium according to the temperature variation of three thermopairs and present position thereof.Its required measurement parameter comprises: bath temperature T
0(℃), thermopair equilibrium temperature T(℃), kettle internal diameter R(mm), thermocouple probe and resistance wire are apart from r(mm) and, resistance wire unit length heating power q(W/m), medium heat conduction coefficient formulas is
To sum up, tool of the present invention has the following advantages:
1, can generate the even saturation degree system of different hydrates under different porous mediums;
2, resistance wire, as a line heat source to system heat supply, can make the inner porous medium of kettle form a stable temperature field, and can directly under condition of high voltage, to porous medium, heat, and handling safety is simple;
3, the radial heat flows method based on steady heat conduction principle, can effectively measure containing hydrate Heat Conduction in Porous Media coefficient, and measuring accuracy is high.
Accompanying drawing explanation
Fig. 1 is apparatus of the present invention structural representation;
Fig. 2 is the autoclave A-A view in Fig. 1.
Embodiment
Below in conjunction with the drawings and specific embodiments, content of the present invention is described in further details.
Embodiment
Refer to shown in Fig. 1, a kind of device of measuring gas hydrate coefficient of heat conductivity in porous medium, comprise for regulation and control autoclave 1 gas-liquid content, generate the voltage stabilizing gas-liquid supplying module of required arbitrary even hydrate concentration system, be used to device that the temperature control modules of steady temperature is provided, temperature control modules generates required low temperature environment for controlling hydrate, autoclave 1 is placed in water bath with thermostatic control 4, along described autoclave, 1 place, axle center is provided with resistance wire 2, resistance wire 2 is connected with extraneous stabilized voltage supply 7, its core is the autoclave 1 in thermal conductivity measurement module, voltage stabilizing gas-liquid supplying module comprises high-pressure air source 8, high-pressure filling pump 9 and a small-sized gas-liquid premixed device 5, gas-liquid premixed device 5 is between autoclave 1 and high-pressure air source 8, for buffer gas and solution, Accurate Calibration injects kettle gas-liquid amount, and provide mixed uniformly gas-liquid solution, in whole device, be also provided with reduction valve 10, safety valve 11, pressure transducer 12, the parts of check valve 13 measurement parameters such as grade, on autoclave 1 cross section at resistance wire 2 central point places, be distributed with three thermopairs 3, between thermopair 3 each other 120 degree angles, thermopair 3 is popped one's head in and is radially stretched into the inner diverse location of autoclave 1, thermopair 3 probes point to resistance wire 2, also comprise the thermal conductivity measurement module being connected with resistance wire 2, and for gathering autoclave 1, the data acquisition module of thermopair 3 and the pipeline parameter that is connected with autoclave 1, thermal conductivity measurement module is connected with data acquisition module, on the pipeline being connected with autoclave 1, be provided with gas-liquid premixed device 5, and in gas-liquid premixed device 5, be provided with high speed agitator 6, Heat Conduction in Porous Media coefficient k (W/m/K) computing formula is
wherein bath temperature is T
0, unit is ℃, thermopair equilibrium temperature T, and unit is ℃, autoclave 1 internal diameter R, unit is mm, and thermopair 3 probes are r with resistance wire 2 distances, and unit is mm, resistance wire 2 unit length heating power q, unit is W/m.
The pass of the inner active volume V of autoclave 1, inside diameter D and length H is: the selection range of V is at 0.4～6.3L, and the selection range of D is 50～100mm, H/D >=8.Resistance wire 2 sleeve pipe external diameter r
2/ D<4%, resistance wire 2 length h/H>=99%.
In use, concrete operation step is as follows for apparatus of the present invention:
1), the autoclave level of filling in porous medium is fixed on support, starts water bath with thermostatic control and also a steady temperature is set, reactor is vacuumized;
2), open gas-liquid premixed device imported valve, by high-pressure air source, to gas-liquid premixed device, injected the pure methane gas of specified pressure, then close gas-liquid premixed device terminal valve standing half an hour;
3), open the valve between liquid charge pump and gas-liquid premixed device, the solution by liquid charge pump to gas-liquid premixed device injection certain mass;
4), close liquid charge pump outlet valve, open high speed agitator, open the outlet valve between gas-liquid premixed device and reactor, to reactor inject stir after solution;
5), after question response still and the pressure equilibrium of gas-liquid premixed device, valve-off, stops stirring; After temperature, pressure is stable, according to equation of state of real gas and mass balance equation, calculate the gas-liquid amount of injecting reactor;
6), off-response still terminal valve, again reduce water bath with thermostatic control temperature to hydrate and generate temperature, hydrate start generate;
7), question response still pressure decreased is to predetermined value, open stabilized voltage supply, resistance wire starts heating, utilize data acquisition system (DAS) to record temperature temporal evolution curve and the Resistant heating power of thermopair in still, in question response still after the temperature stabilization of three thermopairs, system, in steady heat transfer state, can be calculated different measuring points place containing hydrate effective thermal conductivity of porous according to steady heat conduction principle formula.
Above-listed detailed description is for the illustrating of possible embodiments of the present invention, and this embodiment is not in order to limit the scope of the claims of the present invention, and the equivalence that all the present invention of disengaging do is implemented or changed, and all should be contained in the scope of the claims of this case.
