CN105424734B - A kind of cryogenic high pressure control device generated for X ray CT equipment observation water compound with resolution characteristic - Google Patents

A kind of cryogenic high pressure control device generated for X ray CT equipment observation water compound with resolution characteristic Download PDF

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CN105424734B
CN105424734B CN201610017946.8A CN201610017946A CN105424734B CN 105424734 B CN105424734 B CN 105424734B CN 201610017946 A CN201610017946 A CN 201610017946A CN 105424734 B CN105424734 B CN 105424734B
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reactor
pressure
hydrate
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generation
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CN105424734A (en
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王斌
宋永臣
赵佳飞
刘卫国
杨明军
张毅
凌铮
李洋辉
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Dalian University of Technology
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    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006—Controlling or regulating processes
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
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    • B01J19/0006—Controlling or regulating processes
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053—Details of the reactor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/04—Pressure vessels, e.g. autoclaves
    • B01J3/046—Pressure-balanced vessels
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
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    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00162—Controlling or regulating processes controlling the pressure
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    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00—Investigating materials by wave or particle radiation
    • G01N2223/30—Accessories, mechanical or electrical features
    • G01N2223/31—Accessories, mechanical or electrical features temperature control
    • G01N2223/3103—Accessories, mechanical or electrical features temperature control cooling, cryostats
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00—Investigating materials by wave or particle radiation
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    • G01N2223/639—Specific applications or type of materials material in a container

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Abstract

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.Mixer design pressure is 0 10MPa, and design temperature is 268 288K, meets the temperature, pressure condition that hydrate is generated and is stabilized.Semiconductor refrigerating element carries out temperature control by upper and lower ends to reactor, and noiseless, work fast, reliability is high, easy to operate.Reactor is made up of inside and outside two pipe fittings, and inner tube uses titanium alloy material, is mainly used in heat conduction, and outer tube uses polyimides material, belongs to low Heat Conduction Material, be mainly used in heat-insulation pressure keeping, and this characteristic controls heat conduction and heat-insulation pressure keeping respectively, is easier to realize in engineering.The covering device can be positioned over the objective table of CT equipment, and in-situ preparation hydrate, by the three-dimensional imaging of CT equipment, be capable of generation and the resolution characteristic of visual research hydrate.

Description

It is a kind of high for the generation of X ray CT equipment observation water compound and the low temperature of resolution characteristic Pressure control device
Technical field
Control and fill the present invention relates to a kind of cryogenic high pressure for the generation of X ray CT equipment observation water compound and resolution characteristic Put, belong to oil-gas mining scientific research apparatus field.
Background technology
With the consumption of conventional gas and oil resource, human development will face the exhaustion of petroleum resources, and global economic development is by face Face stern challenge, people start to explore new fungible energy source resource in the world.Since the 1990s, generation Various countries of boundary are found that substantial amounts of Gas Hydrate successively, and according to statistics, the organic C storage in Gas Hydrate accounts for More than half of overall organic carbon resource, institute's phosphorus content summation in about all fossil fuel coals, oil and natural gas on the earth Twice.Therefore, undoubtedly there is great attraction as a kind of following alternative energy source, Gas Hydrate resource, People urgently deepen to the understanding of hydrate resource, have started the upsurge of natural gas hydrate resources research.On the other hand, with Oil-gas mining is increasingly turned to deep water sea area, is blocked caused by the generation of oil gas pipeline reclaimed water compound so that manifold pressure raises very To pipeline explosion is caused, huge economic loss and potential safety hazard are brought to industrial production, has caused petroleum industry Pay high attention to.The research of generation and resolution characteristic to gas hydrates, have become a new problem.
