CN101055276A - Natural gas hydrate phase balance emulation experiment device - Google Patents
Natural gas hydrate phase balance emulation experiment device Download PDFInfo
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- CN101055276A CN101055276A CNA2007100269427A CN200710026942A CN101055276A CN 101055276 A CN101055276 A CN 101055276A CN A2007100269427 A CNA2007100269427 A CN A2007100269427A CN 200710026942 A CN200710026942 A CN 200710026942A CN 101055276 A CN101055276 A CN 101055276A
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Abstract
The invention discloses a natural gas hydrate phase equilibrium simulation experiment device, which mainly includes: a phase equilibrium simulation unit, a pressure control unit, a temperature control unit, a stable pressure liquid supply unit, a stable pressure gas supply unit, a measuring unit, and a data collection unit. The hydrate phase equilibrium simulation experiment device can carry hydrate of different gas phase equilibrium experiment, and can detect hydrate phase equilibrium condition under existence of different chemical agents. By weeny change, the device can also carry phase equilibrium experiment in porous medium, and detect phase equilibrium condition of hydrate in porous medium with different pore diameter. Advantages of the invention are: simple operation, accurate measurement, changeable reaction kettle volume, high accuracy control for temperature and pressure.
Description
[technical field]
The present invention relates to a kind of natural gas hydrate phase balance emulation experiment device.
[background technology]
Gas hydrate is that micro-molecular gas is (as CH
4, C
2H
6, C
3H
8, C
4H
10Deng homolog and CO
2, N
2, H
2S etc. often are called guest molecule) a kind of non-stoichiometric, the cage shape crystalline solid (Clathrate) that under uniform temperature and pressure, generate with water.It meets fire is incendivity, is commonly called as " combustible ice ", and its profile such as ice and snow shape are white in color usually.Its molecular formula can be used M.nH
2O represents that M represents the gas molecule in the hydrate, and n is hydration number (water molecule number just).The gas hydrate structure that has been found that now has 4 kinds: I type, II type, H type and a kind of novel hydrate (being generated by biomolecule and hydrone).
Gas hydrate extensively are distributed in the deepwater environment of bump pad, continental platform, polar region and ocean and some interior lakes of area, slope, activity and the passive continental margin on continent, island at nature.Under the status of criterion, the gas hydrate of one unit volume decompose the methane gas that can produce 164 unit volumes at most, it is predicted that the reserves of global gas hydrate are twices of other fossil fuel summations, thereby gas hydrate are a kind of important potential following resources.
Gas hydrate are, non-stoichiometric, cage modle crystalline compounds ice by the class of water and gas composition under certain condition (salinity of suitable temperature, pressure, gas saturation, water, pH value etc.).The generative process of gas hydrate, actual is the process that a hydrate-solution-gas three-phase equilibrium changes, the factor that any energy influence balances each other can both influence the generation/decomposition of hydrate.The research of hydrate phase balance is the basis of gas hydrate study, for the development and use of gas hydrate provide the basic physical chemical parameters.And to carry out the phase balance emulation experiment of gas hydrate, and the data precision, condition is controlled, and visual analogue experiment installation is indispensable.
In fact the experimental study of hydrate phase balance is exactly to measure its balance formation condition, the i.e. profile of equilibrium of temperature and pressure.Along with the appearance of high pressure resistant and material transparent and the development of related experiment determination techniques, the measuring device of hydrate and experimental technique are also in continuous improvement, and the researcher of various countries has carried out the mensuration of the hydrate phase balance condition of a large amount of different systems.For pure water compound many that research carried out that balance each other, then less relatively for the phase equilibrium experiment in the porous medium, Sloan, D. wait and set up an experimental provision that is used for measuring the rock hydrate phase balance condition, reactor is the stainless steel right cylinder, laboratory sample can be placed in the centre, and the entire reaction still is placed in the water-bath.Two thermopairs are fixed on and are used for gathering the experiment variation of temperature on the laboratory sample, and another thermopair is positioned over the temperature variation that is used to gather environment in the water-bath.The rock sample diameter 3.8cm of experiment, long 8.9cm, average pore radius are 550A, this pore radius is selectable minimum value, can produce maximum influence to balancing each other of hydrate.Also carried out the experiment in artificial ceramics sample, it has identical pore size, and pore radius is 5360A.Also carried out other several groups experiments simultaneously, used the sandstone of different aperture size, the average pore radius at 620A between the 84460A.BP Engineering Bureau has set up the higher experimental system of a cover precision and has been used for studying the inhibiting effect that hydrate is generated at natural sediment chemical agent, and the maximum pressure that reactor can bear is 41.4MPa, and the centre is a movably sample cell.The precision of temperature sensor is ± 0.01k, the precision of pressure transducer 4 is ± 0.008MPa, the temperature controlling range of reactor is 253-373k, temperature fluctuation has been measured methane for ± 0.02k., carbon dioxide and mixed gas thereof the phase balance condition in the porous medium in different apertures, and measured the phase balance condition of the methane hydrate that contains methanol system.Some other researcher has also measured the phase balance condition of some other system in porous medium.
