CN105424734A - Low-temperature high-pressure control device for observing aquo-complex generation and decomposition characteristics through X-ray CT device - Google Patents
Low-temperature high-pressure control device for observing aquo-complex generation and decomposition characteristics through X-ray CT device Download PDFInfo
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Abstract
The invention relates to a low-temperature high-pressure control device for observing aquo-complex generation and decomposition characteristics through an X-ray CT device, and belongs to the field of oil and gas production scientific research apparatuses. A reaction still has design pressure of 0-10 MPa and design temperature of 268-288 K, and the temperature and pressure conditions of aquo-complex generation and stable existence are met. The temperature of the reaction still is controlled through the upper end and the lower end of a semiconductor refrigerating element, noise does not exist, the acting speed is high, reliability is high, and operation is convenient. The reaction still is composed of an inner pipe and an outer pipe, wherein the inner pipe is made from titanium alloy and is mainly used for heat conduction, and the outer pipe is made from polyimide belonging to a low-heat-conductivity material and is mainly used for heat preservation and pressure preservation; according to the characteristics, the heat conduction and the heat preservation and pressure preservation are controlled independently and can be more easily controlled in the terms of engineering. The low-temperature high-pressure control device can be put on a carrying table of the CT device and generate aquo-complex in situ; through the three-dimensional imaging of the CT device, the generation and decomposition characteristics of aquo-complex can be visually studied.
Description
Technical field
The present invention relates to a kind of for the generation of X ray CT equipment observation water compound and the cryogenic high pressure control device of resolution characteristic, belong to oil-gas mining scientific research apparatus field.
Background technology
Along with the consumption of conventional gas and oil resource, human development will face the exhaustion of hydrocarbon resources, and global economic development will be faced with formidable challenges, and people start to explore new fungible energy source resource in the world.Since the nineties in 20th century, countries in the world have found a large amount of Gas Hydrates successively, according to statistics, organic C storage in Gas Hydrate accounts for the over half of overall organic carbon resource on the earth, is about the twice of institute's carbon content summation in all fossil fuel coals, oil and natural gas.Therefore, as the substitute energy in a kind of future, Gas Hydrate resource has great attractive force undoubtedly, and the understanding of people to hydrate resource is urgently deepened, and has started the upsurge of natural gas hydrate resources research.On the other hand, along with oil-gas mining turns to deep water sea area gradually, in oil gas pipeline, hydrate generates the blocking caused, and manifold pressure is raised and even causes pipeline explosion, bring huge economic loss and potential safety hazard to commercial production, cause showing great attention to of petroleum industry.To the generation of gas hydrate and the research of resolution characteristic, become a new problem.
Generate hydrate at present and the research of resolution characteristic, large volume carries out in a kettle. mostly, and wherein the overwhelming majority is non-visual, and namely camera bellows is tested.In the later stage, researcher, in order to explore generation and the resolution characteristic of hydrate further, reactor adds visual form, but does not reach real-time monitored monitoring completely.Along with further development, NMR imaging, Raman spectrum etc. are also introduced in this field, but these equipment all cannot carry out three-dimensional imaging to hydrate form.X ray CT equipment is as a kind of visualization tool, and by tomoscan, three-dimensional imaging, has at industrial circles such as defects detection, dimensional measurement, structure analyses and apply extremely widely.The sensitivity that X ray CT equipment is high and resolution, differentiated by density, can differentiate water outlet, hydrate and gas phase clearly, can be used for observing that hydrate generates and decomposable process, thus the generation of research hydrate and resolution characteristic.
Due to the harsh conditions of hydrate stable existence cryogenic high pressure, make to be difficult to in-situ preparation hydrate sample on CT equipment, in order to address this problem, the present invention devises a set of reaction unit that can be used for X ray CT imaging, generates and resolution characteristic for visual research hydrate.
Summary of the invention
In order to generation and the resolution characteristic of visual research hydrate, the present invention devises a set of reaction unit that can be used for the imaging of X ray CT equipment.This device can meet gas hydrate and generate necessary high pressure low temperature condition, can realize the in-situ preparation of hydrate on CT equipment, and adopts the three-dimensional imaging function of CT equipment to catch the change of form in the generation of hydrate and decomposable process in real time.The invention of this device has great importance for the generation of visual research hydrate and resolution characteristic.
