CN105651805A - Method using nuclear magnetic resonance to measure rock porosity - Google Patents
Method using nuclear magnetic resonance to measure rock porosity Download PDFInfo
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- CN105651805A CN105651805A CN201610189194.3A CN201610189194A CN105651805A CN 105651805 A CN105651805 A CN 105651805A CN 201610189194 A CN201610189194 A CN 201610189194A CN 105651805 A CN105651805 A CN 105651805A
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- 239000011435 rock Substances 0.000 title claims abstract description 207
- 238000005481 NMR spectroscopy Methods 0.000 title claims abstract description 56
- 238000000034 method Methods 0.000 title claims abstract description 34
- 238000004090 dissolution Methods 0.000 claims abstract description 124
- 239000011148 porous material Substances 0.000 claims abstract description 119
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 79
- 238000002474 experimental method Methods 0.000 claims abstract description 32
- 229920000742 Cotton Polymers 0.000 claims description 58
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical group ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 46
- 239000004033 plastic Substances 0.000 claims description 18
- 229920003023 plastic Polymers 0.000 claims description 18
- 238000005213 imbibition Methods 0.000 claims description 17
- 239000000463 material Substances 0.000 claims description 16
- 239000002904 solvent Substances 0.000 claims description 15
- 238000005259 measurement Methods 0.000 claims description 14
- 239000005416 organic matter Substances 0.000 claims description 13
- 239000003960 organic solvent Substances 0.000 claims description 10
- 238000000944 Soxhlet extraction Methods 0.000 claims description 6
- 239000010408 film Substances 0.000 claims 1
- 239000010409 thin film Substances 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 4
- 238000010521 absorption reaction Methods 0.000 abstract 2
- 238000003754 machining Methods 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 21
- 238000003384 imaging method Methods 0.000 description 16
- 101100136062 Mycobacterium tuberculosis (strain ATCC 25618 / H37Rv) PE10 gene Proteins 0.000 description 13
- 239000000523 sample Substances 0.000 description 10
- 238000013421 nuclear magnetic resonance imaging Methods 0.000 description 7
- 238000004458 analytical method Methods 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 230000005311 nuclear magnetism Effects 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000000284 extract Substances 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- RPAJSBKBKSSMLJ-DFWYDOINSA-N (2s)-2-aminopentanedioic acid;hydrochloride Chemical compound Cl.OC(=O)[C@@H](N)CCC(O)=O RPAJSBKBKSSMLJ-DFWYDOINSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 101710089042 Demethyl-4-deoxygadusol synthase Proteins 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 108010053993 N-terminal tetrapeptide cystatin C Proteins 0.000 description 1
- WUUNPBLZLWVARQ-QAETUUGQSA-N Postin Chemical compound NC(N)=NCCC[C@@H](C(O)=O)NC(=O)[C@H](CCCCN)NC(=O)[C@@H]1CCCN1C(=O)[C@H]1NCCC1 WUUNPBLZLWVARQ-QAETUUGQSA-N 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 229950005499 carbon tetrachloride Drugs 0.000 description 1
- -1 carrene Chemical compound 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000005446 dissolved organic matter Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 230000002335 preservative effect Effects 0.000 description 1
- 238000013441 quality evaluation Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000007779 soft material Substances 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N24/00—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects
- G01N24/08—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects by using nuclear magnetic resonance
- G01N24/081—Making measurements of geologic samples, e.g. measurements of moisture, pH, porosity, permeability, tortuosity or viscosity
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N15/088—Investigating volume, surface area, size or distribution of pores; Porosimetry
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Abstract
A method using nuclear magnetic resonance to measure rock porosity includes: machining rock with dissolution pores into a core column, and removing organic substances attaching to the core column; filling the dissolution pores of the core column with flexible water-absorption substances; submerging the core column into water under the pressure of 2-5MPa for 24-72 hours; taking out the core column, removing the water on the surface of the core column, and using a film to wrap the core column; performing a nuclear magnetic resonance experiment on the core column to obtain the porosity. The method has the advantages that the water-absorption substances are used to fill the dissolution pores of the rock so as to constrain the water in the dissolution pores, the water in the dissolution pores does not flow out of the dissolution pores during the nuclear magnetic resonance experiment, and the measured rock porosity is accurate.
Description
Technical field
The present invention relates to petrographical analysis technical field, utilize nuclear-magnetism in particular to oneThe method of resonance measuring rock porosity.
