CN1588022A - Method and device for in-site measuring gas hydrate and deposit sediment heat stability containing hydrate - Google Patents
Method and device for in-site measuring gas hydrate and deposit sediment heat stability containing hydrate Download PDFInfo
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- CN1588022A CN1588022A CN200410051811.0A CN200410051811A CN1588022A CN 1588022 A CN1588022 A CN 1588022A CN 200410051811 A CN200410051811 A CN 200410051811A CN 1588022 A CN1588022 A CN 1588022A
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Abstract
The invention provides a method and the setting used for insite measuring the thermonature of the gaseous hydrate and the sediments which containing hydrate. The said measuring system includes a gas inlet and outlett systems; a temperature control system, a high presser viarable capacitied reactor; a hydraulic transmission system; a observing and control gathering system. The said method includes the following steps the reacting gas entering the high pressure viarable capacital reactor which immersed in the temperature control system through gas inlet and outlet system,and reacting with the other reactants in the high pressure variable capcity reactor to produce gaseous hydrate or hydrate sediments on constant temperature and pressure condition controlled by the temperature control system and hydraulic driving system seperatively;last,measuring the thermophysical property of the produced gaseous hydrate or hydrate sediments by the observing and control gathering system. The design of the invention can meet the synthesis of different types and quantity of hydrate and realizes the insite measurement of the thermophysical property of the hydrate.
Description
Technical field
The present invention relates to a kind of measurement gas hydrate and contain the method and the device of the hot rerum natura of hydrate sediment.
Background technology
Gas hydrate is a kind of envelope shape crystal of gas or volatile liquid and water effect formation.Gas hydrate claims clathrate hydrate again, and it has unique molecule framework: hydrone forms the molecule cage by Van der Waals force, and guest molecule then is wrapped in to do relatively freely in the hydrone cage and rotatablely moves.Research at present is gas hydrate and refrigerant hydrate with the most deep hydrate at most, and the former is subjected to extensive concern as a kind of huge potential energy source and the mode of stored energy source; The latter is considered to one of better cool storage medium because it has higher phase transition temperature (5-12 ℃) and the latent heat of phase change suitable with ice.
Though the phase transition temperature of refrigerant hydrate cold-storage is higher than the phase transition temperature of traditional ice cold-storage, there is certain deficiency in the hydrate cold-storage, and it is low mainly to show as crystallization difficulty and coefficient of heat conductivity.Therefore be necessary how research strengthens its heat conductivility, as the metal nanoparticle that adds high thermal conductivity therein or nano-carbon powder etc.As a kind of huge potential energy source, gas hydrate are stored in seabed or continent permafrost zone usually, and its principal ingredient is methane and water.Because methane is more than 20 times of carbon dioxide to the greenhouse effect of atmosphere, and gas hydrate have the mechanical property harder than ice, subside so the stability of gas hydrate is related to the extensive landslide of global warming and seabed sea bed.Simultaneously, gas hydrate are very responsive to variation of temperature, so be necessary to grasp the Changing Pattern of its hot rerum natura when assessing hydrate to the influencing of environmental change.
Studies have shown that clathrate hydrate family has unique thermophysical property, though they are a kind of crystal, its coefficient of heat conductivity varies with temperature has Vitrea variation characteristic.From molecular structure, gas hydrate and ice structure are closely similar, and its coefficient of heat conductivity more approaches the analog value of water.Because most gas hydrates are unsettled at normal temperatures and pressures, at the coefficient of heat conductivity report ten minutes shortage of hydrate.In view of forefathers' experience, our urgent hope can be adopted a kind of rapid and reliable method of testing measuring samples, so that provide important referential data for science and engineering circle.On the other hand, the simple sample of the thermal conductivity ratio of hydrate in porous medium seems even more important, because be concerned about the hot rerum natura Changing Pattern of gas hydrate under the state of nature more in engineering reality, this mainly shows as the heat exploitation of gas hydrate.