Technical scheme of the present invention is:
Generate the cryogenic high pressure control device with resolution characteristic for X ray CT equipment observation water compound, this cryogenic high pressure control device comprises reactor 19, semiconductor refrigeration system, air feed pressure charging system, CT imaging system and data acquisition system (DAS);
Described reactor 19 adopts inside and outside double-layer sleeve structure, heat conduction and pressurize is controlled respectively; Reactor 19 is movably connected to form by upper end cover 6, bottom end cover 13, interior pipe 10 and outer tube 11, is sealed by O RunddichtringO 7; The interior pipe 10 of reactor adopts titanium alloy material, is conducive to the transmission of heat on the one hand, can be used for the three-dimensional imaging of CT equipment on the other hand, which is provided with pressure compensation opening 9, make pipe 10 in reactor not bear pressure by pressure compensation opening 9; The outer tube 11 of reactor adopts polyimide material, belong to low Heat Conduction Material, play the effect of heat-insulation pressure keeping, during use, reaction liquid is filled in pipe 10 in reactor, Sandwich filling gas between the interior pipe 10 of reactor and the outer tube 11 of reactor, both keep the pressure in interlayer and reactor in pipe 10 to keep balance by the pressure compensation opening 9 of interior pipe; Upper end cover 6 is provided with air intake opening 5, and bottom end cover 13 is provided with inlet 14, and upper end cover 6 and bottom end cover 13 all adopt titanium alloy material; Upper end cover 6 is connected semiconductor refrigeration system with bottom end cover 13, carries out refrigeration temperature control to reactor 19 body;
Described semiconductor refrigeration system comprises semiconductor refrigerating hot junction 1, metallic conductor 2, N-type and P-type semiconductor 3 and semiconductor refrigerating cold junction 4, two ends semiconductor refrigerating is adopted to reactor 19, many groups N-type is connected by metallic conductor 2 with P-type semiconductor 3, semiconductor refrigerating cold junction 4 is connected with bottom end cover 13 with the upper end cover 6 of reactor 19, reactor 19 is freezed, and carrying out heat exchange by semiconductor refrigerating hot junction 1 and surrounding medium, the power of semiconductor refrigeration system carries out regulable control by refrigerating system circuit 18; Thermopair 8 is arranged at reactor 19 upper end cover 6, and extend into pipe 10 pressure compensation opening 9 upper limb in reactor 19, for monitoring the temperature in reactor 19;
Described air feed pressure charging system comprises flowmeter 20, supercharge pump 21, vacuum pump 22, pressure transducer 23, gas cylinder 24 syringe pump 27 and hopper 28; Air intake opening 5 Bonding pressure sensor 23, is connected vacuum pump 22 by valve, is connected successively by flowmeter 20 with supercharge pump 21 and gas cylinder 24; Inlet 14 is connected with syringe pump 27 and hopper 28;
Described CT imaging system comprises the outer tube 11 that reactor aimed at by CT imaging device 26, CT imaging device 26, is used for carrying out three-dimensional imaging to the metamorphosis in hydrate generation and decomposable process;
Described data acquisition system (DAS) 17 is the temperature, pressure and the flow signal that thermopair 8, pressure transducer 23 and flowmeter 20 are collected, carries out Real-time Collection and is transferred to computing machine 25.
Described cryogenic high pressure control device, described N-type and P-type semiconductor 3 adopt many group N-types and P-type semiconductor to be in series, to reach required refrigeration.
Cryogenic high pressure control device described in use realizes X ray CT equipment observation water compound and generates the method with resolution characteristic, and step is as follows:
The first step, assembling cryogenic high pressure control device, pipeline connects and sealing, and carries out debugging detection;
Second step, pressure testing and scavenging: the gas injecting certain pressure in reactor 19, carry out pressure testing to reactor 19, guarantees reactor 19 leakproofness, carries out inflation/deflation repeatedly to reactor 19, gets rid of the air in reactor 19;
3rd step, temperature control pressurize and data acquisition: start semiconductor refrigeration system, control at design temperature by reactor 19, and water filling gas injection in reactor 19, until reach set pressure; Meanwhile, data acquisition system (DAS) 17 starts to carry out Real-time Collection and be transferred to computing machine 25 carrying out inventory analysis to the gas flow of the temperature, pressure signal in reactor 19 and input;
4th step, hydrate generates and scanning imagery: cooling generates hydrate, and CT imaging device 26 pairs of generative processes carry out the change that the visual hydrate of scanning imagery generates form simultaneously;
5th step, decomposition of hydrate: in question response still 19 after temperature, pressure signal stabilization, hydrate has generated, and adopt step-down or type of heating to decompose hydrate, in whole process, the metamorphosis of hydrate is all shown by CT imaging device 26 three-dimensional imaging.