Background technology
The porosity of Nuclear Magnetic Resonance Measurement rock is that the nuclear-magnetism containing hydrogen fluid in blowhole is relaxedHenan signal is measured, and by hydrionic response in the large fine pore of difference, finally draws rockStone pore structure and total porosity. Carbonate rock is often because corrosion has largerDissolution pore and solution cavity, but by conventional measuring method in often can not Measurement accuracy rockPore system, this is because the water in macrovoid is lost to around rock in measuring process,Cause the water quality evaluation in irreducible water and aperture too high.
In recent years, nuclear magnetic resonance apparatus is more and more favored in blowhole Measurement and analysis,The smaller rock in hole aperture be full of under regimen condition, measure still more accurate, but toolThere is the conventional nuclear magnetic resonance measuring method of the rock deviation to some extent of the larger dissolution pore in aperture, mainProblem is: there is macroporous rock and is being full of after water, and in plastic sheeting encapsulation process,Water in macrovoid is very easy to lose, and makes the porosity finally measured less than normal; At coreIn acquisition of magnetic resonance data, the easy seepage flow of the water capacity in macrovoid, to film, makes to use nuclear-magnetismThe small-bore hole proportion that resonance measuring goes out increases, and hole shared ratio in large aperture subtractsLittle, cause nuclear magnetic resonance to evaluate inaccurate to macroporous pore structure.
Summary of the invention
The object of the present invention is to provide a kind of side that utilizes Nuclear Magnetic Resonance Measurement rock porosityMethod, can hold onto the water in rock dissolution pore by water imbibition material, improves porosity measurementThe degree of accuracy of value.
The present invention realizes by the following technical solutions:
A method of utilizing Nuclear Magnetic Resonance Measurement rock porosity, comprises the steps:
(1), the rock with dissolution pore is processed to pillared rock core post, remove rock core post attachedThe organic matter of;
(2), in the dissolution pore of rock core post, fill in flexible water imbibition material;
(3), rock core post is immersed in to water under 2MPa-5MPa pressure in 24h-72h;
(4), removal of core post, remove the water on rock core post surface, re-use film coated rockStem;
(5), rock core post is carried out to nuclear magnetic resonance experiment and draw porosity.
The side of what preferred embodiment of the present invention provided utilize Nuclear Magnetic Resonance Measurement rock porosityThe beneficial effect of method is:
The rock with dissolution pore is processed to pillared rock core post, and what removal rock core post adhered to hasMachine thing, prevents the impact of organic matter on nuclear magnetic resonance experiment and makes the value of porosity produce deviation.In the dissolution pore of rock core post, fill in water imbibition material, then by rock core post at 2MPa-5MPaUnder pressure, be immersed in 24h-72h in water, water entered in the dissolution pore of rock core post fully and quiltWater imbibition material is strapped in dissolution pore. Thereafter, removal of core post, removes rock core post surfaceWater, re-uses film coated rock core post, prevents water in the dissolution pore of the rock core post mistake in experimentIn journey, run off, and then remain in dissolution pore, like this in the time carrying out nuclear magnetic resonance experiment,The porosity value obtaining is more accurate, is beneficial to the follow-up research to rock.
Brief description of the drawings
In order to be illustrated more clearly in the technical scheme of the embodiment of the present invention, below will be to embodimentIn the accompanying drawing of required use be briefly described, should be appreciated that the following drawings only showsSome embodiment of the present invention, therefore should not be counted as the restriction to scope, for abilityTerritory those of ordinary skill, is not paying under the prerequisite of creative work, can also basisThese accompanying drawings obtain other relevant accompanying drawings.
Fig. 1 is the T2 collection of illustrative plates that the first test example of the present invention obtains;
Fig. 2 is the T2 collection of illustrative plates that the second test example of the present invention obtains.
Detailed description of the invention
For making object, technical scheme and the advantage of the embodiment of the present invention clearer, below willTechnical scheme in the embodiment of the present invention is clearly and completely described. In embodiment notIndicate actual conditions person, carry out according to the condition of normal condition or manufacturer's suggestion. Examination usedThe unreceipted person of production firm of agent or instrument, is the routine that can obtain by commercially available purchase and producesProduct.
Below the method for utilizing Nuclear Magnetic Resonance Measurement rock porosity of the embodiment of the present invention is enteredRow illustrates.