At the material of low thermal conductivity, main measuring method is a heat-pole method at present.What extensively adopt in the world is sonde method, and it is based on the transient measurement method of line heat source.But hydrate has its singularity, and structure was very loose after it generated.If use probe measurement this moment, the result can be very untrue, needs pressurization to make compact structure.Axial pressure (this is the method for effectively driving away residual gas) normally, but pressurization can make the volume of hydrate change, and probe is axially to place, probe is put and has just been become matter of utmost importance like this.Use at present the thermal conductivity value difference of the hydrate that sonde method measures very big in the world, and can not provide the temperature variant relation of very believable coefficient of heat conductivity.This is because sonde method and be not suitable for measuring the coefficient of heat conductivity of hydrate, the generation quality of its hydrate existing problems on the other hand on the one hand.
Summary of the invention
The objective of the invention is to overcome the deficiency of the hot physical property measurement method of above-mentioned hydrate, provide a kind of can the in site measurement gas hydrate and contain the method and apparatus of the hot rerum natura of hydrate sediment.
For reaching above purpose, the technical solution adopted in the present invention is:
Device involved in the present invention comprises 5 big autonomous systems, is respectively: gas input and output system; Temperature control system; High pressure variable volume reactor; Hydrostatic transmission (pressurization) system; The observing and controlling acquisition system.Be illustrated referring now to Fig. 1 and Fig. 2.
Gas input and output system mainly are made up of valve and pipeline, comprising some instrument and utility appliance.The major function of this system is to realize the circulation of gas and the monitoring of gas state parameter.
Temperature control system is mainly used to realize the desired temperature conditions of experiment, and normally used all is the combination of instruments such as refrigeration compressor set and thermal switch.
High pressure variable volume reactor is shown among Fig. 1 11, and it is to be immersed in fully in the bath 10.This high pressure variable volume reactor comprises the columnar reactor body of an end opening, be arranged on the chamber lid of reactor body openend, the gas pipeline that is arranged on the chamber lid enters the port of reactor, the inlet of thermophysical property measurement instrument probe and the inlet of thermal resistance, is arranged on the piston of reactor body inside and is arranged on the port that the reactor body bottom is connected with the high-pressure pump of Hydraulic Power Transmission System; The thermophysical property measurement instrument probe is clamped by two shells and is placed between the piston and chamber lid in the reactor body, is connected with thermophysical property measurement instrument arithmetic section by external wire.The thermophysical property measurement instrument probe that this place uses can be the Hotdisk probe, and thermal resistance can be thermal resistance Pt100.This structure has realized: 1) to hydrate and contain the in site measurement of the hot rerum natura of hydrate sediment; 2) owing to used Hydraulic Power Transmission System, setting-out and sampling are comparatively convenient; 3) can use hydraulic pressure that sample is pressurizeed and overcome the influence of thermal contact resistance measurement result.
Hydraulic Power Transmission System is to apply certain pressure by the external world to cause pressure reduction, and transmits pressure by seal fluid, and it can be that an external high-voltage power supply produces certain pressure, and by the incompressibility of liquid pressure or power is sent to desired area.The volume of above variable volume reactor changes by hydrostatic transmission change inside reactor piston position to be realized.
The observing and controlling acquisition system mainly refers to the measuring system and the data acquisition system (DAS) 13 of the hot rerum natura of measuring samples.This two cover system can adopt the Agilent34901A data acquisition system (DAS) of being made by the Hotdisk system of Sweden Hotdisk AB company manufacturing and U.S. Agilent company respectively.We have used and can overcome the transient state plane heat source method of testing of thermal contact resistance to the coefficient of heat conductivity influence, it is Hotdisk thermophysical property measurement instrument, and this testing tool has the sonde configuration than small scale, and it is suitable for being placed in the sample, and can carry out compression to a certain degree.The test section more related than sonde method, its test section in sample is much smaller, and the deviation of sample quality reduces greatly to its influence.All the other general data acquisition system (DAS)s also can be used at this.
