CN105601169A - Production method of hot-pressing-based kerogen-containing shale physical model and shale model - Google Patents
Production method of hot-pressing-based kerogen-containing shale physical model and shale model Download PDFInfo
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- CN105601169A CN105601169A CN201510940267.3A CN201510940267A CN105601169A CN 105601169 A CN105601169 A CN 105601169A CN 201510940267 A CN201510940267 A CN 201510940267A CN 105601169 A CN105601169 A CN 105601169A
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B26/00—Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
- C04B26/02—Macromolecular compounds
- C04B26/10—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C04B26/14—Polyepoxides
Abstract
The present invention provides a production method of a hot-pressing-based kerogen-containing shale physical model and the shale model. The production method comprises the following steps: mixed powder is obtained by ball milling of silica power, calcite, illite and kerogen; a binder is added into the mixed powder for uniformly mixing to obtain a mixed material; the mixed material is layer by layer spread in a hot-pressing die, after each layer of the mixed material is spread, pre-compacting treatment is performed, and a mold filled with the mixed material is obtained; and the kerogen-containing shale physical model can be obtained by final room temperature pre-compacting treatment and heating, pressing and heat and pressure preservation treatment. The production method is a physical model production method which is closest to the natural shale diagenesis environment and diagenetic mechanism. Various petrophysical parameters, mechanical characteristics, seismic properties, microstructure and diagenetic conditions of the kerogen-containing shale physical model are closer to that of natural shale.
Description
Technical field
The present invention relates to a kind of preparation method and this preparation method of the kerogenous shale physical model based on hot pressingThe shale physical model that making obtains, belongs to the geophysical research technical field of oil-gas exploration and exploitation.
Background technology
Shale (shale) is the groups such as a kind of particulate chip, clay mineral, organic matter that is less than 0.004mm by particle diameterThe sedimentary rock with lamina and laminated structure of shale structure becoming. Shale is one of Sedimentary Rock the abundantest in the earth's crust, at natureIn widely distributed, nearly in sedimentary rock more than 75% is shale. In produce oil basin, organic shale is main hydrocarbonSource rock; Common shale type has black shale, culm, oil shale, siliceous shale, irony shale, calcareousShale, arenaceous shale etc. The shale of nearly all type can be served as reservoir. In compacting process, shaleLiquid expulsion acts on has important effect in oil-gas migration; In reservoir engineering, shale can be used as fluid barrier;In geological data, shale can show as earthquake reflector and cause the attenuation of seismic wave. Therefore, grinding for shaleStudy carefully oil-gas exploration and reservoir management are all had very important significance.
Theoretical research seriously lags behind exploration production practice and a series of basic aspect and studies a question and formed in restrictionThe bottleneck of state's shale gas exploitation, especially in today of China's shale gas exploration fast starting, shale basis rock physicsThe system of research work launches shale gas industrial expansion to be extremely important. But, test in laboratoryIn process, can find more difficult the obtaining of natural shale sample. The most weathering of the sample of appearing is serious, and processing is difficulty comparatively; Rock coreSample size is few, obtains difficulty larger; Part Natural Samples anisotropism is stronger, and test data is difficult to use in theory and grindsStudy carefully; Affect the many factors of Natural Samples character, be difficult to study targetedly. Due to the difficulty of sample preparation in experiment,Domestic to the mud as usually oil gas reservoir cap rock, shale seismic velocity and anisotropic petrophysical data researchStill inadequate. Physical experiments is the different subject joint researches cracks such as contact geology, geophysics and reservoir engineeringThe tie of oil-gas reservoir and bridge. And wherein a most important job is exactly to produce a set of and natural shale each side to belong toAll more close physical models of property. Considerably less to the research of artificial shale both at home and abroad, although there is afterwards adopting normal temperatureCondition presses down the technique of knot (cold-press method), and the mixed material using kaolin as clay composition is compacted into piece, with skySo diagenetic environment and the Rock-forming Mechanism of shale reality have larger discrepancy, and one of them very large problem cold-press method can notCan consider the variation of kerogen institute's temperature in diagenetic process. And consider that kerogen to the lithology transitivity of shale allHave significant impact and the generation of oil gas is also had to direct correlation and vital effect, ignoring this problem mustTo cause physical model to have natural defect, thereby affect follow-up analysis and application.
Therefore, produce diagenesis condition, microstructure, mineralogical composition, anisotropy, porosity and elastic parameterDeng the shale physical model approaching with actual rock, be still one of this area problem demanding prompt solution.
Summary of the invention
For solving the problems of the technologies described above, the object of the present invention is to provide a kind of kerogenous shale physics based on hot pressingThe preparation method of model and this preparation method are made the shale physical model obtaining. Preparation method energy provided by the inventionEnough making obtains and the similarly artificial shale physical model of natural shale everyway.