A method of utilizing Nuclear Magnetic Resonance Measurement rock porosity, comprises the steps:
(1), the rock with dissolution pore is processed to pillared rock core post, use core holeThe rock with dissolution pore is drilled to the column that diameter is 2cm-2.5cm by sampler, re-usesIt is the rock core post of 4.5cm-5cm that cylindrical Rock cutting is become length by rock cutter,To the rock core post that conveniently carries out nuclear magnetic resonance experiment. Remove the organic side that rock core post adheres toFormula has a lot, for example, use the mode such as high temperature evaporation, activating agent washing. In the present invention, excellentChoosing, with an organic solvent dissolves the organic matter that rock core post adheres to, and organic solvent not only can be fastSpeed is dissolved organic matter completely, and the organic matter of removing rock core post is effective, simultaneously organic solventBoiling point lower, easily remove, can on rock core post, not cause residually, affect nuclear magnetic resonance realityThe effect of testing.
As preferably, organic solvent can select ethanol, carrene, benzene, tetrachloromethane,Chloroform etc. Taking above-mentioned organic solvent as extracting solvent, rock core post is carried out to soxhlet extraction at least24h, then dries rock core post to organic solvent and volatilizees, and prevents that organic matter is to nuclear magnetic resonance experimentAffect and make the value of porosity produce deviation. Soxhlet extraction is from solid matter, to extract chemical combinationA kind of method of thing, it is with solvent, long-term infiltration of solid to be leached needed materialCome, utilize solvent refluxing and siphon principle, making solid matter can be pure solvent each timeInstitute extracts, and when after solvent ebuillition of heated, steam rises by wireway, is condensed into liquidSplash in extractor. In the time that liquid level exceedes siphon pipe highest point, there is siphonage, moltenLiquid passes back into flask, therefore can extract the part material that is dissolved in solvent, utilizes molten like thisAgent backflow and siphonage, be enriched in flask the DDGS in solid. This method is goneMore thorough except the organic matter that rock core post adheres to, be beneficial to and reduce organic existence to porosityThe impact of value, the accuracy of guarantee data.
Better, organic solvent adopts chloroform, and chloroform is again chloroform, and boiling point is61-62 DEG C, volatile and good to most of organic dissolubilities, organic matter can be fastBe dissolved in wherein. Taking chloroform as extracting solvent, rock core post is carried out to soxhlet extraction 24h-48h,Then at 100 DEG C-105 DEG C, dry rock core post to chloroform and volatilize, due to the characteristic of chloroform,In the situation of 24h-48h, can dissolve the organic matter in rock core post completely, at 100 DEG C-105 DEG CUnder can ensure to make chloroform volatilization completely within the time faster, ensure the quick, accurate of experimentTrue carrying out, prevents the impact of organic matter on nuclear magnetic resonance experiment and the value of porosity is producedDeviation.
(2), in the dissolution pore of rock core post, fill in flexible water imbibition material, water imbibition materialRefer to: meet after water can imbibition certain volume and water is stored material. Flexibility isRefer to: there is the soft material of deformability, such as sponge, cotton etc. In the present invention, excellentChoosing adopts cotton as flexible water imbibition material, and cotton has good water absorbing properties, densityVery little, less cotton just can absorb more water, and it can not affect nuclear magnetic resonanceExperiment value. Dissolution pore comprises that the major diameter dissolution pore of aperture>=2mm and aperture<2mm's is little straightFootpath dissolution pore, the aperture of minor diameter dissolution pore is little, and after water infiltrates wherein, the speed of overflowing is slower,Therefore need not fill in water imbibition material water conservation, therefore in embodiments of the invention, all preferredOnly water imbibition material is filled in major diameter dissolution pore. It should be noted that, at minor diameter dissolution poreIn to fill in the water imbibition materials such as cotton be also feasible.
In major diameter dissolution pore, fill in after flexible water imbibition material, the water in dissolution pore can lead toCross water imbibition material and be strapped in dissolution pore, in the dissolution pore of rock core post, can possess for a long time a certain amount ofWater, the current in the process of experiment in dissolution pore lose also can be less, makes follow-up nuclear magnetic resonanceExperiment can reflect the porosity of the dissolution pore in rock accurately.