When this covering device uses, reacting gas enters the high pressure variable volume reactor that is immersed in the temperature control system via the gas input-output system, and under certain temperature and pressure condition, react and generate gas hydrate or hydrate sediment with other reactants in the high pressure variable volume reactor, wherein temperature conditions is controlled by temperature control system, pressure condition is controlled by Hydraulic Power Transmission System, by the observing and controlling acquisition system gas hydrate of reaction generation or the hot rerum natura of hydrate sediment is measured at last.During reaction, existing with in the reaction liquid injecting reactor 11, fastening then lid 11-5 seals up Hotdisk lead 11-3 simultaneously, vacuumizes according to step recited above then.Temperature control system is adjusted to the temperature required condition of reaction, the beginning air inlet.Behind reaction terminating, can carry out in site measurement to sample, this process is that heat-insulation pressure keeping carries out.Therefore this process comprises the experiment of two classes:
1) gas hydrate reaction of formation.The temperature, pressure design of this experimental provision can generate the gas hydrate of nearly all type known today.
2) hot physical property measurement.Hotdisk method based on the transient state plane heat source used in the present invention is initiated.
The invention has the beneficial effects as follows:
1) it is synthetic that the design of Du Te hydrate generating apparatus can be satisfied the hydrate of dissimilar and different amounts, and can relatively easily take out (being released by piston) after synthetic.
2) realize the in site measurement of the hot rerum natura of hydrate, and realize and to carry out the axial pressure densification to measuring samples, can discharge gas unnecessary in the sample effectively.
3) transient state plane heat source method is applied to the measurement of hydrate coefficient of heat conductivity.
4) can when measuring, realize heat-insulation pressure keeping, even realize the constant temperature level pressure.
5) can carry out pressurize, insulation measurement to the sample of the gained of sampling on the spot, thereby determine the effective thermal conductivity of sample, further can instruct heat to exploit and judge the stabilized zone of sea bottom hydrate.
6) can pass through corresponding software, cooperate thermal conductivity measurement to determine the approximate content of hydrate in institute's sample thief on the spot, thereby this regional hydrate total amount is assessed.
7) the temperature, pressure scope of Ce Lianging is wide, can carry out low temperature, High-Voltage Experimentation.
8) adopted integrated design, whole test structure compactness.
Description of drawings
Fig. 1 is the structural representation that whole gas hydrate generates proving installation;
Fig. 2 is a high pressure variable volume inside reactor structural representation.
Specific embodiment
Further specify content of the present invention below in conjunction with embodiment.
Designed an experimental provision by Fig. 1 and Fig. 2, except that dated especially, all connecting tubes are that external diameter is the stainless-steel tube of 6mm, and all connect use and are threaded the sealing of snap ring cutting ferrule.The withstand voltage 30MPa of reactor, internal diameter 50mm, high 250mm, wall thickness 7mm, its lid height is 70mm, above institute three holes of opening by arranging as shown in Figure 2.
The gas input-output system is: mass-flow gas meter 1, and retaining valve 2, exsiccator 3, vacuum pump 8, gas cylinder 9, tensimeter B1, B2, vacuum meter B3, valve F1, F2, F3, F4, F5 forms.Wherein web member is the stainless steel pipes of external diameter 6mm, and the joint is being threaded of snap ring, cutting ferrule sealing.Valve F1 is the switch of control source of the gas turnover; F2 is the switch that pilot-gas enters mass-flow gas meter; F3 is the switch on drop-leg road, and gas shunting herein mainly is to consider to avoid gases at high pressure mass-flow gas meter to precision when just entering system to impact; F4 is that system vacuumizes switch, should close when reaction herein; F5 is the emptying switch, and its effect mainly is to discharge residual gas and vacuum pump resets after reaction.Need before reaction all valve opens, high-speed switch valve F1 continuously squeezes portion of air thereby allow reacting gas in the gas cylinder wash away pipeline continuously, closing valve F1 after this, and F5 opens vacuum pump and begins to vacuumize.Total system is vacuumized finish after, valve-off F4 opens valve F5 vacuum pump is resetted.Valve-off F2 opens valve F1 and begins air inlet, wait the system pressure balance after, valve-off F3 opens valve F2 and begins the monitoring system gas flow.
Temperature control system is by stirring vane 6, heat exchange coil 7, and bath 10 and temperature controller 12 are formed.The body lotion that adopts is an alcohol in the bath 10, and using alcohol rather than water is that ice can influence the heat exchange effect of heat exchange coil and freeze stirring vane because consider at water below 0 ℃ and will freeze as heat transfer medium, finally causes temperature distributing disproportionation in the bath.This control system can be controlled at temperature between-45 ℃ to 50 ℃, and control accuracy is ± 0.1 ℃.
