CN104692726B - A kind of preparation method of hard fragility hydration of clay shale artificial core - Google Patents

A kind of preparation method of hard fragility hydration of clay shale artificial core Download PDF

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CN104692726B
CN104692726B CN201510077223.2A CN201510077223A CN104692726B CN 104692726 B CN104692726 B CN 104692726B CN 201510077223 A CN201510077223 A CN 201510077223A CN 104692726 B CN104692726 B CN 104692726B
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hydration
behavior
dispersant
hard
bentonite
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CN104692726A (en
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卢运虎
陈勉
金衍
杨帅
刘铭
侯冰
杜晓雨
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China University of Petroleum Beijing
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Abstract

The invention discloses the preparation method of a kind of hard fragility hydration of clay shale artificial core, it comprises the following steps according to sequencing: the test clay mineral component on hard brittle shale stratum, comprcssive strength, hydration swelling, and calculates comprehensive brittleness index;Determine the type of cement, bentonite, dispersant;Prepare the bentonite of Different adding amount and the Behavior of Hardened Cement Paste of dispersant, the comprcssive strength of Behavior of Hardened Cement Paste, comprehensive brittleness index, hydration swelling under the different compound proportion of test;Set up the graph of a relation between comprcssive strength, comprehensive brittleness index, hydration swelling compound proportion different from Behavior of Hardened Cement Paste respectively;Determine the compound proportion meeting the cement of hard brittle shale stratum characteristic, bentonite, dispersant;Prepare hard fragility hydration of clay shale artificial core.The preparation method of the present invention is easily understood, simple operation, can obtain the fragility Behavior of Hardened Cement Paste with some strength, easy hydration swelling, it is possible to simulate the mechanical characteristics on hard brittle shale stratum really and accurately.

Description

A kind of preparation method of hard fragility hydration of clay shale artificial core
Technical field
The invention belongs to oil gas drilling field of engineering technology, relate to the preparation method of artificial core, particularly relate to A kind of preparation method of hard fragility hydration of clay shale artificial core.
Background technology
There is the problems such as fragility is strong, intensity is high, easy hydration swelling due to hard brittle shale reservoir, therefore exist Drilling process often occurs serious borehole well instability phenomenon, such as pit shaft undergauge, hole collapse, drilling fluid The problems such as leakage and formation damage.The complicated state of correct understanding effectively analysis stratum host rock environment, probes into The mechanism of wellbore stability, sets up Controlling model, the borehole well instability problem effectively reducing and controlling in drillng operation, To realize safety, high-quality, efficiently, low cost drilling well significant.
At present, keep wellbore stability important research direction be evaluate the intensity of hard brittle shale, brittleness and Hydration swelling feature, but for bad ground, owing to on-the-spot coring is costly and difficult, this will be serious The restriction research to borehole well instability problem.Therefore, it is to grind by prepare artificial core doing simulation test in indoor Study carefully the important technical of borehole well instability problem in drilling process.
At present, artificial core is how as raw material or direct by on-the-spot landwaste compacting using cement and quartz sand Become, but this can not accurately reflect the hydration swelling feature on hard brittle shale stratum.On the one hand, quartz sand Skeleton as artificial core also exists the problem that fragility is poor;On the other hand, if artificial core is only by water Mud and bentonite are formulated, although its fragility and hydration swelling disclosure satisfy that the requirement of simulation test, but Being as the increase of bentonite content, the comprcssive strength of artificial core is substantially reduced, and is unsatisfactory for test demand.
Therefore, it is badly in need of developing the preparation method of a kind of hard fragility hydration of clay shale artificial core, by prepared Artificial core is used for simulation test, to study borehole well instability problem.
