CN103257203A - High-pressure integrated experiment apparatus for novel energy hydrate - Google Patents
High-pressure integrated experiment apparatus for novel energy hydrate Download PDFInfo
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- CN103257203A CN103257203A CN2012100355599A CN201210035559A CN103257203A CN 103257203 A CN103257203 A CN 103257203A CN 2012100355599 A CN2012100355599 A CN 2012100355599A CN 201210035559 A CN201210035559 A CN 201210035559A CN 103257203 A CN103257203 A CN 103257203A
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Abstract
The invention discloses a high-pressure integrated experiment apparatus for novel energy hydrate. The apparatus composed of six modules can realize phase equilibria of single or mixed gas hydrates, generation, and research of decomposition dynamics. The apparatus is convenient to operate, and accurate in measure, and can realize high-precision control for pressure and temperature.
Description
Technical field
The invention belongs to physics facility, relate in particular to the Comprehensive Experiment high-tension unit of a kind of hydrate phase balance, dynamics research.
Background technology
Gas hydrate (Natural Gas Hydrate, be called for short Gas Hydrate) claim the cage modle inclusion compound again, be under certain condition temperature, pressure by water and energy gas molecule (as CH
4, C
2H
6, C
3H
8Etc. short-chain hydrocarbons gas etc.) ice, the non-stoichiometric cage modle crystalline compounds of class that forms.This material is met both incendivities of fire, is commonly called as " combustible ice ".Molecular formula M.nH
2O represents that M represents the gas molecule in the hydrate, and n is hydration number (being water molecule number).
Emphasis in the early stage research of hydrate research is balancing each other, and turns in recent years that hydrate forms, the research of decomposition kinetics process.No matter the research that balances each other of hydrate, or the research of dynamics aspect in fact all are the processes that a water-air-water compound three-phase equilibrium changes, any factor that balances each other that can influence can both influence hydrate formation, decompose.Therefore, precision controlled in in-situ observation, the condition of experimental facilities accurately is absolutely necessary.
The researcher of various countries is used when carrying out the experiment of hydrate mostly to be not visible stainless steel still, and experimental pressure is in tens MPa ranks, and this kind equipment can be used to research as CH
4Etc. hydrate phase balance or the dynamics research of gases such as short-chain hydrocarbons, and can not need the H of high pressure
2And CO2 hydrate phase balance and dynamic (dynamical) research.
Summary of the invention
The object of the invention is to provide a kind of and can also realizes conventional hydrate and H by in-situ observation
2And the balancing each other and the Comprehensive Experiment high-tension unit of dynamics research of CO2 hydrate.
Above-mentioned purpose of the present invention is achieved through the following technical solutions:
According to the present invention, a kind of new forms of energy hydrate composite experiment high-tension unit is provided, comprise inflator module, hydrate generation and characterization apparatus, temperature control modules and vacuum module, wherein,
Inflator module generates with hydrate and characterization apparatus is connected, for it provides one or more reacting gas;
Vacuum module generates with inflator module and hydrate and characterization apparatus is connected, in order to vacuumize;
Temperature control modules generates with hydrate and is connected with characterization apparatus, and hydrate generates and the temperature of characterization apparatus to measure and to control.
In said apparatus, also comprise the supercharging module, one or more reacting gas that provided by inflator module this supercharging module of flowing through arrives hydrate and generates and characterization apparatus.
In said apparatus, described supercharging module comprises filtrator and two-stage supercharger.
In said apparatus, described hydrate generates and bottom surface and the side of characterization apparatus are provided with the optical window that generates, decomposes for the in-situ monitoring hydrate.
In said apparatus, by optical fiber Raman signal is inserted described optical window, be used for the generation of real-time monitored hydrate, decomposition kinetics and feature such as balance each other.
In said apparatus, described inflator module comprises gas cylinder, the mass flowmeter that is connected with gas in the gas cylinder.
In said apparatus, described inflator module also comprises surge tank, is used for multiple gases is mixed.
In said apparatus, described temperature control modules comprises water-bath or air bath, and temperature sensor.