Fill in when too much when cotton in dissolution pore, cotton can expose dissolution pore, and the amount of cotton is excessive,Accordingly, cotton absorb water with the actual water that should fetter of dissolution pore than on the high side, at nuclear-magnetismIn the process of resonance measuring, the porosity value obtaining can be bigger than normal; When cotton in dissolution pore was filled inWhen few, cotton can not fill up dissolution pore, and the amount of cotton is too small, corresponding, the water that cotton absorbs,, in the process of Nuclear Magnetic Resonance Measurement, obtain than on the low side with the actual water that should fetter of dissolution poreThe porosity value arriving can be less than normal. Therefore, preferably, fill in cotton 0.005g-0.02g to holeFootpath is in the major diameter dissolution pore of 2mm-4mm; Filling in cotton 0.02g-0.03g to aperture isIn the major diameter dissolution pore of 4mm-6mm; Filling in cotton 0.03g-0.06g to aperture isIn the major diameter dissolution pore of 6mm-8mm; Fill in cotton 0.06g-0.08g and be greater than 8mm to apertureMajor diameter dissolution pore in. It should be noted that, in minor diameter dissolution pore, can fill in cotton, alsoCan not fill in cotton. Make to be all full of water in the dissolution pore of rock core post, the water in dissolution pore can lead toCross cotton and be strapped in dissolution pore, can in the process of experiment, not cause the current in dissolution pore to lose,Make follow-up nuclear magnetic resonance experiment can reflect accurately the porosity of the dissolution pore in rock core post.
(3), rock core post is immersed in to water under 2MPa-5MPa pressure in 24h-72h, pressPower is too small, and water is not easy to enter in dissolution pore smaller or deep in rock core post, pressureExcessive, can make rock core post that damaged, even damage occurs. The time of immersion water is too short, rock coreIn the dissolution pore of post, can not be full of water completely, the overlong time of immersion water, waste experimental period andExperimental resources. So, use the rock core saturation experiments instrument of finding time to pressurize to press at 2MPa-5MPaUnder power, make rock core post be immersed in 24h-72h in water completely, make in all dissolution pores of rock core post allBe full of water, cotton also absorbs enough water, makes the follow-up nuclear magnetic resonance experiment can be accuratelyThe porosity of the dissolution pore in reflection rock core post.
(4), removal of core post, remove the water on rock core post surface, re-use film coated rockStem, is wound around fast rock core post with plastic sheeting and makes rock core post surface be coated the plastics of 3-5 layerFilm, prevents that the water being stored in water imbibition material from outwards overflowing, and water is remained in dissolution pore,Make follow-up nuclear magnetic resonance experiment can reflect accurately the porosity of the dissolution pore in rock core post.
(5), rock core post is carried out to nuclear magnetic resonance experiment and draw porosity. Particularly, existIn the present invention, use heavy caliber nuclear magnetic resonance spectroscopy and imaging system instrument to record sample rock coreThe T2 spectrogram of post, the content in comprehensive T2 spectrogram, and by heavy caliber nuclear magnetic resonance spectroscopyCalculate the porosity value of rock core post, profit with the porosity calculation software in imaging system instrumentThe method those skilled in the art that survey porosity with nuclear magnetic resonance experiment are with reference to prior artRealize.
Embodiment 1
(1), use the core hole sampler that model is YZ-1 to there is the rock of dissolution poreBe drilled to the column that diameter is 2.5cm, re-use rock cutter cylindrical rock is cutBeing slit into length is the rock core post of 5cm. Taking chloroform as extracting solvent, carry out cable-styled to rock core postExtract 36h, then at 100 DEG C, dry rock core post to chloroform and volatilize.
(2), the dissolution pore of rock core post comprises major diameter dissolution pore and minor diameter dissolution pore, at rock core postMajor diameter dissolution pore in fill in cotton with tweezers, filling in cotton 0.02g is 4mm's to apertureIn major diameter dissolution pore; In the major diameter dissolution pore that to fill in cotton 0.03g be 6mm to aperture; PlugIn the major diameter dissolution pore that to enter cotton 0.06g be 8mm to aperture; Fill in cotton 0.08g to holeIn the major diameter dissolution pore of footpath 10mm.
(3), use the rock core saturation experiments instrument of finding time to pressurize under 5MPa pressure, to make rock core postBe immersed in 24h in water completely.
(4), removal of core post, with clean rag wiping rock core post, remove rock core post tableThe water of face, re-uses PE10 plastic sheeting and is wound around fast rock core post, makes rock core post surface bagCover the PE10 plastic sheeting of 5 layers. In the present embodiment, PE10 plastic sheeting is to purchase in supermarketThe preservative film of buying.