Comprehensive above present Research, mainly there are following problems in the research of hydrate phase balance: more existing experimental provisions generally can only be done the phase equilibrium experiment of pure water compound or porous medium; The system that lacks effective controlled pressure.
[summary of the invention]
The object of the present invention is to provide a kind of phase balance emulation experiment device, be applied to the natural gas hydrate phase balance emulation research of different systems, and the mensuration of natural gas hydrate phase balance emulation in the porous medium.
The technical scheme that solves the foregoing invention purpose is as follows:
Natural gas hydrate phase balance emulation experiment device mainly comprises: the analogue unit that balances each other, pressure control unit, temperature control unit, voltage stabilizing liquid-supply unit, gas supply under constant pressure unit, metering units, data acquisition unit seven major parts.
The described analogue unit that balances each other comprises high pressure resistant reactor, this reactor top has the adjustable speed electromagnetic mixing apparatus, can the gas-liquid in the reactor be stirred carrying out pure water hydrate phase balance laboratory, accelerate hydrate and generate and the speed of decomposing, the bottom of this reactor is provided with piston mobile.
Described high pressure resistant reactor also can adopt following structure, the bottom of this reactor is provided with piston mobile, fill up porous medium in the reactor, adopt constant-flux pump to inject the volume that distilled water can change reactor to piston base, be used for the hydrate phase balance experiment of variable volume, when hydrate phase balance was tested in carrying out porous medium, piston mobile can be used for compressing the porous medium in the reactor.
Described voltage stabilizing liquid-supply unit is made up of electronic balance, constant-flux pump, intermediate receptacle group, electronic balance is used for accurately measuring the quality of injecting with the solution that flows out reactor, when being used to annotate chemical agent, the intermediate receptacle group accurately measures the chemical agent rate of injection, adopt the intermediate receptacle group simultaneously, can avoid the damage of chemical agent constant-flux pump.
Described pressure control unit mainly is made up of pressure control valve, PID pressure controller and gas-holder.By the folding of pressure controller controlled pressure operation valve, in reactor, inject or release gas, can accurately control the pressure in the reactor.
Phase balance emulation experiment device is the general observation that adopts when carrying out the phase equilibrium experiment of pure water compound, at first in reactor, inject the aqueous solution of certain density chemical agent, the gas that reinjects is to certain pressure, set the temperature of water-bath, behind temperature stabilization, begin to stir, a certain amount of hydrate is formed in reactor.Keep a parameter (pressure or temperature) constant, make decomposition of hydrate by reducing pressure or rising temperature then.In reactor, only there is the hydrate crystal of minute quantity to exist, at this moment keep the parameter (temperature, pressure) of the hydrate in the reactor constant, if can there be 3-4h in the hydrate in the reactor, then keep temperature-resistant in the reactor, emit portion gas with the excess pressure operation valve, make pressure reduce 0.05Mpa, if the hydrate in the reactor dissolves fully, then the pressure in the reactor, temperature can be regarded the equilibrium of this system as.