The structure of high pressure variable volume reactor wherein also comprises the layout synoptic diagram of the thermophysical property measurement probe that carries out in site measurement as shown in Figure 2.11-1 is the port that gas pipeline enters reactor, between by being threaded, the sealing of snap ring cutting ferrule.Gas pipeline herein is thinner, use be the stainless steel pipes of 3mm external diameter; 11-2 is the inlet of thermophysical property measurement instrument Hotdisk probe, by being threaded the sealing of O type circle; 11-3 is the external wire of thermophysical property measurement instrument Hotdisk; 11-4 is a thermal resistance Pt100 inlet, by being threaded the sealing of snap ring cutting ferrule; 11-5 is the lid of stainless steel reactor, it in reactor between by being threaded, the sealing of O type circle; 11-6 is the O RunddichtringO; 11-7 is its outside polymethylmethacrylate (PMMA) shell that is clipped in that designs in order to protect soft Hotdisk thermophysical property measurement probe not to be damaged, this shell divides two, place the both sides of probe 11-9 respectively and it is clipped in the middle, fastening by the screw shown in the 11-8, at the shell center section is an open circles hole, guarantees that herein probe 11-9 can fully contact and measure with sample; 11-10 is the main part of reactor, and its wall thickness 7mm uses stainless steel, and internal diameter is 50mm, highly is about 250mm, and the withstand voltage 30MPa that reaches, maximum volume are 200ml; 11-11 is as hydraulicdriven alcohol, and hydraulic pressure is that the port one 1-13 by external high-pressure pump passes over; 11-12 is a piston apparatus, and its material is a stainless steel, by the sealing of double-deck O circle.The uniqueness of this covering device is that it can control the height of sample, and the amount of sample is not subjected to the restriction of reactor volume, and sample can be compressed densification, and reaction end back sampling ratio is more convenient etc.
Hydraulic Power Transmission System comprises high pressure hand pump 5 as shown in Figure 1, valve F6, F7.Connect the sealing of snap ring cutting ferrule therebetween by the 6mm stainless steel pipes.High pressure hand pump 5 maximums can produce the fluid pressure of 50MPa, and by liquid feeding and discharge opeing, piston position and internal pressure in the reactor can be effectively controlled.When adopting alcohol to be the body lotion of bath 10, consider that the driving medium of considerable part is operated in the alcohol bath, therefore the driving medium that herein uses is alcohol.
The observing and controlling acquisition system comprises measuring system and the data acquisition system (DAS) 13 that refers to the hot rerum natura of measuring samples, adopts respectively by the Hotdisk system of Sweden Hotdisk AB company manufacturing and the Agilent 34901A data acquisition system (DAS) of U.S. Agilent company manufacturing.
Embodiment 1
In Fig. 1,2, be reactant with methane gas and 280ppm sodium dodecylsulphonate (SDS) aqueous solution, reaction synthetic generation of methane hydrate.Regulate temperature control system before the experiment earlier, the temperature of reaction is set at 0 ℃, with the SDS aqueous solution cleaning reaction device 11 of the 280ppm that has prepared, inject 100 gram sodium dodecylsulphonate (SDS) aqueous solution subsequently then, cover chamber lid 11-5 and sealing then.Then valve F1, F2, F3, F4 and F5 are opened, continuous high-speed switch valve F1 squeezes portion of air thereby allow methane gas in the gas cylinder 9 wash away pipeline continuously, closing valve F1 after this, and F5 opens vacuum pump 8 and begins to vacuumize.After treating that vacuum meter is stable, valve-off F4 opens valve F5 vacuum pump 8 is resetted.Valve-off F2, open valve F1 and begin air inlet, after the system pressure balance, valve-off F3 opens valve F2, and methane flows out by gas cylinder 9, enter high pressure variable volume reactor 11 through gas meter 1 and retaining valve 2, begin the monitoring system gas flow simultaneously, feed the methane gas of certain pressure, this reaction uses methane pressure to be 6.6MPa.