(5), use the heavy caliber nuclear magnetic resonance spectroscopy that model is MacroMR12-150H-IThe T2 spectrogram that records sample rock core post with imaging system instrument under following parameter, magnetic field is strongDegree: 0.3 ± 0.05T, instrument basic frequency: 12.8MHz, probe coil diameter: 150mm,Content in comprehensive T2 spectrogram, and the heavy caliber that is MacroMR12-150H-I by modelPorosity calculation software in nuclear magnetic resonance spectroscopy and imaging system instrument calculates rock core postPorosity value is 7.34%.
Embodiment 2
(1), use the core hole sampler that model is YZ-1 to there is the rock of dissolution poreBe drilled to the column that diameter is 2.5cm, re-use rock cutter cylindrical rock is cutBeing slit into length is the rock core post of 4.5cm. Taking chloroform as extracting solvent, rock core post is carried out to ropeFormula is extracted 24h, then at 105 DEG C, dries rock core post to chloroform and volatilizees.
(2), the dissolution pore of rock core post comprises major diameter dissolution pore and minor diameter dissolution pore, at rock core postMajor diameter dissolution pore in fill in cotton with tweezers, filling in cotton 0.005g is 2mm to apertureMajor diameter dissolution pore in; In the major diameter dissolution pore that to fill in cotton 0.02g be 4mm to aperture;In the major diameter dissolution pore that to fill in cotton 0.03g be 6mm to aperture; Filling in cotton 0.06g arrivesAperture is in the major diameter dissolution pore of 8mm.
(3), use the rock core saturation experiments instrument of finding time to pressurize under 2MPa pressure, to make rock core postBe immersed in 72h in water completely.
(4), removal of core post, with clean rag wiping rock core post, remove rock core post tableThe water of face, re-uses PE10 plastic sheeting and is wound around fast rock core post, makes rock core post surface bagCover the PE10 plastic sheeting of 3 layers.
(5), use the heavy caliber nuclear magnetic resonance spectroscopy that model is MacroMR12-150H-IThe T2 spectrogram that records sample rock core post with imaging system instrument under following parameter, magnetic field is strongDegree: 0.3 ± 0.05T, instrument basic frequency: 12.8MHz, probe coil diameter: 150mm,Content in comprehensive T2 spectrogram, and the heavy caliber that is MacroMR12-150H-I by modelPorosity calculation software in nuclear magnetic resonance spectroscopy and imaging system instrument calculates rock core postPorosity value 7.37%.
Embodiment 3
(1), use the core hole sampler that model is YZ-1 to there is the rock of dissolution poreBe drilled to the column that diameter is 2.5cm, re-use rock cutter cylindrical rock is cutBeing slit into length is the rock core post of 4.7cm. Taking chloroform as extracting solvent, rock core post is carried out to ropeFormula is extracted 48h, then at 102 DEG C, dries rock core post to chloroform and volatilizees.
(2), the dissolution pore of rock core post comprises major diameter dissolution pore and minor diameter dissolution pore, at rock core postMajor diameter dissolution pore in fill in cotton with tweezers, filling in cotton 0.01g is 3mm's to apertureIn major diameter dissolution pore; In the major diameter dissolution pore that to fill in cotton 0.02g be 5mm to aperture; PlugIn the major diameter dissolution pore that to enter cotton 0.04g be 7mm to aperture; Fill in cotton 0.07g to holeFootpath is in the major diameter dissolution pore of 9mm.
(3), use the rock core saturation experiments instrument of finding time to pressurize under 3MPa pressure, to make rock core postBe immersed in 36h in water completely.
(4), removal of core post, with clean rag wiping rock core post, remove rock core post tableThe water of face, re-uses PE10 plastic sheeting and is wound around fast rock core post, makes rock core post surface bagCover the PE10 plastic sheeting of 4 layers.
(5), use the heavy caliber nuclear magnetic resonance spectroscopy that model is MacroMR12-150H-IThe T2 spectrogram that records sample rock core post with imaging system instrument under following parameter, magnetic field is strongDegree: 0.3 ± 0.05T, instrument basic frequency: 12.8MHz, probe coil diameter: 150mm,Content in comprehensive T2 spectrogram, and the heavy caliber that is MacroMR12-150H-I by modelPorosity calculation software in nuclear magnetic resonance spectroscopy and imaging system instrument calculates rock core postPorosity value is 7.38%.