For achieving the above object, first the present invention provides a kind of system of the kerogenous shale physical model based on hot pressingMake method, it comprises the following steps:
Silicon powder, calcite, illite and kerogen (are comprised to I type kerogen, II type kerogen, III type cheeseRoots etc., can be selected as required by those skilled in the art) carry out ball milling mixing, obtain mixed powder;
In described mixed powder, add binding agent, after mixing, obtain mixed material;
By described mixed material successively lay enter in hot pressing die, and carry out pre-compacted after every lay one deck mixed materialProcess (adopting little pressure), obtain being equipped with the mould of mixed material;
The described mould that mixed material is housed is carried out after the final pre-compacted processing of normal temperature, then heat and pressurize and be incubatedPressurize processing, obtains shale physical model kerogenous.
In above-mentioned preparation method, preferably, taking the gross weight of described mixed powder as benchmark, described silicon powderContent is 20%～60%, and the content of described calcite is 1%～25%, and described illitic content is 15%～50%,Described kerogenic content is 2%～15%.
In above-mentioned preparation method, preferably, the fineness of described silicon powder is 3000～4000 orders, described calciteFineness be 3000～4000 orders, described illitic fineness is 3000～4000 orders. Because kerogen belongs to unsettingState, heating may occur to melt and sizing again, therefore, its fineness is not limited.
According to the specific embodiment of the present invention, preferably, above-mentioned preparation method is further comprising the steps of: describedThe raw material such as silicon powder, calcite, illite and kerogen carry out before ball milling mixing, first by they process processed.This processed can be these raw material are placed to 48h in 40～60 DEG C of insulating boxs more than.
In above-mentioned preparation method, preferably, described ball milling adopts the group of the ball milling pearl of large, medium and small three sizesClose. Wherein, the diameter range of large ball milling pearl can be 15～20mm, and the diameter range of middle ball milling pearl can be10～15mm, the diameter of bead mill pearl can be 5～10mm. And, the ball milling pearl of large, medium and small three sizesNumber ratio can be (10～20): (20～25): (80～100), are preferably 14:23:84. In addition, described ball milling adoptsThe rotating speed of ball mill can be 350～450R/min, and Ball-milling Time can be 36～48h.
In above-mentioned preparation method, preferably, the weight ratio of described mixed powder and described binding agent is10:1～10:2. More preferably, the weight ratio of described mixed powder and described binding agent is 10:1.
In above-mentioned preparation method, preferably, described binding agent comprises YY4250A/B series epoxy adhesive (saltCity Yi Jiayi Electron Material Co., Ltd), this binding agent can play the effect of moulding base substrate. More preferably, described inThe solidification temperature of YY4250A/B series epoxy adhesive is 130 DEG C/2h～150 DEG C/2h. Particularly preferably,In YY4250A/B series epoxy adhesive, A glue proportion is 1.15g/cc, and B glue proportion is 1.10g/cc.
In above-mentioned preparation method, preferably, the mixing of described mixed powder and described binding agent is to adopt manual stone rollerThe mode that mill sieves, and make the above mixed material of 99% (percentage by weight) can pass through 300 object sieves.
In above-mentioned preparation method, preferably, described mould is cleaning and/or wiped clean and smears all scholars of thin layerThe mould of woods and/or silicone oil.
In above-mentioned preparation method, preferably, by described mixed material successively lay enter lay in hot pressing dieNumber is for 4-6 time.
In above-mentioned preparation method, preferably, the pre-compacted processing of carrying out after every lay one deck mixed material is passableEmploying following steps are carried out: after entirely lay enters in mould by mixed material, put into pressure head, knock pressure head end face200～300 times (can use rubber hammer to knock with sudden force).
In above-mentioned preparation method, preferably, the described mould that mixed material is housed is carried out to the final pre-compacted of normal temperatureProcessing is to make described mixed material bear the pressure of 5MPa～20MPa pressurize 0.4～1h.
In above-mentioned preparation method, preferably, in described heating pressurization heat-insulation pressure keeping processing procedure, described mixingThe pressure that material bears is 100MPa～517.5MPa, can choose flexibly as requested force value as long as at above-mentioned modelIn enclosing, the temperature of heating is 100 DEG C～250 DEG C, can choose flexibly as requested temperature value as long as at above-mentioned modelIn enclosing, the time of heat-insulation pressure keeping is 3600～5760min.