The research with resolution characteristic is generated to hydrate at present, big volume is carried out in a kettle mostly, wherein absolutely Most of is non-visualization, i.e., camera bellows is tested.Later stage, researcher in order to further explore the generation of hydrate and resolution characteristic, On reactor plus form is visualized, but real-time monitored monitoring is not fully achieved.With further development, nuclear-magnetism into Picture, Raman spectrum etc. are also introduced into this field, but these equipment can not carry out three-dimensional imaging to hydrate form.X Ray CT apparatus passes through tomoscan, three-dimensional imaging, in defects detection, dimensional measurement, structure point as a kind of visualization tool The industrial circles such as analysis, which have, to be extremely widely applied.The high sensitivity of X ray CT equipment and resolution ratio, are differentiated by density, Water outlet, hydrate and gas phase can be clearly differentiated, can be used for observing hydrate generation and decomposable process, so as to grind Study carefully generation and the resolution characteristic of hydrate.
Because hydrate is stabilized the harsh conditions of cryogenic high pressure so that it is difficult to the in-situ preparation hydrate in CT equipment Sample, in order to solve this problem, the present invention devises a set of reaction unit available for X ray CT imaging, for visualizing Study hydrate generation and resolution characteristic.
The content of the invention
Generation and resolution characteristic for visual research hydrate, the present invention devises a set of to be set available for X ray CT The reaction unit of standby imaging.The device disclosure satisfy that high pressure low temperature condition necessary to gas hydrates generation, it is possible to achieve In-situ preparation of the hydrate in CT equipment, and the generation of the three-dimensional imaging function real-time capture hydrate of CT equipment is used with dividing The change of form in solution preocess.Generation of the invention of the device for visual research hydrate has important with resolution characteristic Meaning.
The technical scheme is that：
A kind of cryogenic high pressure control device generated for X ray CT equipment observation water compound with resolution characteristic, the low temperature High-pressure control device includes reactor 19, semiconductor refrigeration system, supply pressure charging system, CT imaging systems and data acquisition system System；
Double-layer sleeve structure inside and outside the described use of reactor 19, heat conduction is controlled respectively with pressurize；Reactor 19 is by upper End cap 6, bottom end cover 13, inner tube 10 and outer tube 11 are movably connected to form, and are sealed by O-ring seal 7；The inner tube 10 of reactor is adopted With titanium alloy material, be on the one hand advantageous to the transmission of heat, on the other hand available for CT equipment three-dimensional imaging, which is provided with pressure Balance pipe 9, the inner tube 10 for making reactor by pressure compensation opening 9 are not subject to pressure；The outer tube 11 of reactor uses polyimides Material, belong to low Heat Conduction Material, play a part of heat-insulation pressure keeping, in use, filling reaction liquid in reactor inner tube 10, react Sandwich filling gas between the inner tube 10 of kettle and the outer tube 11 of reactor, both pass through the retaining clip of pressure compensation opening 9 of inner tube Pressure in layer and reactor inner tube 10 keeps balance；Upper end cover 6 is provided with air inlet 5, and bottom end cover 13 is provided with inlet 14, upper end Lid 6 and bottom end cover 13 use titanium alloy material；Upper end cover 6 and bottom end cover 13 connect semiconductor refrigeration system, to reactor 19 Body carries out refrigeration temperature control；
Described semiconductor refrigeration system includes semiconductor refrigerating hot junction 1, metallic conductor 2, N-type and P-type semiconductor 3 and half Conductor refrigeration cold end 4, uses both ends semiconductor refrigerating, multigroup N-type and P-type semiconductor 3 pass through the phase of metallic conductor 2 to reactor 19 Even, semiconductor refrigerating cold end 4 is connected with the upper end cover 6 and bottom end cover 13 of reactor 19, reactor 19 is freezed, and passes through Semiconductor refrigerating hot junction 1 is exchanged heat with surrounding medium, and the power of semiconductor refrigeration system is carried out by refrigerating system circuit 18 Adjustment control；Thermocouple 8 is arranged at the upper end cover 6 of reactor 19, and extend into the upper limb of 19 inner tube of reactor, 10 pressure compensation opening 9, For monitoring the temperature in reactor 19；
Described supply pressure charging system includes flowmeter 20, booster pump 21, vavuum pump 22, pressure sensor 23, gas cylinder 24 Syringe pump 27 and hopper 28；Air inlet 5 connect pressure sensor 23, by valve connect vavuum pump 22, by flowmeter 20 according to It is secondary to be connected with booster pump 21 and gas cylinder 24；Inlet 14 is connected with syringe pump 27 and hopper 28；
Described CT imaging systems include CT imaging devices 26, and CT imaging devices 26 are directed at the outer tube 11 of reactor, are used for Three-dimensional imaging is carried out with the metamorphosis in decomposable process to hydrate generation；
Described data collecting system 17 be thermocouple 8, pressure sensor 23 and flowmeter 20 are collected temperature, Pressure and flow signal, gathered in real time and be transferred to computer 25.