Summary of the invention
For solving problems of the prior art, the present invention provides a kind of hard fragility hydration of clay shale people's lithogenesis The preparation method of the heart, it comprises the following steps according to sequencing:
Step one: the test clay mineral component on hard brittle shale stratum, comprcssive strength, hydration swelling, meter Calculate the comprehensive brittleness index on hard brittle shale stratum;
Step 2: determine the type of cement, bentonite, dispersant;
Step 3: the type of cement, bentonite, dispersant determined by according to, prepares the swelling of Different adding amount Soil and the Behavior of Hardened Cement Paste of dispersant, and test the comprcssive strength of Behavior of Hardened Cement Paste, comprehensive fragility under different compound proportion and refer to Number, hydration swelling;
Step 4: comprcssive strength, the comprehensive fragility of Behavior of Hardened Cement Paste are referred to by bentonite and the dispersant of analyzing Different adding amount Number, the impact of hydration swelling, set up comprcssive strength, comprehensive brittleness index, hydration swelling and water respectively Graph of a relation between mudstone difference compound proportion;
Step 5: according to comprcssive strength, comprehensive brittleness index, hydration swelling compound proportion different from Behavior of Hardened Cement Paste it Between graph of a relation, determine meet the cement of hard brittle shale stratum characteristic, bentonite, dispersant compounding Ratio;
Step 6: the compound proportion of cement, bentonite, dispersant determined by according to, prepares hard fragility hydration of clay Shale artificial core.
The preparation method of the hard fragility hydration of clay shale artificial core of the present invention, it is first determined hard brittle shale The features such as the clay mineral component on stratum, hydration swelling, rock brittleness and intensity, then set up aquation swollen Graph of a relation between swollen property, brittleness, intensity from cement, bentonite, the different compound proportion of dispersant, then root The optimal compounding side of the hard fragility hydration of clay shale artificial core being suitable for simulating this stratum is determined according to graph of a relation Case.The artificial core prepared by the method is similar to the mechanical properties of rock on true stratum to the full extent, Can adapt to three axle rock mechanics experiments and hydration swelling test, the most further understanding shale reservoir The mechanical characteristics, beneficially Efficient Development mud such as feature and the simulation hydration swelling of mud shale, fragility, intensity Shale oil gas.
Preferably, in described step one, at least choose five pieces of hard brittle shale formation sample, survey respectively Examination clay mineral component, comprcssive strength, hydration swelling, calculate comprehensive brittleness index respectively, to test knot Fruit and result of calculation are averaged.For a certain depth segment hard brittle shale stratum, to well drilling detritus or Drilling extracting core carries out test processing, obtains testing required standard specimen.At least five pieces of standard specimens are carried out Clay mineral component, comprcssive strength, hydration swelling, the test of fragility or calculating, then average, This meansigma methods can show the features such as the clay mineral component on this stratum, hydration swelling, intensity, brittleness.
In any of the above-described scheme preferably, X-ray diffraction experimental test hard brittle shale stratum is used Clay mineral component.Method of X-ray diffraction have do not damage formation rock sample, pollution-free, quick, Certainty of measurement advantages of higher to mineral constituent.
In any of the above-described scheme preferably, rock mechanics experiment test hard brittle shale stratum is used Tensile strength.
In any of the above-described scheme preferably, the water on linear expansion instrument test hard brittle shale stratum is used Change dilatancy.
In any of the above-described scheme preferably, according to test comprcssive strength the stress-strain diagram meter obtained time Calculate the comprehensive brittleness index on hard brittle shale stratum.Computational methods areThis comprehensive brittleness index IBIt it is the meansigma methods after elastic modulus E and the normalization of Poisson's ratio v.
In any of the above-described scheme preferably, in described step 2, resisting according to hard brittle shale stratum Compressive Strength determines cement type.
In any of the above-described scheme preferably, the standard testing intensity of cement determined by is not less than is tested The comprcssive strength on hard brittle shale stratum.
In any of the above-described scheme preferably, cement determined by is Portland cement, complex silicate Any one in salt cement, special cement.
In any of the above-described scheme preferably, described special cement be lumnite cement, oil-well cement, Any one in sulfate resisting Portland cement.
In any of the above-described scheme preferably, in described step 2, gluing according to hard brittle shale stratum Soil mineral constituent determines bentonite type.
In any of the above-described scheme preferably, bentonite determined by is sodium bentonite or calcio swelling Soil.If smectite content is higher in the clay mineral on hard brittle shale stratum, then select sodium bentonite; If illite content is higher in the clay mineral on hard brittle shale stratum, then select calcium-base bentonite.