Embodiment 4
(1), use the core hole sampler that model is YZ-1 to there is the rock of dissolution poreBe drilled to the column that diameter is 2.5cm, re-use rock cutter cylindrical rock is cutBeing slit into length is the rock core post of 4.5cm. Taking chloroform as extracting solvent, rock core post is carried out to ropeFormula is extracted 24h, then at 105 DEG C, dries rock core post to chloroform and volatilizees.
(2), the dissolution pore of rock core post comprises major diameter dissolution pore and minor diameter dissolution pore, at rock core postMajor diameter dissolution pore in fill in cotton with tweezers, filling in cotton 0.005g is 2mm to apertureMajor diameter dissolution pore in; In the major diameter dissolution pore that to fill in cotton 0.02g be 4mm to aperture;In the major diameter dissolution pore that to fill in cotton 0.03g be 6mm to aperture; Filling in cotton 0.06g arrivesAperture is in the major diameter dissolution pore of 8mm. Make to be all full of water, dissolution pore in the dissolution pore of rock core postIn water can be strapped in dissolution pore by cotton, not can experiment process in cause dissolution poreIn current lose, make follow-up nuclear magnetic resonance experiment can reflect accurately molten in rock core postThe porosity in hole.
(3), use the rock core saturation experiments instrument of finding time to pressurize under 2MPa pressure, to make rock core postBe immersed in 48h in water completely.
(4), removal of core post, with clean rag wiping rock core post, remove rock core post tableThe water of face, re-uses PE10 plastic sheeting and is wound around fast rock core post and makes rock core post surface coated 3The PE10 plastic sheeting of layer.
(5), use the heavy caliber nuclear magnetic resonance spectroscopy that model is MacroMR12-150H-IRecord the T2 spectrogram of sample rock core post with imaging system instrument, the content in comprehensive T2 spectrogram,And the heavy caliber nuclear magnetic resonance spectroscopy that is MacroMR12-150H-I by model and imaging systemPorosity calculation software in system instrument calculates the porosity value of rock core post.
The method of utilizing Nuclear Magnetic Resonance Measurement rock porosity that Fig. 1 provides for this test exampleT2 collection of illustrative plates. Refer to Fig. 1, in Fig. 1, A represents porosity component, i.e. each time point instituteThe porosity of the rock core post of measuring; B represents porosity accumulation, i.e. measured institute aboveThe free cumulant of putting measured porosity; T represents that rock core post at heavy caliber nuclear-magnetism altogetherMeasuring Time in vibration analysis and imaging system instrument. Content in comprehensive T2 spectrogram, andThe heavy caliber nuclear magnetic resonance spectroscopy and the imaging system that are MacroMR12-150H-I by modelThe porosity value that porosity calculation software in instrument calculates rock core post is 7.39%.
Reference examples 1
(1), use the core hole sampler that model is YZ-1 to there is the rock of dissolution poreBe drilled to the column that diameter is 2.5cm, re-use rock cutter cylindrical rock is cutBeing slit into length is the rock core post of 4.5cm. Taking chloroform as extracting solvent, rock core post is carried out to ropeFormula is extracted 24h, then at 105 DEG C, dries rock core post to chloroform and volatilizees.
(2), use the rock core saturation experiments instrument of finding time to pressurize under 2MPa pressure, to make rock core postBe immersed in 48h in water completely.
(3), removal of core post, with clean rag wiping rock core post, remove rock core post tableThe water of face, re-uses PE10 plastic sheeting and is wound around fast rock core post, makes rock core post surface bagCover the PE10 plastic sheeting of 3 layers.
(4), use the heavy caliber nuclear magnetic resonance spectroscopy that model is MacroMR12-150H-IRecord the T2 spectrogram of sample rock core post with imaging system instrument, the content in comprehensive T2 spectrogram,And the heavy caliber nuclear magnetic resonance spectroscopy that is MacroMR12-150H-I by model and imaging systemPorosity calculation software in system instrument calculates the porosity value of rock core post.