Described cryogenic high pressure control device, described N-type and P-type semiconductor 3 use multigroup N-type and P-type semiconductor string Connection forms, to reach required refrigeration.
A kind of cryogenic high pressure control device described in realizes the generation of X ray CT equipment observation water compound and resolution characteristic Method, step are as follows：
The first step, cryogenic high pressure control device, pipeline connection and sealing are assembled, and carry out debugging detection；
Second step, pressure testing and scavenging：The gas of certain pressure is injected into reactor 19, pressure testing is carried out to reactor 19, Ensure the seal of reactor 19, inflation/deflation repeatedly is carried out to reactor 19, exclude the air in reactor 19；
3rd step, temperature control pressurize and data acquisition：Start semiconductor refrigeration system, reactor 19 is controlled in setting temperature Degree, the water filling gas injection into reactor 19, until reaching setting pressure；Meanwhile data collecting system 17 starts in reactor 19 Temperature, pressure signal and the gas flow of input gathered in real time and be transferred to computer 25 and carry out storage analysis；
4th step, hydrate generation and scanning imagery：Cooling generation hydrate, while CT imaging devices 26 are to generating process It is scanned the change of imaging visual hydrate generation form；
5th step, decomposition of hydrate：In question response kettle 19 after temperature, pressure signal stabilization, hydrate generation is completed, and is used Decompression or mode of heating decompose to hydrate, and the metamorphosis of hydrate all passes through CT imaging devices 26 in whole process Three-dimensional imaging is shown.
The beneficial effects of the invention are as follows：This be used for X ray CT equipment imaging reaction unit mainly include a reactor, Semiconductor refrigeration system, supply pressure charging system, CT imaging systems, data collecting system.Reactor is used for hydrate generation and decomposed, Semiconductor refrigeration system can accurately control the temperature and pressure in reactor with supply pressure charging system, meet hydrate generation Condition, CT imaging devices are used for generation and the decomposable process for visualizing hydrate, and data collecting system being capable of real-time collecting temperature Pressure and flow signal are simultaneously transferred to computer and analyzed.Its advantage is：
1) reactor can bear 0-10MPa pressure and 268-288K temperature, meet that hydrate is generated and stably deposited Temperature, pressure condition；
2) reactor inner tube is mainly used in heat conduction temperature control, and outer tube is mainly used in keeping reacting kettle inner pressure, temperature control and pressurize Separate, on the premise of CT imagings are met, the environment of cryogenic high pressure can be controlled, it is raw in the original position of CT equipment that hydrate can be achieved Into；
3) reactor two end cap and inner tube use titanium alloy material, while mitigating reactor weight, can be good at protecting Hinder the transmission of heat, reach good refrigeration；
4) reactor outer tube uses polyamides ethamine material, on the premise of reacting kettle inner pressure is ensured, can also play thermal insulation The effect of insulation；
5) reactor is freezed using semiconductor both ends, and noiseless during work, work fast, reliability is high, service life It is long, it is easy to adjust, refrigerating capacity can be adjusted by adjusting size of current；
6) freezed using semiconductor refrigerating technology, it is small to CT Imagings without the disturbance of circulation fluid；
7) system can be used in X ray CT equipment, and can be visualized hydrate generation with in-situ preparation hydrate and divided The change of form in solution preocess.
