CN102495090A - Device and method for low-temperature high-pressure nuclear magnetic resonance imaging of natural gas hydrate - Google Patents
Device and method for low-temperature high-pressure nuclear magnetic resonance imaging of natural gas hydrate Download PDFInfo
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- CN102495090A CN102495090A CN2011103800503A CN201110380050A CN102495090A CN 102495090 A CN102495090 A CN 102495090A CN 2011103800503 A CN2011103800503 A CN 2011103800503A CN 201110380050 A CN201110380050 A CN 201110380050A CN 102495090 A CN102495090 A CN 102495090A
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Abstract
The invention discloses a device and a method for low-temperature high-pressure nuclear magnetic resonance imaging of a natural gas hydrate, and belongs to the field of basic physical property research of natural gas hydrates and exploitation technologies of hydrates. The device provided by the invention comprises end covers, an inner pipe, a vacuum outer pipe, a circulating fluid inlet, a circulating fluid outlet, sealing rings, filter screens and heads. The heads and the inner pipe compose an enclosed space. The enclosed space is a test area of a nuclear magnetic resonance imaging system. The vacuum outer pipe, the inner pipe and the end covers compose a space. The space is utilized for realizing reaction temperature control through circulating fluid circulation. All the parts of the device provided by the invention are prepared from a non-metallic material of polyamide-imide except the filter screens and the sealing rings. The device provided by the invention is vertically put into an imaging probe of a nuclear magnetic resonance imaging instrument, wherein design pressure is in a range of 0 to 40MPa and a design temperature is in a range of -20 to 180 DEG C. Through the device and the method, the research on natural gas hydrate generation and decomposition characteristics under multiple deposition conditions is realized. The device adopts a small amount of a magnetic material, has high pressure resistance, does not produce any influence on a nuclear magnetic resonance system, has a compact structure and can be used conveniently.
Description
Technical field
The present invention relates to a kind of gas hydrate cryogenic high pressure NMR imaging device and method, belong to gas hydrate basis rerum natura research and hydrate production practice technical field.
Background technology
Gas hydrate have been subjected to worldwide strong interest as new forms of energy.Simulation and experimental study to gas hydrate in the worldwide extensively launch.Because gas hydrate mainly are distributed in frozen soil and seabed, the cost of field research is very big, and research now mainly is to study at the state that the true gas hydrate of laboratory simulation are hidden.
To experimental study, its research method mainly contains tradition, optics, ultrasonic, electricity, CT and nmr imaging technique.Wherein conventional art is exactly that the Direct observation gas hydrate generate and decomposition, and cost is lower, but can only do qualitative analysis, and the data that obtain are inaccurate; Optical research mainly is to utilize logical light rate to change or optical photography is judged the generation and the decomposition of hydrate, and the method than higher, needs withstand voltagely and transparent to the requirement of agitated reactor, also needs response matrix transparent simultaneously; Ultrasonic technique is exactly the parameters,acoustic according to actual measurement; Like the velocity of sound, frequency, decay or the like; Reflect the various physical property infomations (factor of porosity, saturation degree, permeability or the like) in the gas hydrate Tibetan, but this kind method can not be observed the generation and the decomposition of hydrate intuitively; Electroporation is that some electrology characteristics through the detection reaction medium are (like resistance; Specific inductive capacity etc.) generation and the decomposition of hydrate judged in variation; The method is very high to the sample requirement of hydrate, and the not perfect hydrate that can only qualitatively judge of the method generate to decompose, can't quantitative measurment; The CT technology is exactly to utilize X ray that the certain thickness aspect of sample is scanned; Because gas, water, hydrate, ice are different to the absorptivity of X ray with porous medium; Measuring the generation of hydrate decomposes; But the CT technology can only be carried out two-dimensional scan to sample, and because porous medium is also formed images, and has a strong impact on so porous medium causes the observation of gas hydrate; Nmr imaging technique (MRI) is a newer research method; Be by atomic nucleus with magnetic distance under the high-intensity magnetic field effect, can absorb the electromagnetic radiation of suitable frequency, and nuclear chemical environment is different in the different molecular; To have different resonant frequency; Produce different resonance spectrums, thereby intuitively measure the various characteristics (comprising factor of porosity, saturation degree, permeability, field of flow, temperature field etc.) of gas hydrate, the method is can carry out quantitative three-dimensional visualization to sample interior to measure; The character that can accurately reflect various fluids in the porous medium; Get rid of the influence of medium skeleton, but the agitated reactor of NMR imaging is required than higher, need no magnetic, high pressure resistant and certain operating temperature range arranged.