In any of the above-described scheme preferably, in described step 2, the method determining Dispersant types, press Comprise the following steps according to sequencing:
Step one: mixed with bentonite by fixed cement, cement and bentonitic weight ratio are 9:1, join Make three parts of identical mixture;
Step 2: add the dissimilar dispersant of identical weight respectively in three parts of mixture, prepares three kinds of cement Stone;
Step 3: use the content of hydrated calcium silicate in three kinds of Behavior of Hardened Cement Pastes of X-ray diffraction experimental test;
Step 4: according to the content of hydrated calcium silicate, determine the type of dispersant.
In any of the above-described scheme preferably, dispersant determined by be sodium lignin sulfonate, citric acid, Any one in Sulfonated Copolymer of Styrene and Maleic Anhydride.
The Main Function of dispersant is to reduce the bentonite Ca to hydrated cementitious2+Absorption, suppresses hydrated product water Change the minimizing of calcium silicates (CSH).By the containing of hydrated calcium silicate in X-ray diffraction experimental test Behavior of Hardened Cement Paste Amount, selects the dispersant that hydrated calcium silicate content is high.
In any of the above-described scheme preferably, in described step 3, comprise only cement, do not contain bentonite Time, the addition of dispersant is the 0.5% of cement weight, 0.6%, 0.7%, 0.8%, 0.9%, 1.0%, joins Make six kinds of Behavior of Hardened Cement Pastes.
In any of the above-described scheme preferably, in described step 3, cement and bentonitic weight ratio are 9:1 Time, the addition of dispersant is cement with the 0.5% of bentonite weight sum, 0.6%, 0.7%, 0.8%, 0.9%, 1.0%, prepare six kinds of Behavior of Hardened Cement Pastes.
In any of the above-described scheme preferably, in described step 3, cement and bentonitic weight ratio are 8:2 Time, the addition of dispersant is cement with the 0.5% of bentonite weight sum, 0.6%, 0.7%, 0.8%, 0.9%, 1.0%, prepare six kinds of Behavior of Hardened Cement Pastes.
In any of the above-described scheme preferably, in described step 3, cement and bentonitic weight ratio are 7:3 Time, the addition of dispersant is cement with the 0.5% of bentonite weight sum, 0.6%, 0.7%, 0.8%, 0.9%, 1.0%, prepare six kinds of Behavior of Hardened Cement Pastes.
In any of the above-described scheme preferably, in described step 4, comprcssive strength, comprehensive brittleness index, Between hydration swelling compound proportion different from Behavior of Hardened Cement Paste, the foundation of graph of a relation, includes following according to sequencing Step:
Step one: Behavior of Hardened Cement Paste comprcssive strength C that test is obtained and bentonite addition W1With dispersant addition W2Carry out nonlinear fitting, obtain determining the functional relation C=F (W of Behavior of Hardened Cement Paste comprcssive strength1, W2);
Step 2: the stress-strain diagram obtained during according to test Behavior of Hardened Cement Paste comprcssive strength calculates the most crisp of Behavior of Hardened Cement Paste Sex index, by comprehensive for calculated Behavior of Hardened Cement Paste brittleness index IBWith bentonite addition W1Add with dispersant Amount W2Carry out nonlinear fitting, obtain determining the functional relationship Formulas I of the comprehensive brittleness index of Behavior of Hardened Cement PasteB=F (W1, W2);
Step 3: the Behavior of Hardened Cement Paste hydration swelling E that test is obtained and bentonite addition W1With dispersant addition W2Carry out nonlinear fitting, obtain determining the functional relation E=F (W of Behavior of Hardened Cement Paste hydration swelling1, W2);
Step 4: the functional relation obtained according to analytical calculation, set up respectively comprcssive strength, comprehensive brittleness index, Graph of a relation between hydration swelling compound proportion different from Behavior of Hardened Cement Paste.