Brief description of the drawings
Fig. 1 is a kind of for the generation of X ray CT equipment observation water compound and the cryogenic high pressure control device of resolution characteristic Operation principle block diagram.
Fig. 2 is a kind of for the generation of X ray CT equipment observation water compound and the cryogenic high pressure control device of resolution characteristic Reaction kettle body structure chart.
Fig. 3 is a kind of for the generation of X ray CT equipment observation water compound and the cryogenic high pressure control device of resolution characteristic System diagram.
In figure：1 semiconductor refrigerating hot junction；2 metallic conductors；3N types and P-type semiconductor；4 semiconductor refrigerating cold ends；5 air inlets Mouthful；6 upper end covers；7O type sealing rings；8 thermocouples；9 pressure compensation openings；10 inner tubes；11 outer tubes；12 rubber washers；13 bottom end covers； 14 inlets；15 semiconductor refrigerating wires；16 reactor bases；17 data collecting systems；18 refrigerating system circuits；19 reactions Kettle；20 flowmeters；21 booster pumps；22 vavuum pumps；23 pressure sensors；24 gas cylinders；25 computers；26CT imaging devices；27 notes Penetrate pump；28 hoppers.
Embodiment
Below in conjunction with accompanying drawing and technical scheme, embodiment of the invention is further illustrated.
Fig. 1-3 illustrates a kind of for the generation of X ray CT equipment observation water compound and the cryogenic high pressure reaction of resolution characteristic Device.The device is overall to be made up of two end caps, two semiconductor refrigerating units and inner and outer sleeves.End cap is formed with outer tube High pressure resistant reactor, outer tube play a part of temperature control pressurize, and end cap is connected with semiconductor refrigerating element, end cap and interior effective titanium Alloy makes, and plays a part of heat conduction temperature control, has aperture to keep pipe internal and external pressure balance above inner tube, to inner tube aperture with bottom Dispense into liquid, remainder filling gas.The step of being studied and used based on apparatus described above is as follows：
The first step, assemble each system.A system is assembled in sequence, and carries out debugging detection.
Second step, sealing and pipeline connection.By reactor end cap seal, it is ensured that end cap fastens and reactor sealing is good It is good, inlet and air inlet are connected with syringe pump and gas booster pump respectively, to control the pressure in reactor.
3rd step, pressure testing and scavenging.The gas of certain pressure is injected into reactor, pressure testing is carried out to reactor, it is ensured that After reactor seal is good, inflation/deflation repeatedly is carried out to reactor, excludes the air in reactor.
4th step, temperature control pressurize and data acquisition.Start semiconductor refrigerating element, reactor controlled in design temperature, The water filling gas injection into reactor, until reaching setting pressure, at the same time, data collecting system starts to the temperature in reactor Pressure signal and the gas flow of input are gathered and store analysis in real time.
5th step, hydrate generation and scanning imagery.Cooling generation hydrate, while CT equipment is swept to generating process Retouch change of the imaging in the form of visualizing hydrate generation.
6th step, decomposition of hydrate.After question response temperature in the kettle pressure signal is stable, it imply that hydrate has generated Into, using decompression or heating by the way of hydrate is decomposed, the metamorphosis of hydrate all passes through in whole process CT equipment three-dimensional imaging is shown.
7th step, collator.After treating that decomposition of hydrate is completed, reactor and pipeline are cleared up, arranged real Experiment device, the experiment of a new round can be started by repeating above step.