Fig. 2 is the T2 collection of illustrative plates that this test example obtains. Refer to Fig. 2, in Fig. 2, A representsPorosity component, the i.e. porosity of the measured rock core post of each time point; B represents holeGap degree accumulation, the i.e. cumulant of the measured porosity of measured all time points above;When T represents the measurement of rock core post in heavy caliber nuclear magnetic resonance spectroscopy and imaging system instrumentBetween. Content in comprehensive T2 spectrogram, and it is large to be MacroMR12-150H-I by modelPorosity calculation software in bore nuclear magnetic resonance spectroscopy and imaging system instrument calculates rock coreThe porosity value of post is 6.76%.
Specific experiment condition and the result of embodiment 4 and reference examples 1 are asked for an interview table 1.
Table 1 embodiment 4 and reference examples 1 experimental data table
Embodiment 4 and reference examples 1 are used identical rock core post, and the dissolution pore of rock core post comprises greatlyDiameter dissolution pore and minor diameter dissolution pore, the porosity value of the rock core post using in embodiment is known,Its porosity value is 7.38%. By finding out in table 1, embodiment 4 and reference examples 1The difference of experiment condition be only, in the major diameter dissolution pore of test example 4, filled in cotton,Illustrate that in major diameter dissolution pore, filling in cotton can make water be easy to, be strapped in completely dissolution poreIn, the heavy caliber nuclear magnetic resonance spectroscopy that is MacroMR12-150H-I in follow-up use modelIn the process of the porosity value of imaging system apparatus measures rock core post, in major diameter dissolution poreWater can not run off, and ensures the accuracy of the porosity value finally recording. Embodiment 4 drawsPorosity value is greater than the porosity value that reference examples 1 draws, and the hole that obtains of embodiment 4The porosity value of degree value and this rock core post is very approaching, illustrates that water in large dissolution pore is due to cottonEffect, not do not lose, make by heavy caliber nuclear magnetic resonance spectroscopy and imaging system apparatus measuresThe porosity value obtaining is more accurate.
In order to verify in the present invention, cotton itself can not make rock core post that nuclear magnetic resonance recordsThe value of porosity changes, and we carry out test example 1 and test example 2 is tested. ExaminationTest rock core post that example 1 and test example 2 use and be the minor diameter dissolution pore that only has aperture < 2mmRock core post, the porosity value of this rock core post is 4.24%.
Test example 1
(1) it is molten that the core hole sampler that, use model is YZ-1 will only have minor diameterThe rock in hole is drilled to the column that diameter is 2.5cm, re-uses rock cutter by cylinderRock cutting to become length be the rock core post of 4.5cm. Taking chloroform as extracting solvent, to rock corePost carries out soxhlet extraction 24h, then at 105 DEG C, dries rock core post to chloroform and volatilizees.
(2), in the minor diameter dissolution pore of rock core post, fill in cotton with tweezers, fill in cottonIn the major diameter dissolution pore that 0.002g is 1mm to aperture; Filling in cotton 0.001g to aperture isIn the major diameter dissolution pore of 0.5mm. Make to be all full of water, the water in dissolution pore in the dissolution pore of rock core postCan be strapped in dissolution pore by cotton, can in the process of experiment, not cause the water in dissolution poreRun off, make follow-up nuclear magnetic resonance experiment can reflect accurately the hole of the dissolution pore in rock core postGap degree.
(3), use the rock core saturation experiments instrument of finding time to pressurize under 2MPa pressure, to make rock core postBe immersed in 48h in water completely.
(4), removal of core post, with clean rag wiping rock core post, remove rock core post tableThe water of face, re-uses PE10 plastic sheeting and is wound around fast rock core post and makes rock core post surface coated 3The PE10 plastic sheeting of layer.
(5), use the heavy caliber nuclear magnetic resonance spectroscopy that model is MacroMR12-150H-IRecord the T2 spectrogram of sample rock core post with imaging system instrument, the content in comprehensive T2 spectrogram,And the heavy caliber nuclear magnetic resonance spectroscopy that is MacroMR12-150H-I by model and imaging systemPorosity calculation software in system instrument calculates the porosity value of rock core post. Comprehensive T2 spectrumContent in figure, and the heavy caliber nuclear magnetic resonance that is MacroMR12-150H-I by modelPorosity calculation software in analysis and imaging system instrument calculates the porosity value of rock core postBe 4.23%.
Test example 2
The difference of the experimental technique of this test example and test example 1 is only, rock core post little straightIn the dissolution pore of footpath, do not fill in cotton. Content in comprehensive T2 spectrogram, and by model beHole in heavy caliber nuclear magnetic resonance spectroscopy and the imaging system instrument of MacroMR12-150H-IThe porosity value that gap degree software for calculation calculates rock core post is 4.22%.