In any of the above-described scheme preferably, in described step 5, determine and meet hard brittle shale stratum The cement of feature, bentonite, the method for compound proportion of dispersant, comprise the following steps according to sequencing:
Step one: determine and meet the bentonite addition W that hard brittle shale stratum aquation dilatancy requires1
Step 2: determine and meet the dispersant addition W that hard brittle shale stratum comprcssive strength requires2a
Step 3: determine and meet the dispersant addition W that the comprehensive brittleness index in hard brittle shale stratum requires2b
Step 4: determine that meet hard brittle shale stratum comprcssive strength requires and the requirement of comprehensive brittleness index simultaneously Dispersant addition W2
In any of the above-described scheme preferably, in described step one, according to the hard brittle shale tested Graph of a relation between stratum aquation dilatancy and the hydration swelling set up compound proportion different from Behavior of Hardened Cement Paste, Determine bentonite addition W1
In any of the above-described scheme preferably, in described step 2, according to the hard brittle shale tested Graph of a relation between stratum comprcssive strength and the comprcssive strength set up compound proportion different from Behavior of Hardened Cement Paste, really Determine bentonite addition W1Under conditions of, determine dispersant addition W2a
In any of the above-described scheme preferably, in described step 3, according to the hard brittle shale tested Relation between the comprehensive brittleness index in stratum and the comprehensive brittleness index set up compound proportion different from Behavior of Hardened Cement Paste Figure, is determining bentonite addition W1Under conditions of, determine dispersant addition W2b
In any of the above-described scheme preferably, in described step 4, dispersant addition W2=(W2a+W2b) /2。
In any of the above-described scheme preferably, in described step 6, hard fragility hydration of clay shale artificial core Preparation, comprise the following steps according to sequencing:
Step one: the cement having determined that compound proportion is mixed with bentonite;
Step 2: be added to have determined that the dispersant of compound proportion, then add water, mix, is formed Mixture;
Step 3: watered by mixture and build up Behavior of Hardened Cement Paste, after Behavior of Hardened Cement Paste drying and moulding, i.e. can get hard fragility aquation Mud shale artificial core.After Behavior of Hardened Cement Paste drying and moulding, maintenance 28 days.
The preparation method of the hard fragility hydration of clay shale artificial core of the present invention, is easily understood, simple operation, Material therefor is simple, with low cost, can obtain having some strength, easy hydration swelling by the method Fragility Behavior of Hardened Cement Paste, it is possible to simulate the mechanical characteristics on hard brittle shale stratum really and accurately.
Accompanying drawing explanation
Fig. 1 is a preferred embodiment of the preparation method according to the present invention hard fragility hydration of clay shale artificial core Flow chart;
Fig. 2 be the preparation method according to the present invention hard fragility hydration of clay shale artificial core Fig. 1 shown in implement Hydration swelling and the graph of a relation of bentonite addition in example;
Fig. 3 be the preparation method according to the present invention hard fragility hydration of clay shale artificial core Fig. 1 shown in implement Comprcssive strength and the graph of a relation of Behavior of Hardened Cement Paste compound proportion in example;
Fig. 4 be the preparation method according to the present invention hard fragility hydration of clay shale artificial core Fig. 1 shown in implement Comprehensive brittleness index and the graph of a relation of Behavior of Hardened Cement Paste compound proportion in example;
Fig. 5 be the preparation method according to the present invention hard fragility hydration of clay shale artificial core Fig. 1 shown in implement Actual formation and artificial core mechanical property comparison diagram in example;
Fig. 6 is that another of the preparation method according to the present invention hard fragility hydration of clay shale artificial core is preferable to carry out Hydration swelling and the graph of a relation of bentonite addition in example;
Fig. 7 be the preparation method according to the present invention hard fragility hydration of clay shale artificial core Fig. 6 shown in implement Comprcssive strength and the graph of a relation of Behavior of Hardened Cement Paste compound proportion in example;
Fig. 8 be the preparation method according to the present invention hard fragility hydration of clay shale artificial core Fig. 6 shown in implement Comprehensive brittleness index and the graph of a relation of Behavior of Hardened Cement Paste compound proportion in example;
Fig. 9 be the preparation method according to the present invention hard fragility hydration of clay shale artificial core Fig. 6 shown in implement Actual formation and artificial core mechanical property comparison diagram in example.
Detailed description of the invention
In order to be further understood that the summary of the invention of the present invention, elaborate this below in conjunction with specific embodiment Invention.