In said apparatus, described temperature controller comprises two kinds, and a kind of being arranged in hydrate generation and the characterization apparatus is used for measuring the internal temperature of hydrate generation and characterization apparatus, another kind is arranged in the water-bath, is used for measuring the external temperature of hydrate generation and characterization apparatus.
In said apparatus, also comprise with hydrate generating the data acquisition module that links to each other with characterization apparatus, be used for gathering temperature and the pressure data of hydrate generation and characterization apparatus.
Compared with prior art, the invention has the advantages that:
1, can realize CH
4, H
2And CO
2Height in hydrate is pressed into;
2, can realize CH
4, H
2And CO
2Deng characteristic presents such as hydrate high pressure dynamics in place;
3, system is easy and simple to handle, measurement is accurate and to the control of pressure, temperature high precision.
Description of drawings
It is following that embodiments of the present invention is further illustrated with reference to accompanying drawing, wherein:
Fig. 1 is the rough schematic view of hydrate composite experiment high-tension unit according to an embodiment of the invention;
Fig. 2 is each ingredient synoptic diagram of hydrate composite experiment high-tension unit according to an embodiment of the invention;
Fig. 3 is that the hydrate of hydrate composite experiment high-tension unit according to an embodiment of the invention generates and the characterization apparatus synoptic diagram.
Embodiment
Fig. 1 is the rough schematic view of hydrate composite experiment high-tension unit according to an embodiment of the invention.As shown in Figure 1, this hydrate composite experiment high-tension unit comprises inflator module, hydrate generation and characterization apparatus, supercharging module, vacuum module, temperature control modules and data acquisition module.Below referring to Fig. 2, each module is done specific descriptions.
As shown in Figure 2, inflator module is that hydrate generates and characterization apparatus (for example being reactor 33) provides one or more reacting gas, and it specifically can comprise gas cylinder 1, reduction valve 2, mass flowmeter 4,7,10, counterbalance valve 12 and surge tank 14,17,20.Inflator module can realize the premix of multiple gases different component by the accurate control amount of mass flowmeter realization to differential responses gas by surge tank.
After reacting gas is transported in hydrate generation and the characterization apparatus, under uniform temperature and the pressure will hydrate generate and characterization apparatus in hydrate reaction takes place, for the ease of processes such as the generation of in-situ observation hydrate, decomposition, can be on hydrate generation and characterization apparatus, more specifically, on the bottom surface or side of hydrate generation and characterization apparatus, one or more optical windows are set, in order to observe.As shown in Figure 3, in one embodiment, optical window can be arranged on the bottom surface of hydrate generation and characterization apparatus.In addition, see through this optical window and can also insert Raman signal by optical fiber, be used for the generation of real-time monitored hydrate, decomposition kinetics and feature such as balance each other.
Alternatively, also the supercharging module can be set between inflator module and hydrate generation and characterization apparatus, the gaseous tension that this supercharging module is used for inflator module is carried raises, thereby reaches the required pressure condition of experiment.This module specifically can comprise filtrator 28 (prime filtrator), 30 (high pressure filters) and two-stage supercharger 29, when work, the reacting gas that is transferred enters from prime filtrator 28, flows out from high pressure filter 30, enters at last in hydrate generation and the characterization apparatus.In one embodiment, this supercharging module can realize any hydrate experiment in 200 MPas, and comprises the H of formation condition harshness
2Hydrate.
Hydrate composite experiment high-tension unit of the present invention also comprises vacuum module, it generates with inflator module, supercharging module and hydrate and characterization apparatus is connected, can vacuumize each module respectively, in addition, the vacuum purification function to installing before can also realizing testing.This module specifically can comprise tensimeter 22, pressure transducer 23 and vacuum pump 24 and connecting pipeline.In one embodiment, the vacuum tightness after vacuumizing can reach less than 3 Pascals.
Generate the temperature control module that also has that is connected with characterization apparatus with hydrate, it is mainly used in measuring and controlling, and hydrate generates and the temperature of characterization apparatus, for example can measure temperature in the kettle by the smart temperature sensor that is arranged in hydrate generation and the characterization apparatus, or can measure still temperature outward by being arranged on water bath with thermostatic control or the air bath 35 that hydrate generates and characterization apparatus is outer, and can in the water-bath 35 another temperature sensor 34 be set, with real-time monitoring water temperature.Since course of reaction sometimes the duration longer, the multistage temperature can be set in course of reaction, and this multi-segment program temperature controlled water bath can realize that in conjunction with the smart temperature sensor in hydrate generation and the characterization apparatus hydrate generates, decomposes and the accuracy control over temperature that balances each other.