Methane enters reactor port 11-1 by the gas pipeline on the high pressure variable volume reactor 11 and enters in the reactor 11, with 280ppm sodium dodecylsulphonate (SDS) reactant aqueous solution in the reactor 11.Deng the back (reactor temperature, pressure no longer changes) that reacts completely, continued to keep the used temperature, pressure parameter of reaction 2～3 days, guarantee that sample is aging.Begin the thermal physical property parameter of in site measurement sample subsequently, the result shows that in the time of 0 ℃, when sample was not pressurizeed densification by piston, its coefficient of heat conductivity was 0.36W/mK, and after the sample pressurization densification, coefficient of heat conductivity is 0.57W/mK.When temperature changed continuously from-10 ℃ to 5 ℃, the coefficient of heat conductivity of measuring rose with temperature, presents the Changing Pattern of tangible vitreum coefficient of heat conductivity.Experimental result proves that this device is synthesized hydrate preferably, and used measuring method adapting device is well finished in site measurement to the hot rerum natura of hydrate.
Embodiment 2
Mix with sand and tetrahydrofuran solution and to measure the effective thermal conductivity that contains tetrahydrofuran sand porous medium, this example is that simulation is measured the effective thermal conductivity of actual samples sample.As mentioned above, before the experiment temperature control system is set at 0 ℃, be in 21% the tetrahydrofuran aqueous solution injecting reactor then with mass ratio, the construction sand of 300-125 μ m that will be by screening with glass bar slowly imports in the solution, until the sand layer Hotdisk probe is flooded fully.With the unnecessary tetrahydrofuran aqueous solution sucking-off in sand layer top, whole reactor is placed temperature control system with suction pipe, begin reaction.After about 5～10 hours, liquid phase all is converted into the tetrahydrofuran hydrate, continues under the Current Temperatures pressure condition, and it wears out insulation 2～3 angels.Carry out in site measurement subsequently between-10 ℃ ~-2 ℃, its thermal conductivity value is about about 1.9W/mK.Experiment showed, that this device can measure the effective thermal conductivity that contains the hydrate porous medium preferably.
After testing the result, the cooperation correspondent computer software is asked the hydrate content in the sample.This software is based on the mathematical model of deriving in this laboratory and uses Visual Basic language to work out, the hypothesis hydrate is equally distributed in model, and the intrinsic coefficient of heat conductivity of sand and the coefficient of heat conductivity of tetrahydrofuran hydrate are known, can calculate the approximate content of tetrahydrofuran hydrate like this by the effective thermal conductivity that records, to the result of calculation of example two be: the volume content of tetrahydrofuran hydrate is about 53.5% of cumulative volume.The long-pending content of ice body of considering the sand porous medium that contains ice is about 49%, and the density of tetrahydrofuran hydrate is less than the density of ice, so this calculated value still relatively reasonably.This proves that this device cooperates corresponding software can estimate hydrate content in the sample.
Claims (10)
1. a gas hydrate and contain the measurement mechanism of the hot rerum natura of hydrate sediment, it is characterized in that: described measurement mechanism comprises gas input and output system; Temperature control system; High pressure variable volume reactor (11); Hydraulic Power Transmission System; The observing and controlling acquisition system.
2. gas hydrate according to claim 1 and contain the measurement mechanism of the hot rerum natura of hydrate sediment, it is characterized in that: described high pressure variable volume reactor is immersed in the bath 10 fully, the columnar reactor body (11-10) that comprises an end opening, be arranged on the chamber lid (11-5) of reactor body (11-10) openend, be arranged on the port (11-1) that gas pipeline on the chamber lid (11-5) enters reactor, the inlet (11-4) of inlet of thermophysical property measurement instrument probe (11-2) and thermal resistance (4) is arranged on the inner piston (11-12) of reactor body (11-10) and is arranged on the port (11-13) that reactor body (11-10) bottom is connected with the high-pressure pump (5) of Hydraulic Power Transmission System (d); Thermophysical property measurement instrument probe (11-9) is clamped by two shells (11-7) and is placed between reactor body (11-10) the interior piston (11-12) and chamber lid (11-5), is connected with the thermophysical property measurement instrument by external wire (11-3).