Claims (2)

1. a kind of exist for the generation of X ray CT equipment observation water compound and the cryogenic high pressure control device of resolution characteristic, its feature In, the cryogenic high pressure control device include reactor (19), semiconductor refrigeration system, supply pressure charging system, CT imaging systems and Data collecting system；
Double-layer sleeve structure inside and outside described reactor (19) use, controls heat conduction and pressure holding function respectively；Reactor (19) by Upper end cover (6), bottom end cover (13), inner tube (10) and outer tube (11) are movably connected to form, and are sealed by O-ring seal (7)；Reaction The inner tube (10) of kettle uses titanium alloy material, which is provided with pressure compensation opening (9), makes reactor by pressure compensation opening (9) Inner tube (10) is not subject to pressure；The outer tube (11) of reactor uses polyimides material, plays a part of heat-insulation pressure keeping, uses When, the middle filling reaction liquid of reactor inner tube (10), the interlayer between the inner tube (10) of reactor and the outer tube (11) of reactor Filling gas, both are kept in the inner tube (10) of interlayer and reactor by the pressure compensation opening (9) of the inner tube (10) of reactor Pressure balance；Upper end cover (6) is provided with air inlet (5), and bottom end cover (13) is provided with inlet (14), upper end cover (6) and bottom end cover (13) titanium alloy material is used；Upper end cover (6) and bottom end cover (13) connection semiconductor refrigeration system, enter to reactor (19) body Row refrigeration temperature control；
Described semiconductor refrigeration system include semiconductor refrigerating hot junction (1), metallic conductor (2), N-type and P-type semiconductor (3) and Semiconductor refrigerating cold end (4), uses both ends semiconductor refrigerating to reactor (19), multigroup N-type and P-type semiconductor (3) from beginning to end according to It is secondary to be contacted by metallic conductor (2), semiconductor refrigerating cold end (4) and the upper end cover (6) and bottom end cover (13) phase of reactor (19) Even, reactor (19) is freezed, and exchanged heat by semiconductor refrigerating hot junction (1) with surrounding medium, semiconductor refrigerating Control is adjusted by refrigerating system circuit (18) in the power of system；Thermocouple (8) is arranged at reactor (19) upper end cover (6), and inner tube (10) pressure compensation opening (9) upper limb of reactor (19) is extend into, for monitoring the temperature in reactor (19)；
Described supply pressure charging system includes flowmeter (20), booster pump (21), vavuum pump (22), pressure sensor (23), gas Bottle (24), syringe pump (27) and hopper (28)；Air inlet (5) connection pressure sensor (23), vavuum pump is connected by valve (22), pass sequentially through flowmeter (20) and booster pump (21) is connected with gas cylinder (24)；Inlet (14) is connected with syringe pump (27) With hopper (28)；
Described CT imaging systems include CT imaging devices (26), and CT imaging devices (26) are directed at the outer tube (11) of reactor, use To carry out three-dimensional imaging with the metamorphosis in decomposable process to hydrate generation；
Described data collecting system (17) collects thermocouple (8), pressure sensor (23) and flowmeter (20) Temperature, pressure and flow signal, gathered in real time and be transferred to computer (25).
2. a kind of cryogenic high pressure control device with described in claim 1 is realized the generation of X ray CT equipment observation water compound and divided The method for solving characteristic, it is characterised in that step is as follows：
The first step, cryogenic high pressure control device, pipeline connection and sealing are assembled, and carry out debugging detection；
Second step, pressure testing：Injection nitrogen carries out pressure testing, it is ensured that anti-to setting pressure to reactor (19) in reactor (19) Answer kettle (19) seal；
3rd step, scavenging：Using methane gas, inflation/deflation repeatedly is carried out to reactor (19), excluded remaining in reactor (19) Air/nitrogen；
4th step, temperature control pressurize and data acquisition：Start semiconductor refrigeration system, reactor (19) controlled in design temperature, To the interior water filling gas injection of reactor (19), until reaching setting pressure；Meanwhile data collecting system (17) starts to reactor (19) Interior temperature, pressure signal and the gas flow of input are gathered and be transferred to computer (25) in real time carries out storage analysis；
5th step, hydrate generation and scanning imagery：Cooling generation hydrate, while CT imaging devices (26) enter to generating process The change of row scanning imagery visualization hydrate generation form；
6th step, decomposition of hydrate：After the interior temperature, pressure signal stabilization of question response kettle (19), hydrate generation is completed, using drop Pressure or mode of heating decompose to hydrate, and the metamorphosis of hydrate all passes through CT imaging devices (26) in whole process Three-dimensional imaging is shown.
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