Preferably, arrange with hydrate and generate the data acquisition module that is connected with characterization apparatus, this module is mainly used in experimental datas such as the relevant temperature of collection, pressure from hydrate generation and characterization apparatus, and it can be connected with temperature sensor or pressure transducer.In one embodiment, this module can be computing machine or multiprogram switch board 36.
Be to utilize hydrate composite shown in Figure 3 experiment high-tension unit to carry out the method for hydrate compound experiment below, comprise following 8 steps: hydrate generates and characterization apparatus filler, gas circuit are cleaned, vacuumize, inflation, supercharging (optionally), temperature control, synthesize, exhaust.
1) hydrate generates and the characterization apparatus filler.The experimental solutions rinse water compound that being about to of at first will preparing in advance carried out generates and characterization apparatus 33 3 times, the required solution quality of experiment weighs with scale, and measure its volume with graduated cylinder, to guarantee that testing the solutions employed volume is no more than 2/3rds of hydrate generation and characterization apparatus volume.
2) gas circuit is cleaned.Open all valves in the gas circuit, earlier purge whole gas circuit three times with nitrogen, use the whole gas circuit of gas purging that is about to experimentize then three times.
3) vacuumize.At first close gas cylinder 1 gas admittance valve and vent valve 26 before the vacuum module work, other all valves in the gas circuit are opened simultaneously, guarantee that gas circuit and vacuum module constitute a path.During vacuum module work, before this vacuum tightness of gas circuit was evacuated to smaller or equal to 3 Pascals, shut-off valve 25 uses then to be about to do the used whole gas circuit of purge of gas of experiment, and then vacuumizes three precision to guarantee to test like this.
4) inflation.Gas replenishment process can be selected pure gas gas replenishment process or combination gas gas gas replenishment process.
When using pure gas, close vacuum module operation valve 25, supercharger and use operation valve 27,32 and vent port operation valve 26, open valve and the valve 3,5,13,15 and 31 of gas cylinder 1 successively, other valve closures.Regulate reduction valve 2, counterbalance valve 12 guaranteeing stable gas differential pressure, thereby obtain to test gases used amount accurately, reach the experiment setting value after, shut-off valve 31,15,13,5,3 and the valve of gas cylinder 1 successively.
When using mixed gas, the mixed gas gas replenishment process is Duoed air mixing process between different surge tanks than the pure gas gas replenishment process.Be mixed into example with methane and two kinds of gases of ethane, close vacuum module operation valve 25 and vent port operation valve 26, open valve and the valve 3,5,13 and 15 of gas cylinder 1 successively, other valve closures.Make methane gas pressure reach the required value of experiment, shut-off valve 15,13,5 and 3 successively in conjunction with tensimeter 22, pressure transducer 23.Open 6,8,16 and 18 then, make ethane gas pressure reach the required value of experiment in conjunction with tensimeter 22, pressure transducer 23, close 16,8 and 6 successively.Open valve 15 and valve 31 then, methane and ethane be can be good in surge flask and hydrate generate and characterization apparatus constitutes cavity the inside mixing.
5) supercharging.As previously mentioned, supercharging is optional step, and this mainly is in the use of storage pressure deficiency.When storage pressure was not enough to provide the required pressure of experiment, first shut-off valve 31 made gas directly be transported to the supercharging module from inflator module along pipeline, can realize High-Voltage Experimentation in 200 MPas by the supercharging module then.Particularly, gas through inflator module at first enters prime filtrator 28, flow into hydrate and generate and characterization apparatus 33 through two-stage supercharger 29, high pressure filter 30, valve 32 backs then, determine the pressure that experiment is required by tensimeter 22 and pressure transducer 23.Can reach pure H by the gaseous tension after the supercharging of supercharging module
2Hydrate generates pressure, for research storage hydrogen hydrate provides sound assurance.