Embodiment one:
As it is shown in figure 1, the preparation method of a kind of hard fragility hydration of clay shale artificial core, it is according to the most suitable Sequence comprises the following steps:
Step one: the test clay mineral component on hard brittle shale stratum, comprcssive strength, hydration swelling, meter Calculate the comprehensive brittleness index on hard brittle shale stratum;
Step 2: determine the type of cement, bentonite, dispersant;
Step 3: the type of cement, bentonite, dispersant determined by according to, prepares the swelling of Different adding amount Soil and the Behavior of Hardened Cement Paste of dispersant, and test the comprcssive strength of Behavior of Hardened Cement Paste, comprehensive fragility under different compound proportion and refer to Number, hydration swelling;
Step 4: comprcssive strength, the comprehensive fragility of Behavior of Hardened Cement Paste are referred to by bentonite and the dispersant of analyzing Different adding amount Number, the impact of hydration swelling, set up comprcssive strength, comprehensive brittleness index, hydration swelling and water respectively Graph of a relation between mudstone difference compound proportion;
Step 5: according to comprcssive strength, comprehensive brittleness index, hydration swelling compound proportion different from Behavior of Hardened Cement Paste it Between graph of a relation, determine meet the cement of hard brittle shale stratum characteristic, bentonite, dispersant compounding Ratio;
Step 6: the compound proportion of cement, bentonite, dispersant determined by according to, prepares hard fragility hydration of clay Shale artificial core.
In step one, for a certain depth segment hard brittle shale stratum, to well drilling detritus or drilling extracting core Carry out test processing, obtain testing required standard specimen.Choose five pieces of standard specimens, test clay respectively Mineral constituent, comprcssive strength, hydration swelling, then calculate comprehensive brittleness index respectively.To test result and Result of calculation is averaged, this meansigma methods can show the clay mineral component on this stratum, hydration swelling, The feature such as intensity, brittleness.
Using the clay mineral component on X-ray diffraction experimental test hard brittle shale stratum, five groups of data take Meansigma methods, result shows that the clay mineral content on this stratum is 23.0%, based on montmorillonite.
Using the tensile strength on rock mechanics experiment test hard brittle shale stratum, five groups of data are averaged, Result shows that the comprcssive strength on this stratum is 40.5MPa, and elastic modulus E is 2.5GPa, and Poisson's ratio v is 0.35.
Using the hydration swelling on linear expansion instrument test hard brittle shale stratum, five groups of data are averaged, Result shows that the hydration swelling on this stratum is 0.5%/h.
The stress-strain diagram obtained during according to test comprcssive strength calculates the most crisp of hard brittle shale stratum Sex index.Computational methods areThis comprehensive brittleness index IBIt is that elastic modulus E is returned with Poisson's ratio v Meansigma methods after one change.Five groups of data are averaged, and result shows that the comprehensive brittleness index on this stratum is 1.425.
In step 2, determine cement type according to the comprcssive strength on hard brittle shale stratum, determined by water The standard testing intensity of mud is not less than the comprcssive strength on tested hard brittle shale stratum.Resisting of this stratum Compressive Strength is 40.5MPa, so selecting 425# Portland cement, its comprcssive strength is 42.5MPa.
Clay mineral component according to hard brittle shale stratum determines bentonite type.This stratum clay mineral The content of middle montmorillonite is higher, so selecting sodium bentonite.
The method determining Dispersant types, comprises the following steps according to sequencing:
(1) being mixed with bentonite by fixed cement, cement and bentonitic weight ratio are 9:1, preparation Three parts of identical mixture;
(2) in three parts of mixture, add the dissimilar dispersant of identical weight respectively, prepare three kinds of Behavior of Hardened Cement Pastes;
(3) content of hydrated calcium silicate in three kinds of Behavior of Hardened Cement Pastes of X-ray diffraction experimental test is used;
(4) according to the content of hydrated calcium silicate, the type of dispersant is determined.
By the content of hydrated calcium silicate (CSH), final aquation in X-ray diffraction experimental test Behavior of Hardened Cement Paste What in product, CSH content was high is citric acid, so selecting citric acid as the dispersant of artificial core.
In step 3, preparing the Behavior of Hardened Cement Paste of 24 kinds of different compound proportions altogether, its compound proportion is as follows:
Comprise only cement, when not containing bentonite, the addition of dispersant is the 0.5% of cement weight, 0.6%, 0.7%, 0.8%, 0.9%, 1.0%, prepare six kinds of Behavior of Hardened Cement Pastes.