When the hydrate phase balance in carrying out porous medium is tested, at first in reactor, fill up sand, and adopt piston to compress sand grains, make the porous medium in the reactor reach certain porosity.Annotate the chemical agent aqueous solution then in the reactor, determine that it is saturated, injecting gas reaches certain pressure then.Begin cooling generation hydrate, after a large amount of generations of hydrate, heat up and decompose, what the speed of intensification will be enough is slow, is 0.5K/5-24h, makes each step all reach equilibrium state, adopts the picture method to determine balancing each other a little of hydrate then.
Hydrate phase balance emulation experiment device of the present invention can carry out the hydrate phase balance experiment of different component gas, and can carry out the chemical agent existence mensuration of hydrate phase balance down.Also can carry out the hydrate phase balance experiment of porous medium in depositing, the phase balance condition of hydrate in the porous medium of different aperture diameter is measured.Device of the present invention is easy and simple to handle in addition, measures accurately, and reactor volume is variable, can realize the advantages such as High Accuracy Control of temperature, pressure.
[description of drawings]
Fig. 1 is the experimental system schematic flow sheet of hydrate phase balance emulation experiment device of the present invention;
Fig. 2 is the reactor structural representation that hydrate phase balance emulation experiment device of the present invention is used for the experiment of pure water hydrate phase balance;
Fig. 3 is the reactor structural representation that hydrate phase balance emulation experiment device of the present invention is used for the experiment of porous medium hydrate phase balance;
1, reactor, 2, gas-holder, 3, pressure control valve, 4, pressure transducer, 5, PID pressure controller, 6, temperature sensor, 7, water bath with thermostatic control, 8, gas cylinder, 9, reduction valve, 10, stop valve, 11, retaining valve, 12, atmospheric valve, 13, balance, 14, constant-flux pump, 15, intermediate receptacle, 16, balance, 17, data acquisition unit, 18, piston, 19, stirring apparatus, 20, kettle cover.
[embodiment]
Below in conjunction with accompanying drawing the concrete performance of the present invention is done detailed description:
As shown in Figure 1, phase balance emulation experiment device of the present invention mainly comprises: the analogue unit that balances each other, pressure control unit, temperature control unit, voltage stabilizing liquid-supply unit, gas supply under constant pressure unit, metering units, data acquisition unit seven major parts.
The described analogue unit main body that balances each other is high pressure resistant reactor 1, pressure-bearing 20Mpa.In the experiment of pure water compound, be piston mobile 18 in the bottom of reactor, reactor top has electric mixing device 19, can the gas-liquid in the reactor be stirred, and accelerates hydrate and generates and the speed of decomposing.Stirring apparatus is driven by stepper motor, can adjust stirring rate.When hydrate phase balance is tested in carrying out porous medium, fill up porous medium in the reactor, do not need stirring apparatus this moment, changes the kettle cover 20 of not being with stirring apparatus and get final product.In the bottom of reactor is piston mobile 18, is used for the porous medium that changes the volume of reactor and compress reactor.During use, change the reactor volume to the piston base water filling by constant-flux pump 14.
Voltage stabilizing liquid-supply unit assembly comprises: balance 13, constant-flux pump 14, intermediate receptacle group 15.The intermediate receptacle group is when experimentation need add chemical agent, and a kind of indirect container of avoiding chemical agent that the damage of constant-flux pump is used also can be used for the chemical agent amount that delicate metering injects simultaneously.
The gas supply under constant pressure unit block comprises: gas cylinder 8, reduction valve 9, stop valve 10, retaining valve 11, atmospheric valve 12.
Pressure control unit is mainly by pressure control valve 3, PID pressure controller 5 and gas-holder 2 are formed, folding by PID controller controlled pressure operation valve 3, by gas-holder 2 injecting gas or discharge gas to gas-holder in reactor by reactor, can accurately control the pressure in the reactor, pressure controling precision is ± 0.02Mpa.
Temperature control unit is a high-precision water bath with thermostatic control 7, and for experiment provides evenly constant external environment temperature field, precision is ± 0.1K.
Metering units comprises: two temperature sensors of high precision 6 that are used to measure temperature of reaction kettle, and precision is ± 0.05K; Be used to measure 4 two of the pressure transducers of reactor and gas-holder pressure, precision ± 0.02MPa; Two 13,16 of electronic balances, precision 0.01g is used to measure the quality of injecting with the solution that flows out reactor.