According to the specific embodiment of the present invention, preferably, above-mentioned preparation method is further comprising the steps of: described in inciting somebody to actionThe mould that mixed material is housed heats after pressurization heat-insulation pressure keeping processing, sheds pressure and stops insulation, then willThe temperature of hot pressing die is adjusted to 37 DEG C of left and right (for example 34 DEG C～40 DEG C) and is incubated after 18-36h, then to the page obtainingRock physical model carries out the demoulding, and can also carry out afterwards edge and polish smooth, and can be by modes such as cutting drill stringsBe processed into needed shape and size.
In addition, the present invention also provides a kind of shale physical model kerogenous, its by above-mentioned based on hot pressingThe preparation method of kerogenous shale physical model and making obtains.
According to the specific embodiment of the present invention, preferably, the density of above-mentioned shale physical model kerogenous is greater than2.0g/cc, porosity is less than 5%, and permeability is less than 0.1mD, and velocity of longitudinal wave is that 2500m/s～4500m/s is (parallelIn bedding direction and perpendicular to the velocity of longitudinal wave of bedding direction all within the scope of this), Shear Waves Splitting speed is1500m/s～3000m/s (be parallel to bedding direction and perpendicular to fast, the slow shear wave velocity of bedding direction all at thisIn scope), ripple anisotropy is all greater than 10% in length and breadth.
According to the specific embodiment of the present invention, preferably, above-mentioned shale physical model kerogenous is in microstructureAspect, the microstructure height of vertical stratification and parallel bedding direction and natural shale correspondence direction is approximate, can observeTo obvious layering and/or stacked in layers structure, above-mentioned shale physical model kerogenous is kerogenic simultaneouslyThe kerogen of microstructure spatial and natural shale is similar.
The preparation method of the kerogenous shale physical model based on hot pressing provided by the invention can be for a certain concreteInfluence factor, makes the synthetic sample theorizing, and can change arbitrarily the size of this influence factor, produces passIn this influence factor continually varying synthetic sample series. Preparation method provided by the invention and preparing by the methodThe artificial shale physical model obtaining mainly has the following advantages: (1) (shows by scanning electron aspect microstructureMicro mirror is observed), shale physical model of the present invention is at vertical stratification and parallel bedding direction and natural shale correspondence directionMicrostructure height approximate, can observe obvious layering and/or stacked in layers structure, simultaneously kerogenicThe kerogen of microstructure spatial and natural shale has similarity; (2) aspect physical characteristic, of the present inventionShale physical model meets the characteristic of the natural shale low-porosity low-permeability with extraction value, of the present invention artificialThe porosity of kerogenous shale physical model is less than 5%, and permeability is less than 0.1mD; (3) aspect seismic character,The compressional wave of shale physical model of the present invention and Shear Waves Splitting speed, density parameter corresponding to natural shale are similar to, simultaneouslyCan ensure the strong anisotropic character of shale, the compressional wave anisotropic degree of this shale physical model is not less than 10%,Shear wave anisotropic degree is also not less than 10%; (4) aspect mechanical property, the bullet of shale physical model of the present inventionProperty modulus, Young's modulus and Poisson's ratio are consistent with the scope of natural shale; (5) and, this making flow process is reliable and stable,Homogenieity repeatable strong, each position of single sample is better, and meets laboratory related experiment test sample and wantAsk.
In addition, the present invention also provides a kind of hot pressing die of manufacturing artificial petrophysical model, and this hot pressing die at least comprisesDie ontology and mould pressure head; Wherein,
Described die ontology has the cavity for manufacturing artificial petrophysical model, and the bottom of cavity is provided with base, cavityAnd the surrounding of base has wearing layer, the outer surface of wearing layer has bearing course, the upper surface of bearing course, lower surfaceAnd outer surface has heat insulation layer, close contact between base and wearing layer, close contact between wearing layer and bearing course,Close contact between bearing course and heat insulation layer, and in bearing course, be provided with thermocouple and some heaters;
The front end face of described mould pressure head is the plane consistent with the cavity cross section shape of die ontology. Be appreciated thatMould pressure head is generally the cylinder body shape matching with cavity cavity.
In the hot pressing die of above-mentioned manufacturing artificial petrophysical model, preferably, the cross section of cavity be rectangle, circle,Ellipse, triangle or parallelogram, those skilled in the art can be according to artificial rock's model sample of think compactingConcrete shape cavity can be arranged to corresponding shape. Conventionally, the cross-sectional area of cavity is 25～400cm2, cavityThe degree of depth be 7～40cm. According to a specific embodiments of the present invention, the heat of manufacturing artificial petrophysical model of the present inventionIn compression mould, the rectangle that the cross section of described cavity is 5～20cm × 5～20cm. Wherein, if the cross section of cavityFor the shape with angle such as triangle or parallelogram etc., possible angle can cause and be subject in pressure processPower inequality, affects final mask effect, but now only need be after model forming, and shape as required cutsCan. Be appreciated that the degree of depth of cavity is greater than the height of the artificial rock's model that will make, so that by Artificial RockStone model compacting. Preferably, the degree of depth of cavity is normally according to 1.5～2 of the length and width of artificial rock's model or heightProportionality design doubly.