3. gas hydrate as claimed in claim 2 and contain the measurement mechanism of the hot rerum natura of hydrate sediment, it is characterized in that: the body lotion that uses in the described bath 10 is alcohol.
4. a gas hydrate and contain the measuring method of the hot rerum natura of hydrate sediment, it is characterized in that this method may further comprise the steps: reacting gas enters the high pressure variable volume reactor that is immersed in the temperature control system via the gas input-output system, and under certain temperature and pressure condition, react and generate gas hydrate or hydrate sediment with other reactants in the high pressure variable volume reactor, wherein temperature conditions is controlled by temperature control system, pressure condition is controlled by Hydraulic Power Transmission System, by the observing and controlling acquisition system gas hydrate of reaction generation or the hot rerum natura of hydrate sediment is measured at last.
5. gas hydrate as claimed in claim 4 and contain the measuring method of the hot rerum natura of hydrate sediment is characterized in that this method may further comprise the steps:
A, open the gas cylinder (9) of gas input and output system, supplant the portion of air in the gas pipeline after, open vacuum pump (8) and begin to vacuumize.Total system is vacuumized finish after, begin to feed reacting gas, wait the system pressure balance after, beginning monitoring system gas flow;
B, regulate the temperature controller (12) in the temperature control system, the temperature of bath (10) is controlled in the setting range, start stirring vane (6) and heat exchange coil (7) and guarantee that the temperature of whole bath (10) is even;
C, start the high pressure hand pump (5) in the Hydraulic Power Transmission System, the reaction pressure in the high pressure variable volume reactor (11) is controlled in the setting range;
D, the reacting gas of gas cylinder (9) output is input in the high pressure variable volume reactor (11), under the temperature and pressure of setting, reacts, generate gas hydrate or contain the hydrate sediment with other reactant of high pressure variable volume reactor (11);
The gas hydrate that e, question response generate or contain the hydrate sediment aging after, start observing and controlling acquisition system and data acquisition system (DAS) (13), begin gas hydrate or contain the sedimental hot rerum natura of hydrate to carry out in site measurement.
6. according to claim 4 or 5 described gas hydrates and contain the measuring method of the hot rerum natura of hydrate sediment, it is characterized in that: used driving medium is an alcohol in the Hydraulic Power Transmission System.
7. high pressure variable volume reactor that is used to implement claim 4 or 5 described methods, it is characterized in that: described high pressure variable volume reactor comprises the columnar reactor body (11-10) of an end opening, be arranged on the chamber lid (11-5) of reactor body (11-10) openend, be arranged on the port (11-1) that gas pipeline on the chamber lid (11-5) enters reactor, the inlet (11-4) of inlet of thermophysical property measurement instrument probe (11-2) and thermal resistance (4) is arranged on the inner piston (11-12) of reactor body (11-10) and is arranged on the port (11-13) that reactor body (11-10) bottom is connected with the high-pressure pump (5) of Hydraulic Power Transmission System (d); Thermophysical property measurement instrument probe (11-9) is clamped by two shells (11-7) and is placed between reactor body (11-10) the interior piston (11-12) and chamber lid (11-5), is connected with the thermophysical property measurement instrument by external wire (11-3).
8. high pressure variable volume reactor according to claim 7 is characterized in that: described reactor body (11-10) is made by stainless steel material.
9. high pressure variable volume reactor according to claim 7 is characterized in that: by being threaded, and seal with O type circle (11-6) between described chamber lid (11-5) and the reactor body (11-10); By being threaded, seal between the port (11-1) that described gas pipeline enters reactor and the chamber lid (11-5), between the inlet (11-4) of thermal resistance (4) and the chamber lid (11-5) with the snap ring cutting ferrule.
10. a kind of high pressure variable volume reactor according to claim 7, it is characterized in that: piston (11-12) is made by stainless steel material, seals by double-deck O type circle (11-6) with reactor body (11-10) inwall; Described two shells (11-7) are made by polymethyl methacrylate, and (11-8) is fastening by screw.
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2004
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