6) temperature control.By the temperature difference in control bath temperature and hydrate generation and the characterization apparatus, the realization hydrate generated, decomposes and the accuracy control over temperature that balances each other after hydrate generation and characterization apparatus 33 inflations were finished, and accuracy of temperature control is positive and negative 0.1 degree.Temperature is set to the required temperature of experiment.
7) synthetic.Through after the above operation, hydrate generates and characterization apparatus pressure and temperature has at this moment reached the experiment setting value, begins every experiment of hydrate sample immediately.
8) exhaust.After treating that experiment is finished, open valve 31,26, unreacted gas is discharged by vent port 37.
Below only schematically describe an embodiment that can realize the object of the invention, in other embodiments of the invention, the process of mixing gas by surge tank also can be by allowing the mixed gas of gas generation manufacturer production corresponding proportion substitute in advance.In addition, two-stage supercharger can use the solid pressure transmission, is placed on the pressing accessory such as hydrate generation and characterization apparatus, and hydrate generates and the rising of the volume realization pressure of characterization apparatus by changing.Need to prove, owing to the experimental apparatus such as vacuum pump, tensimeter, counterbalance valve, supercharger, filtrator etc. is those skilled in the art's common part, therefore in the present invention, they are not done more detailed description.In addition, it will be understood by those skilled in the art that, when some instruments that use the present invention to mention, need be used other supporting parts, should use UHV (ultra-high voltage) pipeline and needle-valve when for example using supercharger, need gas pressure reducer when using gas cylinder, need pipeline etc. during transport gas, because these are known in the art, do not repeat them here.
Although the present invention is made specific descriptions with reference to the above embodiments, but for the person of ordinary skill of the art, should be appreciated that and to make amendment based on content disclosed by the invention within spirit of the present invention and the scope or improve not breaking away from, these modifications and improving all within spirit of the present invention and scope.
Claims (10)
1. a new forms of energy hydrate composite experiment high-tension unit comprises inflator module, hydrate generation and characterization apparatus, temperature control modules and vacuum module, wherein,
Inflator module generates with hydrate and characterization apparatus is connected, for it provides one or more reacting gas;
Vacuum module generates with inflator module and hydrate and characterization apparatus is connected, in order to vacuumize;
Temperature control modules generates with hydrate and is connected with characterization apparatus, and hydrate generates and the temperature of characterization apparatus to measure and to control.
2. device as claimed in claim 1 is characterized in that, also comprises the supercharging module, and one or more reacting gas that provided by inflator module this supercharging module of flowing through arrives hydrate and generates and characterization apparatus.
3. device as claimed in claim 2 is characterized in that, described supercharging module comprises filtrator and two-stage supercharger.
4. device as claimed in claim 1 is characterized in that, described hydrate generates and bottom surface and the side of characterization apparatus are provided with the optical window that generates, decomposes for the in-situ monitoring hydrate.
5. device as claimed in claim 4 is characterized in that, by optical fiber Raman signal is inserted described optical window, is used for the generation of real-time monitored hydrate, decomposition kinetics and feature such as balance each other.
6. device as claimed in claim 1 is characterized in that, described inflator module comprises gas cylinder, the mass flowmeter that is connected with gas in the gas cylinder.
7. device as claimed in claim 1 is characterized in that, described inflator module also comprises surge tank, is used for multiple gases is mixed.
8. device as claimed in claim 1 is characterized in that, described temperature control modules comprises water-bath or air bath, and temperature sensor.
9. device as claimed in claim 8, it is characterized in that, described temperature controller comprises two kinds, a kind of being arranged in hydrate generation and the characterization apparatus, be used for measuring the internal temperature of hydrate generation and characterization apparatus, another kind is arranged in the water-bath, is used for measuring the external temperature of hydrate generation and characterization apparatus.
10. as each described device among the claim 1-9, it is characterized in that, also comprise with hydrate generating the data acquisition module that links to each other with characterization apparatus, be used for gathering temperature and the pressure data of hydrate generation and characterization apparatus.
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Cited By (2)
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| CN104549050A (en) * | 2014-12-25 | 2015-04-29 | 中国科学院深圳先进技术研究院 | Hydrogen aqueous solution preparation device and preparation method of hydrogen aqueous solution |
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Application publication date: 20130821 |