In the hot pressing die of above-mentioned manufacturing artificial petrophysical model, preferably, what described wearing layer was formed in one quenchesFire steel wearing layer or integrated hardened steel wearing layer or surrounded by polylith quenched nickelclad and/or hardened steel plate wear-resistingLayer, carbon steel bearing course that described bearing course is formed in one (more preferably integrated 45#Ordinary steel bearing course),Described heat insulation layer is fibrous glass insulation layer, asbestos heat insulation layer, rock wool heat insulation layer or silicate heat insulation layer etc., described mouldTool pressure head is hardened steel mould pressure head, and described base is hardened steel base. About wearing layer, quenched nickelclad and/or hardChanging the quantity of steel plate can be designed according to the concrete shape of cavity by those skilled in the art, for example, when cavity transversalWhen face is rectangle, the wearing layer that can adopt four quenched nickelclads and/or hardened steel plate to surround; When cavity cross section isWhen circular, the wearing layer that can adopt two semicircle quenched nickelclads and/or hardened steel plate to surround splices. CloseIn heat insulation layer, also can adopt multiple pieces of glass fiberboard, polylith asbestos board, polylith rock cotton board or polylith silicate board to spellConnect and form, as long as closely wrap up upper surface, lower surface and the outer surface of bearing course. Adopt heat insulation layer parcel to holdWhile pressing layer, should at least make the bottom surface of the die ontology after parcel in same level, that is to say, can at least makeThe bottom close contact heat insulation layer of the outer surface of wearing layer.
In the hot pressing die of above-mentioned manufacturing artificial petrophysical model, preferably, the thickness of described wearing layer is1.5～5.5cm, the thickness of described bearing course is 6～16cm, the thickness of described heat insulation layer is 2～4cm, described baseThickness is 2～4cm.
In the hot pressing die of above-mentioned manufacturing artificial petrophysical model, preferably, the quantity of described heater is 6～10Individual. These heaters can be evenly arranged in bearing course.
In the hot pressing die of above-mentioned manufacturing artificial petrophysical model, preferably, the side wall surface of described mould pressure head is provided withMany connect upper and lower air guide groove. More preferably, the degree of depth of described air guide groove is 0.3～1mm. Conventionally cylinder shapeThe mould pressure head of shape can seamlessly be embedded in the cavity of die ontology, the cavity inner wall of mould pressure head side and die ontologyThe laminating degree of (being wearing layer) is high, and in pressure process, pressure head presses down, and discharges air in cavity, produces in inside cavityRaw negative pressure, is difficult to pressure head again to take out, and therefore, at the side wall surface of pressure head, air guide groove is set, the establishing of air guide groovePut can do not affect sample press form under the prerequisite of type, make cavity internal and external pressure balance, be convenient to powder or granular materialsFilling and pressurization make.
In the hot pressing die of above-mentioned manufacturing artificial petrophysical model, preferably, the upper surface of described bearing course, following tableBetween face and outer surface and described heat insulation layer, be screwed and be connected. The quantity of screw can be by art technology peopleMember carries out routine and selects.
According to the specific embodiment of the present invention, preferably, the hot pressing die of above-mentioned manufacturing artificial petrophysical model also wrapsDraw together some demoulding fixed heads (also can be called handle), they are symmetricly set in the outer surface of described heat insulation layer. De-Mould fixed head can be connected in the outer surface of heat insulation layer by conventional methods, and it mainly plays in the process of the demoulding and liftsRise the effect of described die ontology.
In the hot pressing die of above-mentioned manufacturing artificial petrophysical model, preferably, the bottom of described heat insulation layer is provided with props upSpike. The quantity of feet can be carried out routine selection by those skilled in the art, and its effect is for supporting described mouldTool body, and make on its work top that is stably positioned over forcing press.
According to the specific embodiment of the present invention, preferably, the hot pressing die of above-mentioned manufacturing artificial petrophysical model also wrapsDraw together substrate, described substrate is arranged at the bottom of described die ontology, and tight with described base, wearing layer and heat insulation layerConnect airtight tactile. Described substrate can be hardened steel substrate, and its thickness can be 1～4cm. Can be screwed connectionSubstrate and heat insulation layer. In addition, more preferably, the bottom of described substrate is provided with feet.
Hardened steel described in the present invention, hardened steel, carbon steel (comprise 45#Ordinary steel) be the steel of prior art.Glass fibre described in the present invention, asbestos, rock wool and silicate are the heat-insulating material of prior art.