When cement and bentonitic weight ratio are 9:1, the addition of dispersant is cement and bentonite weight sum 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1.0%, prepare six kinds of Behavior of Hardened Cement Pastes.
When cement and bentonitic weight ratio are 8:2, the addition of dispersant is cement and bentonite weight sum 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1.0%, prepare six kinds of Behavior of Hardened Cement Pastes.
When cement and bentonitic weight ratio are 7:3, the addition of dispersant is cement and bentonite weight sum 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1.0%, prepare six kinds of Behavior of Hardened Cement Pastes.
In step 4, comprcssive strength, comprehensive brittleness index, hydration swelling compound proportion different from Behavior of Hardened Cement Paste Between the foundation of graph of a relation, comprise the following steps according to sequencing:
(1) Behavior of Hardened Cement Paste comprcssive strength C test obtained and bentonite addition W1With dispersant addition W2 Carry out nonlinear fitting, obtain determining the functional relation C=F (W of Behavior of Hardened Cement Paste comprcssive strength1, W2);
(2) stress-strain diagram obtained time according to test Behavior of Hardened Cement Paste comprcssive strength calculates the comprehensive fragility of Behavior of Hardened Cement Paste and refers to Number, by comprehensive for calculated Behavior of Hardened Cement Paste brittleness index IBWith bentonite addition W1With dispersant addition W2Carry out nonlinear fitting, obtain determining the functional relationship Formulas I of the comprehensive brittleness index of Behavior of Hardened Cement PasteB=F (W1, W2);
(3) Behavior of Hardened Cement Paste hydration swelling E test obtained and bentonite addition W1With dispersant addition W2Carry out nonlinear fitting, obtain determining the functional relation E=F (W of Behavior of Hardened Cement Paste hydration swelling1, W2);
(4) functional relation obtained according to analytical calculation, sets up comprcssive strength, comprehensive brittleness index, water respectively Change the graph of a relation between dilatancy compound proportion different from Behavior of Hardened Cement Paste.
In step 5, determine and meet the cement of hard brittle shale stratum characteristic, bentonite, the answering of dispersant The method of proportioning example, comprises the following steps according to sequencing:
(1) determine and meet the bentonite addition W that hard brittle shale stratum aquation dilatancy requires1
As in figure 2 it is shown, according to the hard brittle shale stratum aquation dilatancy tested and the aquation set up Graph of a relation between dilatancy compound proportion different from Behavior of Hardened Cement Paste, determines bentonite addition W1It is 20.0%.
(2) determine and meet the dispersant addition W that hard brittle shale stratum comprcssive strength requires2a
As it is shown on figure 3, according to the hard brittle shale stratum comprcssive strength tested and the pressure resistance set up Spend the graph of a relation between compound proportions different from Behavior of Hardened Cement Paste, determine bentonite addition W1Under conditions of, really Determine dispersant addition W2aIt is 0.80%.
(3) determine and meet the dispersant addition W that hard brittle shale stratum comprehensive brittleness index requires2b
As shown in Figure 4, according to the comprehensive brittleness index in hard brittle shale stratum tested and set up combine Close the graph of a relation between brittleness index compound proportion different from Behavior of Hardened Cement Paste, determine bentonite addition W1Bar Under part, determine dispersant addition W2bIt is 0.82%.
(4) determine and meet the dispersion that hard brittle shale stratum comprcssive strength requires and comprehensive brittleness index requires simultaneously Agent addition W2.Dispersant addition W2=(W2a+W2b)/2, i.e. W2It is 0.81%.
In step 6, the preparation of hard fragility hydration of clay shale artificial core, include following step according to sequencing Rapid:
(1) cement having determined that compound proportion is mixed with bentonite, stir;
(2) it is added to have determined that the dispersant of compound proportion, then adds water, mix, stir, Form mixture;
(3) mixture is watered build up Behavior of Hardened Cement Paste sample, after Behavior of Hardened Cement Paste sample drying molding, i.e. can get hard fragility Hydration of clay shale artificial core.After Behavior of Hardened Cement Paste sample drying molding, need maintenance 28 days.