In order to overcome the various deficiencies of existing method of testing; The present invention provides a kind of gas hydrate cryogenic high pressure NMR imaging device; This device can conveniently utilize nmr imaging technique gas hydrate to be carried out the PHYSICAL MODELING OF IN of three-dimensional visualization; The test pattern that obtains can carry out quantitative test, can obtain the parameters such as permeability, saturation degree, the field of flow when generation is decomposed, temperature field of gas hydrate in factor of porosity and the porous medium of porous medium.
Summary of the invention
The invention provides a kind of gas hydrate cryogenic high pressure NMR imaging device and method; This device is vertically put into the imaging probe of NMR imaging instrument, and the hydrate that can carry out under the condition of the multiple heavy Tibetan of gas hydrate generates resolution characteristic research; The magnetic material that this device uses is few and high pressure resistant, NMR system had no effect, and compact conformation, easy to use.
The technical scheme that technical solution problem of the present invention is adopted is:
Gas hydrate cryogenic high pressure NMR imaging device comprises end cap, interior pipe, vacuum outer tube, circulating fluid import and export, O-ring seal, filter screen, end socket.Upper and lower two end sockets and interior pipe have been formed the space of a sealing, and end socket has O-ring seal, and ability and interior pipe effectively seal, and the seal cavity of formation is the test zone of MRI system; This test zone can add the material that various participation gas hydrate generate, like water, gas, solution and porous medium etc.; Porous medium is meant materials such as beaded glass, silica sand or clay; Upper and lower two end caps and interior pipe pass through the screw thread strong bonded, and push down the two ends end socket, and pipe can bear high pressure in making like this; The end socket upper/lower terminal all is provided with filter screen, can effectively intercept moving of various interpolation solids; The space that vacuum outer tube, interior pipe and two ends end cap are formed is used for circulation fluid circulates and controls temperature of reaction, and circulation gets into from the circulating fluid import of lower end, flows out from the circulating fluid outlet of upper end; The vacuum outer tube is to select vacuum design can effectively intercept circulating fluid to managing the outer heat conduction of carrying out;
Except that rubber ring and filter screen, all the nonmetallic materials polyamide-imides material by no magnetic forms.
Said gas hydrate cryogenic high pressure NMR imaging device is after the gas hydrate reaction desired substance of packing into; Put into MRI system; Satisfy reaction conditions through controlling its temperature, pressure; Utilize NMR imaging device to detect simultaneously, and image quantitative analysis is obtained factor of porosity, data such as the saturation degree of gas hydrate and growth structure, the field of flow when generating decomposition and temperature field.
The invention has the beneficial effects as follows; This gas hydrate cryogenic high pressure NMR imaging device is packed into after the reaction desired substance, controls the temperature and pressure of total system through the temperature, pressure control system, to satisfy the working condition of gas hydrate; And put into MRI system and carry out quantitative measurment; Can obtain porous medium factor of porosity, permeability, the saturation degree of gas hydrate, and data such as field of flow when generate decomposing and temperature field.This cryogenic high pressure NMR imaging device design pressure is 0-40Mpa, design temperature is-20-180 ℃, can fully satisfy the environmental baseline under the condition of the various heavy Tibetan of gas hydrate; Minimum serviceability temperature is 10 ℃ because the MRI system coil is popped one's head in; So in order to prevent the normal use of NMR imaging device; Outer tube at simulation porous medium device adopts the design of vacuum interlayer; Good obstruct the heat conduction between device outer wall and the nuclear-magnetism coil coil probe, reach good effect of heat insulation, protection is popped one's head in; A complete set of simulation porous medium device is processed with the polyamide-imides material, no magnetic and satisfy the requirement of high pressure, and compact conformation, easy to use.
Description of drawings
Below in conjunction with accompanying drawing and embodiment the present invention is further specified.
Fig. 1 is a simulation porous medium structure drawing of device synoptic diagram.
Fig. 2 is the B-B sectional structure chart of Fig. 3.
Fig. 3 is the A-A sectional structure chart of Fig. 1.