The hot pressing die of manufacturing artificial petrophysical model provided by the invention can be placed in forcing press and use, thermoelectricity whereinIdol and heater can be connected in humidostat, so that mould is heated up and temperature control; Pressure head can connect pressureThe pressure cylinder of power machine, and can adopt pressure controller to regulate and control the pressure of pressurization.
The hot pressing die of manufacturing artificial petrophysical model of the present invention, the hardness of hardened steel and hardened steel and manufacturing artificial rockThe Mohs' hardness of the quartz material that model uses is suitable, the wearing layer, the end that in the present invention, directly contact with quartz materialSeat and mould pressure head are hardened steel or hardened steel material, can tolerate well quartz material pair in pressing processThe wearing and tearing of mould, have effectively protected mould. The sidewall of cavity is double-layer nested structure, arranges in internal layer wearing layer peripheryThere is bearing course, the complete close contact of wearing layer and bearing course, in the process that applies directed pressure, what use is artificialThe pressure that petrophysical model material produces mould side wall conducts to bearing course by wearing layer, has guaranteed the peace of experimentationEntirely, quenching steel have effectively been made up or sclerosis steel fragility greatly, does not almost have plasticity, in pressing process, easily occursBurst apart fragmentation and cause the experiment defect such as cause danger. And the present invention has designed heater and thermoelectricity in bearing courseIdol, is particularly useful for making the hot-forming artificial rock's models of need such as shale physical model kerogenous, has solvedThe problem that in prior art, cold-press process exists. Therefore, the hot pressing die of manufacturing artificial petrophysical model provided by the inventionThere is good wearability and compressive property, can guarantee the safety of experimentation, and can be used in making containing kerogenShale physical model etc. need hot-forming artificial rock's model.
In sum, the preparation method of the kerogenous shale physical model based on hot pressing provided by the invention is to connect very muchA kind of physical model preparation method of nearly natural shale diagenetic environment and Rock-forming Mechanism. And, obtain by this preparation methodHaving arrived every petrophysical parameter, mechanical characteristics, seismic character, microstructure and diagenesis condition approaches natural moreThe shale physical model kerogenous of shale.
Brief description of the drawings
The preparation method flow process of the kerogenous shale physical model based on hot pressing that Fig. 1 provides for the embodiment of the present invention 1Figure.
The schematic appearance of the shale physical model kerogenous that Fig. 2 a and Fig. 2 b provide for the embodiment of the present invention 1.
The shear wave that Fig. 3 a and Fig. 3 b are respectively the shale physical model kerogenous that the embodiment of the present invention 1 provides respectively toOpposite sex oscillogram and velocity of wave figure;
The compressional wave that Fig. 3 c and Fig. 3 d are respectively the shale physical model kerogenous that the embodiment of the present invention 1 provides respectively toOpposite sex oscillogram and velocity of wave figure;
Fig. 4 a and Fig. 4 b are respectively the shale physical model kerogenous that natural shale and the embodiment of the present invention 1 providePerpendicular to the electron scanning micrograph of bedding direction;
Fig. 4 c and Fig. 4 d are respectively the shale physical model kerogenous that natural shale and the embodiment of the present invention 1 provideBe parallel to the electron scanning micrograph of bedding direction;
The page kerogenous that Fig. 5 a, Fig. 5 b, Fig. 5 c and Fig. 5 d provide for natural shale and the embodiment of the present invention 1The kerogen electron scanning micrograph of rock physical model;
The structural representation of the hot pressing die of the manufacturing artificial petrophysical model that Fig. 6 provides for the embodiment of the present invention 2;
Fig. 7 is the knockout course schematic diagram after the embodiment of the present invention 2 manufacturing artificial petrophysical models finish;
Number in the figure:
1: mould pressure head; 2: die ontology; 3: cavity; 4: air guide groove; 5: wearing layer; 6: bearing course;7: base; 8: screw; 9: artificial rock's model sample; 10: cushion block; 11: thermocouple; 12: heater;13: heat insulation layer; 14: demoulding fixed head.
Detailed description of the invention
Understand for technical characterictic of the present invention, object and beneficial effect being had more clearly, existing to skill of the present inventionArt scheme is carried out following detailed description, but can not be interpreted as restriction that can practical range of the present invention.