The invention has the beneficial effects as follows: this reaction unit being used for the imaging of X ray CT equipment mainly comprises a reactor, semiconductor refrigeration system, air feed pressure charging system, CT imaging system, data acquisition system (DAS).Reactor is used for hydrate and generates decomposition, semiconductor refrigeration system and air feed pressure charging system accurately can control the temperature and pressure in reactor, meet the condition that hydrate generates, CT imaging device is used for the generation of visual hydrate and decomposable process, and data acquisition system (DAS) can Real-time Collection temperature, pressure and flow signal be transferred to computing machine analysis.Its advantage is:
1) reactor can bear the pressure of 0-10MPa and the temperature of 268-288K, meets hydrate and generates and the temperature, pressure condition of stable existence;
2) in reactor, pipe is mainly used in heat conduction temperature control, and outer tube is mainly used in keeping reacting kettle inner pressure, and temperature control and pressurize separately, under the prerequisite meeting CT imaging, can control the environment of cryogenic high pressure, can realize the in-situ preparation of hydrate at CT equipment;
3) reactor two end cap and interior pipe adopt titanium alloy material, while alleviating reactor weight, can be good at the transmission ensureing heat, reach good refrigeration;
4) reactor outer tube adopts polyamides ethamine material, under the prerequisite ensureing reacting kettle inner pressure, also can play the effect of adiabatic heat-insulation;
5) reactor adopts semiconductor two ends refrigeration, noiseless during work, and speed of action is fast, and reliability is high, long service life, easy to adjust, regulates refrigerating capacity by regulating size of current;
6) adopt semiconductor refrigerating technology refrigeration, there is no the disturbance of circulation fluid, little to CT Imaging;
7) this system can be used in X ray CT equipment, and can in-situ preparation hydrate, and visual hydrate generates the change with form in decomposable process.
Accompanying drawing explanation
Fig. 1 is a kind of for the principle of work block diagram of X ray CT equipment observation water compound generation with the cryogenic high pressure control device of resolution characteristic.
Fig. 2 is a kind of for the reaction kettle body structural drawing of X ray CT equipment observation water compound generation with the cryogenic high pressure control device of resolution characteristic.
Fig. 3 is a kind of for the system diagram of X ray CT equipment observation water compound generation with the cryogenic high pressure control device of resolution characteristic.
In figure: 1 semiconductor refrigerating hot junction; 2 metallic conductors; 3N type and P-type semiconductor; 4 semiconductor refrigerating cold junctions; 5 air intake openings; 6 upper end covers; 7O RunddichtringO; 8 thermopairs; 9 pressure compensation openings; Pipe in 10; 11 outer tubes; 12 rubber washers; 13 bottom end covers; 14 inlets; 15 semiconductor refrigerating wires; 16 reactor bases; 17 data acquisition system (DAS)s; 18 refrigerating system circuit; 19 reactors; 20 flowmeters; 21 supercharge pumps; 22 vacuum pumps; 23 pressure transducers; 24 gas cylinders; 25 computing machines; 26CT imaging device; 27 syringe pumps; 28 hoppers.
Embodiment
Below in conjunction with accompanying drawing and technical scheme, further illustrate the specific embodiment of the present invention.
Fig. 1-3 illustrates a kind of for the cryogenic high pressure reaction unit of X ray CT equipment observation water compound generation with resolution characteristic.This device is overall by two end caps, and two semiconductor refrigerating unit and inner and outer sleeves are formed.End cap and outer tube form high pressure resistant reactor, outer tube plays the effect of temperature control pressurize, end cap and semiconductor refrigerating element are connected, end cap and interior effective titanium alloy make, play the effect of heat conduction temperature control, have aperture holding tube internal and external pressure balance above interior pipe, inside pipe aperture with lower part injection liquid body, remainder blanketing gas.The step carrying out studying and using based on the above device is as follows:
The first step, assembles each system.Assemble a system in order, and carry out debugging detection.
Second step, sealing and pipeline connect.By reactor end cap seal, guarantee that end cap is fastening and reactor sealing good, inlet is connected with gas supercharge pump with syringe pump respectively with air intake opening, to control the pressure in reactor.
3rd step, pressure testing and scavenging.In reactor, inject the gas of certain pressure, pressure testing is carried out to reactor, after guaranteeing that reactor leakproofness is good, inflation/deflation is repeatedly carried out to reactor, get rid of the air in reactor.
4th step, temperature control pressurize and data acquisition.Start semiconductor refrigerating element, controlled by reactor at design temperature, water filling gas injection in reactor, until reach set pressure, meanwhile, data acquisition system (DAS) starts to carry out Real-time Collection and inventory analysis to the gas flow of the temperature, pressure signal in reactor and input.
5th step, hydrate generates and scanning imagery.Cooling generates hydrate, and CT equipment carries out scanning imagery with the change of visual hydrate generation form to generative process simultaneously.
6th step, decomposition of hydrate.After question response temperature in the kettle pressure signal is stable, imply that hydrate has generated, adopt the mode of step-down or heating to decompose hydrate, in whole process, the metamorphosis of hydrate is all shown by the three-dimensional imaging of CT equipment.
7th step, collator.After treating that decomposition of hydrate completes, reactor and pipeline are cleared up, arrange experimental provision, repeat the experiment that above step can start a new round.