1 upper cover among the figure; The outlet of 2 circulating fluid; 3 upper end end caps; 4 upper end filter screens; 5 vacuum outer tubes; Pipe in 6; 7 reactants; 8 lower end filter screens; 9 O-ring seals; 10 low heads; 11 lower end end caps; 12 circulating fluid imports.
Embodiment
Fig. 1,2,3 show a kind of gas hydrate high pressure low temperature NMR imaging device.This device adopts two end sockets 1,9 and interior pipe 6 to form the space of a sealing; End socket has O-ring seal 9; Ability and interior pipe 6 carry out effective seal; Add the various reactants 7 such as water, gas, solution and porous medium that various participation gas hydrate generate; On end socket, be provided with upper filter screen 4, lower filter screen 8 and can effectively intercept moving of various interpolation solids; The inside thread of upper end cover 3, bottom end cover 11 and interior pipe 6 strong bonded; And push down upper cover 1, low head 10; Pipe can bear high pressure in making like this; The space that vacuum jacket 6, interior pipe 5, upper end cover 3, bottom end cover 11 formed is used for circulation fluid and circulates and control temperature of reaction; Circulation fluid gets into from the circulating fluid import 12 of lower end; Flow out from the circulating fluid outlet 2 of upper end; Circulation fluid gateway 2,12 respectively symmetry be provided with alternate enclosure opening; As think the temperature of more accurate Control Circulation liquid; Can insert temperature sensor in the alternate enclosure opening position and measure temperature.
Utilize the step of above-mentioned gas hydrate high pressure low temperature NMR imaging device following:
The first step; Accomplish the preparation of simulation porous medium.Open upper end end cap 3 and upper cover 1, inwardly manage and add required beaded glass, silica sand or the clay of setting of concrete operating mode in 6, compacting guarantees that the required gas of reaction, water or solution still can keep stable after injecting; Refill upper end end cap 3 beyond the Great Wall behind the upper cover 1, screw; The space of the full filler of the filling of being formed between two end sockets and the interior pipe is as the simulation porous medium.
Second step; With this device MRI system of packing into.In pipe 6, vacuum jacket 5 and up and down the space formed of two end cap be used for flowing of circulating fluid; Circulating fluid import 12 connects the outlet of constant temperature circulation groove; The circulating fluid outlet connects the inlet of constant temperature circulation groove; Form a circulation and control interior pipe temperature; Upper cover 1, low head 10 external pipelines provide reaction required reactant; Like gas, water or solution etc., be fixed at last within the imaging probe of NMR imaging instrument.
The 3rd step; Carry out gas hydrate and generate decomposition.Utilizing vacuum pump will install interior pipe earlier vacuumizes; Utilize injection pump to inject the required reactant of reaction again; Utilize back pressure system to control the pressure in the interior pipe 6, reach setup pressure value; The temperature of control constant temperature circulation groove satisfies gas hydrate and generates the needs that decompose; Utilize NMR imaging instrument that whole gas hydrate are generated decomposable process and carry out the visual quantitative test of in-situ three-dimensional.
Claims (5)
1. gas hydrate NMR imaging device, this NMR imaging device comprises end cap, interior pipe, vacuum outer tube, circulating fluid import and export, O-ring seal, filter screen, end socket; It is characterized in that upper cover, low head and interior pipe have been formed the space of a sealing, end socket has O-ring seal, and the seal cavity of formation is the test zone of MRI system; This test zone adds the material that various participation gas hydrate generate; Upper end cover, bottom end cover and interior pipe pass through the screw thread strong bonded, and push down the two ends end socket; End socket all is provided with filter screen in two ends up and down; The space that vacuum outer tube, interior pipe and two ends end cap are formed is used for circulation fluid circulates and controls temperature of reaction, and circulation gets into from the circulating fluid import of lower end, flows out from the circulating fluid outlet of upper end.
2. a kind of gas hydrate NMR imaging device according to claim 1 is characterized in that, except that rubber ring and filter screen, all the nonmetallic materials polyamide-imides material by no magnetic forms.
3. a kind of gas hydrate NMR imaging device according to claim 1 is characterized in that, described test zone adds the material that various participation gas hydrate generate, and comprises water, gas, solution and porous medium.
4. a kind of gas hydrate NMR imaging device according to claim 3 is characterized in that described porous medium is meant beaded glass, silica sand or clay.