Embodiment 1
The present embodiment provides a kind of preparation method of the kerogenous shale physical model based on hot pressing, as Fig. 1 instituteShow, it comprises the following steps:
Be that 3000 object silicon powder 300g, fineness are that 4000 object illite 250g, fineness are 4000 by finenessObject calcite 25g and kerogen 100g place after 48h respectively in 50 DEG C of insulating boxs, take out and put into ball millIn carry out ball milling mixing, ball milling adopts the combination of the ball milling pearl of large, medium and small three sizes, wherein, large ball milling pearlDiameter is 15mm, and the diameter of middle ball milling pearl is 12mm, and the diameter of bead mill pearl is 5mm, and, big or middle,The number ratio of the ball milling pearl of little three sizes is 14:23:84, and the rotating speed of ball mill is 425.4R/min, Ball-milling TimeFor 48h, obtain mixed powder;
(it is limited that Yancheng one adds one electronic material in described mixed powder, to add YY4250A/B series epoxy adhesiveCompany, the solidification temperature of this YY4250A/B series epoxy adhesive is 130 DEG C/2h～150 DEG C/2h, and A whereinGlue proportion is 1.15g/cc, and B glue proportion is 1.10g/cc), and the weight ratio of described mixed powder and described binding agentFor 10:1, adopt the manual mode of milling and sieving, finally make the above mixed material of 99% (percentage by weight) canBy 300 object sieves, obtain uniform mixed material;
The cavity inner wall, base and the pressure head bottom surface that clean and assemble complete hot pressing die are smeared to vaseline or siliconOil, after entirely lay enters in mould by mixed material described in 100g, puts into pressure head, uses rubber hammer to knock with sudden forcePressure head end face 200～300 times, will add second part of 100g mixed material, then put into after Bas Discharged in mixed materialPressure head, uses rubber hammer to knock with sudden force pressure head end face 200～300 times, circulates until mixed material is all loaded with thisEnter in mould and carry out pre-compacted process after (altogether can lay 6 times, put into for the last time 175g mixed material),Obtain being equipped with the mould of mixed material;
The described mould that mixed material is housed is placed on press, under normal temperature condition, directly bears at mixed materialUnder the constant pressure of 20MPa, keep carrying out half an hour, after final pre-compacted processing, mould being heated to130 DEG C, after in mould, mixed material is heated evenly, the pressure that mixed material is born is adjusted to 200MPa and protectsHold constant, heat-insulation pressure keeping 4880min under this stationary temperature and pressure condition, treat the heat-insulation pressure keeping time arrive setValue, sheds pressure and stops after thermal protection, and mold temperature is adjusted to 37 DEG C, and carries out again the demoulding after being incubated 24h,To shale physical model kerogenous.
The edge of the shale physical model obtaining can be polished smooth, and can be by modes such as cutting drill strings by itBe processed into needed shape and size.
The schematic appearance of this shale physical model kerogenous is as Fig. 2 a (before cutting drill string) and Fig. 2 b (cuttingAfter drill string) shown in.
The density of the shale physical model kerogenous that after tested, the present embodiment provides is about 2.136g/cc; HoleDegree is about 2.29%; Permeability is about 0.0028mD; The velocity of longitudinal wave that is parallel to bedding direction is about 3721m/s, fastShear wave velocity is about 2243m/s, and slow shear wave velocity is about 2045m/s; Velocity of longitudinal wave perpendicular to bedding direction is about3177m/s, fast transverse wave speed is about 2037m/s, and slow shear wave velocity is about 2036m/s (as Fig. 3 a, Fig. 3 b, figureShown in 3c, Fig. 3 d). Therefore the compressional wave anisotropy that draws this shale physical model kerogenous is 16.9%, horizontal strokeRipple anisotropy is 10.2%, meets strong anisotropic requirement.
The actual density containing the natural shale in crack is 2.01～2.64g/cc, and porosity is for being less than 5%, and permeability is less than0.1mD(BOWKERKA.BarnettShalegasproduction,FortWorthBasin:issuesandDiscussion[J] .AAPGBulletin, 2007,91 (4): 523-533), ripple anisotropy is all greater than 10% in length and breadth(ThomsenL.Weakelasticanisotropy[J].GEOPHYSICS,1986,51(10):1954-66.)。
Therefore, the present embodiment provides above parameters and the actual fracture reservoir rock of shale physical model kerogenousStone physical parameter and seismic wave response approach.
The bulk modulus of the shale physical model kerogenous that the present embodiment provides is 15.4Gpa, and modulus of shearing is11.8Gpa, Young's modulus is 28.3Gpa, Poisson's ratio is 0.194. The different buried depths in different regions are dissimilarMechanical property parameter with the natural shale of component differs larger, but the artificial shale physics that the present embodiment preparesThe above-mentioned mechanical property parameter of model is all in the effective range of natural shale mechanical property parameter.