Claims (3)
1. one kind generates the cryogenic high pressure control device with resolution characteristic for X ray CT equipment observation water compound, it is characterized in that, this cryogenic high pressure control device comprises reactor (19), semiconductor refrigeration system, air feed pressure charging system, CT imaging system and data acquisition system (DAS);
Described reactor (19) adopts inside and outside double-layer sleeve structure, controls heat conduction and pressure retaining part respectively; Reactor (19) is movably connected to form by upper end cover (6), bottom end cover (13), interior pipe (10) and outer tube (11), is sealed by O RunddichtringO (7); The interior pipe (10) of reactor adopts titanium alloy material, which is provided with pressure compensation opening (9), makes the interior pipe (10) of reactor not bear pressure by pressure compensation opening (9); The outer tube (11) of reactor adopts polyimide material, play the effect of heat-insulation pressure keeping, during use, reaction liquid is filled in pipe (10) in reactor, Sandwich filling gas between the interior pipe (10) of reactor and the outer tube (11) of reactor, both keep the pressure equilibrium in the interior pipe (10) of interlayer and reactor by the pressure compensation opening (9) of the interior pipe (10) of reactor; Upper end cover (6) is provided with air intake opening (5), and bottom end cover (13) is provided with inlet (14), and upper end cover (6) and bottom end cover (13) all adopt titanium alloy material; Upper end cover (6) is connected semiconductor refrigeration system with bottom end cover (13), carries out refrigeration temperature control to reactor (19) body;
Described semiconductor refrigeration system comprises semiconductor refrigerating hot junction (1), metallic conductor (2), N-type and P-type semiconductor (3) and semiconductor refrigerating cold junction (4), two ends semiconductor refrigerating is adopted to reactor (19), many groups N-type is connected by metallic conductor (2) with P-type semiconductor (3), semiconductor refrigerating cold junction (4) is connected with bottom end cover (13) with the upper end cover (6) of reactor (19), reactor (19) is freezed, and carry out heat exchange by semiconductor refrigerating hot junction (1) and surrounding medium, the power of semiconductor refrigeration system carries out regulable control by refrigerating system circuit (18), thermopair (8) is arranged at reactor (19) upper end cover (6), and extend into interior pipe (10) pressure compensation opening (9) upper limb of reactor (19), for monitoring the temperature in reactor (19),
Described air feed pressure charging system comprises flowmeter (20), supercharge pump (21), vacuum pump (22), pressure transducer (23), gas cylinder (24), syringe pump (27) and hopper (28); Air intake opening (5) Bonding pressure sensor (23), connects vacuum pump (22) by valve, is connected successively by flowmeter (20) with supercharge pump (21) and gas cylinder (24); Inlet (14) is connected with syringe pump (27) and hopper (28);
Described CT imaging system comprises CT imaging device (26), and the outer tube (11) of reactor aimed at by CT imaging device (26), is used for carrying out three-dimensional imaging to the metamorphosis in hydrate generation and decomposable process;
Described data acquisition system (DAS) (17) is the temperature, pressure and the flow signal that thermopair (8), pressure transducer (23) and flowmeter (20) are collected, carries out Real-time Collection and is transferred to computing machine (25).
2. cryogenic high pressure control device according to claim 1, is characterized in that, described N-type and P-type semiconductor (3) adopt many group N-types and P-type semiconductor to be in series.
3. realize X ray CT equipment observation water compound with the cryogenic high pressure control device described in claim 1 or 2 and generate the method with resolution characteristic, it is characterized in that, step is as follows:
The first step, assembling cryogenic high pressure control device, pipeline connects and sealing, and carries out debugging detection;
Second step, pressure testing: to reactor (19) interior nitrogen injection to set pressure, carries out pressure testing to reactor (19), guarantees reactor (19) leakproofness;
3rd step, scavenging: adopt methane gas, carry out inflation/deflation repeatedly to reactor (19), gets rid of air/nitrogen remaining in reactor (19);
4th step, temperature control pressurize and data acquisition: start semiconductor refrigeration system, control at design temperature by reactor (19), to the interior water filling gas injection of reactor (19), until reach set pressure; Meanwhile, data acquisition system (DAS) (17) starts to carry out Real-time Collection and be transferred to computing machine (25) carrying out inventory analysis to the gas flow of the temperature, pressure signal in reactor (19) and input;
5th step, hydrate generates and scanning imagery: cooling generates hydrate, and CT imaging device (26) carries out to generative process the change that the visual hydrate of scanning imagery generates form simultaneously;
6th step, decomposition of hydrate: after the interior temperature, pressure signal stabilization of question response still (19), hydrate has generated, adopt step-down or type of heating to decompose hydrate, in whole process, the metamorphosis of hydrate is all shown by CT imaging device (26) three-dimensional imaging.
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