Experiment condition and the result of test example 1 and test example 2 are asked for an interview table 2.
Table 2 the 3rd test example experimental data table
As can be seen from Table 2, the experiment condition of test example 1 and test example 2 difference onlyBe, in the minor diameter dissolution pore of test example 1, filled in cotton, re-use model and beThe heavy caliber nuclear magnetic resonance spectroscopy of MacroMR12-150H-I and imaging system apparatus measures rockThe porosity value of stem, the hole that the porosity value that test example 1 draws and test example 2 drawDegree value is basic identical, and the same with the practical porosity value of this rock core post, and minor diameter is describedDissolution pore just can hold onto water originally, so can not occur the amount of irreducible water after adding cottonChange, cotton can not exert an influence to the value of the porosity of measuring. Illustrate that filling in cotton fillsAfter major diameter dissolution pore, by nuclear magnetic resonance experiment, the porosity value recording is tied more accuratelyOpinion has confidence level, explanation simultaneously, and minor diameter dissolution pore just had the energy of very strong irreducible water originallyPower need to not filled in cotton and carry out the measurement of porosity value in minor diameter dissolution pore.
Embodiment described above is the present invention's part embodiment, instead of whole realitiesExecute example. The detailed description of embodiments of the invention is not intended to limit claimed the present inventionScope, but only represent selected embodiment of the present invention. Based on the enforcement in the present inventionExample, those of ordinary skill in the art are not making the institute obtaining under creative work prerequisiteThere are other embodiment, all belong to the scope of protection of the invention.
Claims (10)
1. a method of utilizing Nuclear Magnetic Resonance Measurement rock porosity, is characterized in that, bagDraw together following steps:
(1), the rock with dissolution pore is processed to pillared rock core post, remove described rock coreThe organic matter that post adheres to;
(2), in the described dissolution pore of described rock core post, fill in flexible water imbibition material;
(3), described rock core post is immersed in to water under 2MPa-5MPa pressure in 24h-72h;
(4), take out described rock core post, remove the water on described rock core post surface, re-use thinFilm is coated described rock core post;
(5), described rock core post is carried out to nuclear magnetic resonance experiment and draw porosity.
2. method according to claim 1, is characterized in that, in described step (2)In, described dissolution pore comprises the major diameter dissolution pore of aperture>=2mm and the minor diameter of aperture<2mmDissolution pore, in described step (2), described water imbibition material is filled in described major diameter dissolution pore.
3. method according to claim 2, is characterized in that, described water imbibition materialFor cotton.
4. method according to claim 3, is characterized in that, in described step (2),Filling in described cotton 0.005g-0.02g is the described major diameter dissolution pore of 2mm-4mm to apertureIn; The described major diameter of filling in described cotton 0.02g-0.03g and to aperture be 4mm-6mm is moltenKong Zhong; Fill in the described major diameter that described cotton 0.03g-0.06g is 6mm-8mm to apertureIn dissolution pore; Fill in described cotton 0.06g-0.08g is greater than 8mm described major diameter to apertureIn dissolution pore.
5. method according to claim 1, is characterized in that, in described step (1),The diameter of described rock core post is 2cm-2.5cm, and length is 4.5cm-5.0cm.
6. method according to claim 1, is characterized in that, in described step (1),With an organic solvent dissolve the organic matter that described rock core post adheres to.
7. method according to claim 6, is characterized in that, in described step (1),With an organic solvent dissolving the described organic matter that described rock core post adheres to carries out in the following manner:Taking described organic solvent as extracting solvent, described rock core post is carried out at least 24h of soxhlet extraction,Then dry described rock core post to described organic solvent volatilization.
8. according to the method described in claim 6 or 7, it is characterized in that, described organic moltenAgent is chloroform.
9. method according to claim 8, is characterized in that, in described step (1),Removing the described organic matter that described rock core post adheres to carries out in the following manner: taking described chloroform asExtract solvent, described rock core post is carried out to soxhlet extraction 24h-48h, then at 100 DEG C-105 DEG CThe described rock core post of lower baking is to described chloroform volatilization.
10. method according to claim 1, is characterized in that, described step (4)In, described film is plastic sheeting, described plastic sheeting is coated described rock core post 3-5 layer.
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