As Fig. 4 a and Fig. 4 b (perpendicular to bedding direction), Fig. 4 c and Fig. 4 d (being parallel to bedding direction), Fig. 5 a (SaeedZargariet.al.,2013,Organicmaturity,elasticproperties,andtexturalcharacteristicsofselfResourcingreservoirs, GEOPHYSICS, VOL.78, NO.4), Fig. 5 b (the present embodiment), Fig. 5 c (Saeed Zargariet.al.,2013,Organicmaturity,elasticproperties,andtexturalcharacteristicsofselfResourcingreservoirs, GEOPHYSICS, VOL.78, NO.4) and Fig. 5 d (the present embodiment) shown in, shouldThe microstructure height of the vertical stratification of shale physical model and parallel bedding direction and natural shale correspondence direction is approximate,Can observe obvious layering and/or stacked in layers structure, the kerogen of this shale physical model is mobile simultaneouslyShape and near-spherical, the kerogen of its microstructure spatial and natural shale is similar.
Wherein, density, porosity, velocity of longitudinal wave, shear wave velocity, compressional wave anisotropy, shear wave anisotropy, bodyThe survey that the test of product module amount, modulus of shearing, Young's modulus, Poisson's ratio and computational methods are known to the skilled personExamination and computational methods, specifically please refer to " petrophysics " (publishing house of Chinese University of Science and Technology, 12.4,288 pages, 13.1,293 pages) described in test and computational methods.
Embodiment 2
Shown in Figure 6, the hot pressing die of its manufacturing artificial petrophysical model providing for the present invention's one specific embodimentStructural representation, this hot pressing die at least comprises die ontology 2 and mould pressure head 1; Wherein,
Described die ontology 2 has the cavity 3 for manufacturing artificial petrophysical model, and the bottom of cavity 3 is provided with base7, the surrounding of cavity 3 and base 7 has wearing layer 5, and the outer surface of wearing layer 5 has bearing course 6, bearing course6 upper surface, lower surface and outer surface has heat insulation layer 13 and is fixedly connected with by screw 8, base 7 withClose contact between wearing layer 5, close contact between wearing layer 5 and bearing course 6, wearing layer 5, bearing course 6 are equalAnd close contact between heat insulation layer 13, and in bearing course 6, be provided with thermocouple 11 and some heaters 12;
The front end face of described mould pressure head 1 is the plane consistent with the cavity cross section shape of die ontology 2, Ke YiliSeparate, mould pressure head is generally the cylinder body shape matching with the cavity of cavity 3, and at the side wall surface of mould pressure head 1Equally distributed air guide groove 4 is set.
As the optional detailed description of the invention of one, the hot pressing die of above-mentioned manufacturing artificial petrophysical model has following materialMatter and size: described base 7 is hardened steel base, its length × wide × height is 70mm × 70mm × 20mm, described skyThe length in chamber 3 × wide × be 70mm × 70mm × 140mm deeply, its cross section is square, its for pressed section for justSquare artificial rock's model sample; Described wearing layer 5 is surrounded by the quenched nickelclad of 4 thickness 25mm, and hardness is high,Wearability is good, directly contacts with pressed powder or particle, plays protection mould and avoids the effect scratching; Described bearing course6 be formed in one 45#Ordinary steel bearing course, its thickness is 70mm, its good toughness, with hardened steel wearing layer 5Between complete close contact, in the process that applies directed pressure, powder or particle produce die ontology 2 sidewallsPressure conducts to integrated 45 by hardened steel wearing layer 5#Ordinary steel bearing course 6, therefore, this mould is being protectedWhen protecting mould, guarantee the safety of experimentation; The quantity of described heater 12 is 6, and they are at bearing courseIn 6, be evenly arranged; The asbestos board that described heat insulation layer 13 is 20mm for several thickness surrounds, and insulation effect is good, andAnd upper surface, lower surface and outer surface close contact with bearing course 6; Described mould pressure head 1 is hardened steel mouldPressure head, the square that its cross section is 70mm × 70mm, the cavity 3 that it can substantially seamless embedding die ontology 2In, the side wall surface of mould pressure head 1 is uniformly distributed 0.5mm degree of depth air guide groove 4 and can makes do not affecting sample pressure knotUnder the prerequisite of moulding, make cavity internal and external pressure balance, filling and the pressurization of being convenient to powder or granular materials are made.
The hot pressing die of the manufacturing artificial petrophysical model that the present embodiment provides can be placed in forcing press and use, heat whereinGalvanic couple 11 and heater 12 can be connected in humidostat, so that mould is heated up and temperature control; Mould is pressed1 can Bonding pressure machine pressure cylinder, and adopt pressure controller to regulate and control the pressure of pressurization.
In addition,, in order to facilitate carrying and the demoulding of die ontology, can be symmetrical arranged two at the outer surface of heat insulation layer 13Individual demoulding fixed head 14. Can also feet be set in the bottom of described heat insulation layer 13, for example, can arrange fourSpike.