5. utilize the method for the arbitrary said gas hydrate NMR imaging device of claim 1-5, it is characterized in that following steps,
The first step; Accomplish the preparation of simulation porous medium: open upper end end cap and upper cover, inwardly add the required material of setting of concrete operating mode in the pipe, guarantee that the required gas of reaction, water or solution still can keep stable after injecting; Refill the upper end end cap beyond the Great Wall behind the upper cover, screw; The space of the full filler of the filling of being formed between two end sockets and the interior pipe is as the simulation porous medium;
Second step; With this device MRI system of packing into: interior pipe, vacuum jacket and up and down the space formed of two end cap be used for flowing of circulating fluid; The circulating fluid import connects the outlet of constant temperature circulation groove; The circulating fluid outlet connects the inlet of constant temperature circulation groove; Form a circulation and control interior pipe temperature; Upper cover, the external pipeline of low head provide reaction required reactant, are fixed at last within the imaging probe of NMR imaging instrument;
The 3rd step; Carry out gas hydrate and generate decomposition: utilize vacuum pump will install interior pipe earlier and vacuumize; Utilize injection pump to inject the required reactant of reaction again; Utilize back pressure system to control the pressure in the interior pipe, reach setup pressure value; The temperature of control constant temperature circulation groove satisfies gas hydrate and generates the needs that decompose; Utilize NMR imaging instrument that whole gas hydrate are generated decomposable process and carry out the visual quantitative test of in-situ three-dimensional.
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| CN104390902A (en) * | 2014-11-20 | 2015-03-04 | 大连理工大学 | Method for analyzing pore distribution of sediment by virtue of saturation change of gas hydrate |
| CN104677806A (en) * | 2015-03-24 | 2015-06-03 | 苏州纽迈电子科技有限公司 | Nuclear magnetic resonance low-temperature pore analysis system |
| CN105659074A (en) * | 2013-09-05 | 2016-06-08 | 沙特阿拉伯石油公司 | Tri-axial NMR test instrument |
| WO2017028161A1 (en) * | 2015-08-17 | 2017-02-23 | Irock Technologies Co., Ltd | Nmr anaylysis system and method for porous media |
| CN106896212A (en) * | 2017-02-22 | 2017-06-27 | 中国石油大学(华东) | The device of monitoring deepwater drilling liquid invasion procedure hydrate reservoir physical property change |
| CN107807143A (en) * | 2017-11-30 | 2018-03-16 | 青岛海洋地质研究所 | The special low-field nuclear magnetic resonance Multi probe quantitative testing system of hydrate and method |
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| CN109374489A (en) * | 2018-08-21 | 2019-02-22 | 中国地质大学（武汉） | The hydrate sediment NMR relaxation signals amount caliberating device and method of joint X-CT technology |
| CN109668916A (en) * | 2018-12-11 | 2019-04-23 | 大连理工大学 | A kind of hydrate sediment CT Triaxial tester |
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| CN111289553A (en) * | 2020-03-05 | 2020-06-16 | 青岛海洋地质研究所 | Device and method for analyzing mechanical properties of hydrate sediments based on low-field nuclear magnetic analysis |
| CN111589393A (en) * | 2020-05-26 | 2020-08-28 | 中国科学院西北生态环境资源研究院 | Natural gas hydrate experiment reaction kettle device suitable for low-field nuclear magnetic resonance |
| CN112611778A (en) * | 2020-12-24 | 2021-04-06 | 广州海洋地质调查局 | Nuclear magnetic resonance system for natural gas hydrate forming and decomposing process |
| CN115201246A (en) * | 2022-07-29 | 2022-10-18 | 青岛海洋地质研究所 | Low-temperature control device and experiment method for hydrate decomposition nuclear magnetic resonance experiment |
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| CN105659074B (en) * | 2013-09-05 | 2018-12-18 | 沙特阿拉伯石油公司 | Three axis nuclear magnetic resonance test equipments |
| CN104390902A (en) * | 2014-11-20 | 2015-03-04 | 大连理工大学 | Method for analyzing pore distribution of sediment by virtue of saturation change of gas hydrate |
| CN104677806A (en) * | 2015-03-24 | 2015-06-03 | 苏州纽迈电子科技有限公司 | Nuclear magnetic resonance low-temperature pore analysis system |
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Application publication date: 20120613 |