Adopt present embodiment can carry out following experiment:
1, pure water hydrate phase balance experiment
Observation is adopted in this experiment, and the method has to be measured accurately, the advantage that experimental period is short, and main experimental procedure is as follows:
1) at first adopt balance 13, constant-flux pump 14, intermediate receptacle group 15 in reactor 1, to inject certain density chemical agent aqueous solution, by the time begin after the temperature stabilization gas in the gas cylinder 8 to be injected reactor 1 by reduction valve 9, stop valve 10, retaining valve 11, and begin to stir, accelerate the generating rate of hydrate, (pressure, temperature) under certain conditions forms a certain amount of hydrate in reactor;
2) keep a parameter (pressure or temperature) constant, make decomposition of hydrate by reducing pressure or rising temperature then;
3) in reactor, only there is the hydrate crystal of minute quantity to exist, at this moment keep the parameter (temperature, pressure) of the hydrate in the reactor constant, if can there be 3-4h in the hydrate in the reactor, then keep temperature-resistant in the reactor, emit portion gas with excess pressure operation valve 3, make pressure reduce 0.05Mpa, if the hydrate in the reactor dissolves fully, then the pressure in the reactor, temperature can be regarded the equilibrium of this system as.
In this experiment, the most important thing is and to control accurately temperature, the pressure of reactor 1, in general keep temperature-resistant, change pressure and can reach equilibrium state faster, in this experiment, the control of pressure is finished by PID pressure controller 5 and pressure control valve 3, can improve pressure or outwards discharge gas by reactor by pressure control valve 3 injecting gas in reactor and reduce pressure.
2, hydrate phase balance experiment in the porous medium
This experiment is mainly studied under the sandstone state, and chemical agent is in conjunction with the influence of capillary force to natural gas hydrate phase balance emulation, and main experimental procedure is as follows:
1) in reactor, fills up sand, and adopt piston to compress sand grains, make the porous medium in the reactor reach certain porosity, draw its porosity by the weight and volume of determining sand;
2) annotate the chemical agent aqueous solution in reactor, determine that it is saturated, injecting gas reaches certain pressure then;
3) begin cooling generation hydrate, after a large amount of generations of hydrate, heat up and decompose, what the speed of intensification will be enough is slow, is 0.5K/5-24h, makes each step all reach equilibrium state, adopts the picture method to determine balancing each other a little of hydrate then;
4) adopt different original pressures, repeated experiments obtains the equilibrium point data under different pressures, the temperature.
The above only is a preferable embodiment of the present invention, and protection scope of the present invention is not limited thereto, and those of skill in the art are any to be included within protection domain of the present invention based on non-material change on the technical solution of the present invention.
Claims (5)
1, a kind of natural gas hydrate phase balance emulation experiment device is characterized in that, comprises the analogue unit that balances each other, pressure control unit, temperature control unit, voltage stabilizing liquid-supply unit, gas supply under constant pressure unit, metering units, data acquisition unit.
2, natural gas hydrate phase balance emulation experiment device as claimed in claim 1, it is characterized in that, the described analogue unit that balances each other comprises high pressure resistant reactor (1), the bottom of this reactor (1) is provided with piston mobile (18), and this reactor (1) top has adjustable speed electromagnetic mixing apparatus (19).
3, natural gas hydrate phase balance emulation experiment device as claimed in claim 1, it is characterized in that, the described analogue unit that balances each other comprises high pressure resistant reactor (1), and the bottom of this reactor (1) is provided with piston mobile (18), fills up porous medium in the reactor.
As the arbitrary described natural gas hydrate phase balance emulation experiment device of claim 1-3, it is characterized in that 4, described voltage stabilizing liquid-supply unit is made up of electronic balance (13) (16), constant-flux pump (14), intermediate receptacle group (15).
As the arbitrary described natural gas hydrate phase balance emulation experiment device of claim 1-3, it is characterized in that 5, described pressure control unit is mainly by pressure control valve (3), pressure transducer (4), PID pressure controller (5) and gas-holder (2) are formed.
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