Utilize the concrete side of the hot pressing die compacting artificial rock model sample of the manufacturing artificial petrophysical model of the present embodimentMethod as described in Example 1, repeats no more herein.
As shown in Figure 7, in the process of the demoulding, can utilize steel cable connect demoulding fixed head 14 so that by mould thisBody 2 liftings are got up, below heat insulation layer 13, add simultaneously cushion block 10, the height of cushion block 10 can be greater than pressThe height of artificial rock's model sample 9 of system, then continues slowly pressurization above mould pressure head 1, can be by peopleWork petrophysical model sample 9 takes out.
Claims (11)
1. a preparation method for the kerogenous shale physical model based on hot pressing, it comprises the following steps:
Silicon powder, calcite, illite and kerogen are carried out to ball milling mixing, obtain mixed powder;
In described mixed powder, add binding agent, after mixing, obtain mixed material;
By described mixed material successively lay enter in hot pressing die, and carry out pre-compacted after every lay one deck mixed materialProcess, obtain being equipped with the mould of mixed material;
The described mould that mixed material is housed is carried out after the final pre-compacted processing of normal temperature, then heat and pressurize and be incubatedPressurize processing, obtains shale physical model kerogenous.
2. preparation method according to claim 1, wherein, taking the gross weight of described mixed powder as benchmark,The content of described silicon powder is 20%～60%, and the content of described calcite is 1%～25%, described illitic contentBe 15%～50%, described kerogenic content is 2%～15%; And the fineness of described silicon powder is 3000～4000Order, the fineness of described calcite is 3000～4000 orders, described illitic fineness is 3000～4000 orders.
3. preparation method according to claim 1, it is further comprising the steps of: at described silicon powder, Fang XieStone, illite and kerogen carry out before ball milling mixing, first by they process processed; Preferably, this processedBe described silicon powder, calcite, illite and kerogen are placed to 48h in 40～60 DEG C of insulating boxs more than.
4. preparation method according to claim 1, wherein, described ball milling adopts large, medium and small three sizesThe combination of ball milling pearl, the diameter range of large ball milling pearl is 15～20mm, the diameter range of middle ball milling pearl is10～15mm, the diameter of bead mill pearl is 5～10mm; Preferably, the ball milling pearl of described large, medium and small three sizesNumber ratio be (10～20): (20～25): (80～100); The rotating speed of the ball mill that more preferably, described ball milling adoptsBe 350～450R/min, Ball-milling Time is 36～48h.
5. preparation method according to claim 1, wherein, the weight of described mixed powder and described binding agentThan being 10:1～10:2.
6. preparation method according to claim 1, wherein, described binding agent comprises YY4250A/B series of loopsOxygen binding agent; Preferably, the solidification temperature of described YY4250A/B series epoxy adhesive is 130 DEG C/2h～150 DEG C/ 2h; More preferably, in described YY4250A/B series epoxy adhesive, A glue proportion is 1.15g/cc, B glue proportionFor 1.10g/cc.
7. preparation method according to claim 1, wherein, the mixing of described mixed powder and described binding agentBe to adopt the manual mode of milling and sieving, and more than 99% mixed material of weight can be sieved by 300 objectsSon.
8. preparation method according to claim 1, wherein, by described mixed material successively lay enter hot-dieLay number of times in tool is 4-6 time.
9. preparation method according to claim 1, wherein, carries out often the described mould that mixed material is housedThe final pre-compacted processing of temperature is to make described mixed material bear the pressure of 5MPa～20MPa pressurize 0.4～1h.
10. preparation method according to claim 1, in described heating pressurization heat-insulation pressure keeping processing procedure, instituteStating the pressure that mixed material bears is 100MPa～517.5MPa, and the temperature of heating is 100 DEG C～250 DEG C, heat-insulation pressure keepingTime be 3600～5760min.
11. 1 kinds of shale physical models kerogenous, its be by described in claim 1-10 any one based on hot pressingThe preparation method made of kerogenous shale physical model obtain; Preferably, this shale physics kerogenousThe density of model is greater than 2.0g/cc, and porosity is less than 5%, and permeability is less than 0.1mD, and velocity of longitudinal wave is2500m/s～4500m/s, Shear Waves Splitting speed is 1500m/s～3000m/s, and ripple anisotropy is all greater than 10% in length and breadth,And this shale physical model kerogenous is at vertical stratification and parallel bedding direction and natural shale correspondence directionMicrostructure is approximate, has obvious layering and/or stacked in layers structure, simultaneously this shale physics kerogenousThe kerogenic microstructure spatial of model and the kerogen of natural shale are similar.
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