Claims (4)
1. measure the device of gas hydrate coefficient of heat conductivity in porous medium for one kind, comprise for regulation and control autoclave (1) gas-liquid content, generate the voltage stabilizing gas-liquid supplying module of required arbitrary even hydrate concentration system, be used to device that the temperature control modules of steady temperature is provided, autoclave (1) is placed in water bath with thermostatic control (4), along described autoclave (1), place, axle center is provided with resistance wire (2), and resistance wire (2) is connected with extraneous stabilized voltage supply;
It is characterized in that: on autoclave (1) cross section at resistance wire (2) central point place, be distributed with three thermopairs (3), between thermopair (3) each other 120 degree angles, thermopair (3) probe radially stretches into the inner diverse location of autoclave (1), thermopair (3) probe points to resistance wire (2), also comprise the thermal conductivity measurement module being connected with resistance wire (2), and for gathering autoclave (1), the data acquisition module of thermopair (3) and the pipeline parameter that is connected with autoclave (1), described thermal conductivity measurement module is connected with data acquisition module, on the pipeline being connected with autoclave (1), be provided with gas-liquid premixed device (5), and in gas-liquid premixed device (5), be provided with high speed agitator (6),
Described Heat Conduction in Porous Media coefficient k (W/m/K) computing formula is
wherein bath temperature is T
0, unit is ℃, thermopair equilibrium temperature T, and unit is ℃, autoclave (1) internal diameter R, unit is mm, and thermopair (3) probe is r with resistance wire (2) distance, and unit is mm, resistance wire (2) unit length heating power q, unit is W/m.
2. a kind of device of measuring gas hydrate coefficient of heat conductivity in porous medium as claimed in claim 1, it is characterized in that: the pass of the inner active volume V of described autoclave (1), inside diameter D and length H is: the selection range of V is at 0.4～6.3L, the selection range of D is 50～100mm, H/D >=8.
3. a kind of device of measuring gas hydrate coefficient of heat conductivity in porous medium as claimed in claim 2, is characterized in that: described resistance wire (2) sleeve pipe external diameter r
2/ D<4%, resistance wire (2) length h/H>=99%.
4. measure a method for gas hydrate coefficient of heat conductivity in porous medium, the autoclave level of filling in porous medium is fixed on support, start water bath with thermostatic control and a steady temperature is set, reactor is vacuumized; It is characterized in that, comprise the steps:
Step 1: open gas-liquid premixed device imported valve, injected the pure methane gas of specified pressure by high-pressure air source to gas-liquid premixed device, then close gas-liquid premixed device terminal valve standing half an hour;
Step 2: open the valve between liquid charge pump and gas-liquid premixed device, injected the solution of predetermined quality by liquid charge pump to gas-liquid premixed device;
Step 3: close liquid charge pump outlet valve, open high speed agitator, open the outlet valve between gas-liquid premixed device and reactor, inject the solution after stirring to autoclave;
Step 4: after autoclave and the pressure equilibrium of gas-liquid premixed device, valve-off, stops stirring; After temperature, pressure is stable, according to equation of state of real gas and mass balance equation, calculate the gas-liquid amount of injecting autoclave;
Step 5: close autoclave terminal valve, again reduce water bath with thermostatic control temperature to hydrate and generate temperature, hydrate starts to generate;
Step 6: treat that autoclave pressure decreased is to predetermined value, open stabilized voltage supply, resistance wire starts heating, utilize data acquisition system (DAS) to record temperature temporal evolution curve and the Resistant heating power of thermopair in still, in question response still after the temperature stabilization of three thermopairs, system, in steady heat transfer state, can be calculated different measuring points place containing hydrate effective thermal conductivity of porous according to steady heat conduction principle formula, and described Heat Conduction in Porous Media coefficient k (W/m/K) computing formula is
wherein bath temperature is T
0, unit is ℃, thermopair equilibrium temperature T, and unit is ℃, autoclave (1) internal diameter R, unit is mm, and thermopair (3) probe is r with resistance wire (2) distance, and unit is mm, resistance wire (2) unit length heating power q, unit is W/m.
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| CN104316558A (en) * | 2014-10-15 | 2015-01-28 | 中国海洋石油总公司 | Device and method for measuring heat conductivity of sediments of gas hydrates |
| CN104359747A (en) * | 2014-10-27 | 2015-02-18 | 中国地质调查局油气资源调查中心 | Device and method for preparing and measuring frozen soil sample |
| CN104849310A (en) * | 2015-06-02 | 2015-08-19 | 哈尔滨工业大学 | Experimental device for measuring high-temperature heat exchange between porous material in tube and airflow |
| CN105842275A (en) * | 2016-03-28 | 2016-08-10 | 河南理工大学 | Steam driven coal gas desorption heat conduction test method |
| CN105928975A (en) * | 2016-05-31 | 2016-09-07 | 西安交通大学 | Variable-atmosphere pressure heat conductivity coefficient testing device based on transient plane source method |
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| CN104359747A (en) * | 2014-10-27 | 2015-02-18 | 中国地质调查局油气资源调查中心 | Device and method for preparing and measuring frozen soil sample |
| CN104849310A (en) * | 2015-06-02 | 2015-08-19 | 哈尔滨工业大学 | Experimental device for measuring high-temperature heat exchange between porous material in tube and airflow |
| CN105842275A (en) * | 2016-03-28 | 2016-08-10 | 河南理工大学 | Steam driven coal gas desorption heat conduction test method |
| CN105842275B (en) * | 2016-03-28 | 2018-07-03 | 河南理工大学 | A kind of test method of steam drive coal gas desorption heat transfer |
| CN105928975A (en) * | 2016-05-31 | 2016-09-07 | 西安交通大学 | Variable-atmosphere pressure heat conductivity coefficient testing device based on transient plane source method |
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