In the present embodiment, the size of Behavior of Hardened Cement Paste sample is 100mm × 100mm × 100mm, at Behavior of Hardened Cement Paste sample On drill through a diameter of 25mm, height is the standard cylindrical artificial core of 50mm.
The method utilizing the present embodiment prepares hard fragility hydration of clay shale artificial core, and it is carried out rock mechanics Test and hydration swelling are tested, and the material properties of rock of test result with formation at target locations mud shale are compared Relatively analyzing, to evaluate the artificial core quality of the present embodiment, concrete evaluation result is shown in Table 1.1, actual formation with The mechanical property of artificial core contrasts as shown in Figure 5.
Table 1.1 actual formation and the Evaluating Mechanical Properties result of artificial core
Hydration swelling (%/h) Comprcssive strength (MPa) Comprehensive brittleness index
Actual formation 0.50 40.5 1.425
Artificial core 0.51 39.8 1.416
Relative error 2.0% 1.73% 0.63%
Embodiment two:
A kind of preparation method of hard fragility hydration of clay shale artificial core, its preparation process, principle, useful effect Fruits etc. are identical with embodiment one, except for the difference that:
In step one, make ten pieces of standard specimens, test clay mineral component, comprcssive strength, aquation respectively Dilatancy, then calculate comprehensive brittleness index respectively.Averaging test result and result of calculation, this is average Value can show the features such as the clay mineral component on this stratum, hydration swelling, intensity, brittleness.
Using the clay mineral component on X-ray diffraction experimental test hard brittle shale stratum, ten groups of data take Meansigma methods, result shows that the clay mineral content on this stratum is 25.0%, based on illite.
Using the tensile strength on rock mechanics experiment test hard brittle shale stratum, ten groups of data are averaged, Result shows that the comprcssive strength on this stratum is 53.5MPa, and elastic modulus E is 2.6GPa, and Poisson's ratio v is 0.38.
Using the hydration swelling on linear expansion instrument test hard brittle shale stratum, ten groups of data are averaged, Result shows that the hydration swelling on this stratum is 0.4%/h.
The stress-strain diagram obtained during according to test comprcssive strength calculates the most crisp of hard brittle shale stratum Sex index.Ten groups of data are averaged, and result shows that the comprehensive brittleness index on this stratum is 1.49.
In step 2, selecting 625# Portland cement, its comprcssive strength is 62.5MPa.This stratum is glued In soil mineral, illitic content is higher, so selecting calcium-base bentonite.By X-ray diffraction experimental test The content of hydrated calcium silicate (CSH) in Behavior of Hardened Cement Paste, what in final hydrated product, CSH content was high is lignin Sodium sulfonate, so selecting sodium lignin sulfonate as the dispersant of artificial core.
In step 3, preparing the Behavior of Hardened Cement Paste of 24 kinds of different compound proportions altogether, its compound proportion is as follows:
Comprise only cement, when not containing bentonite, the addition of dispersant is the 0.5% of cement weight, 0.6%, 0.7%, 0.8%, 0.9%, 1.0%, prepare six kinds of Behavior of Hardened Cement Pastes.
When cement and bentonitic weight ratio are 9:1, the addition of dispersant is cement and bentonite weight sum 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1.0%, prepare six kinds of Behavior of Hardened Cement Pastes.
When cement and bentonitic weight ratio are 8:2, the addition of dispersant is cement and bentonite weight sum 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1.0%, prepare six kinds of Behavior of Hardened Cement Pastes.
When cement and bentonitic weight ratio are 7:3, the addition of dispersant is cement and bentonite weight sum 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1.0%, prepare six kinds of Behavior of Hardened Cement Pastes.
In step 4, comprcssive strength, comprehensive brittleness index, hydration swelling compound proportion different from Behavior of Hardened Cement Paste Between the foundation of graph of a relation, comprise the following steps according to sequencing:
(1) Behavior of Hardened Cement Paste comprcssive strength C test obtained and bentonite addition W1With dispersant addition W2 Carry out nonlinear fitting, obtain determining the functional relation C=F (W of Behavior of Hardened Cement Paste comprcssive strength1, W2);
(2) stress-strain diagram obtained time according to test Behavior of Hardened Cement Paste comprcssive strength calculates the comprehensive fragility of Behavior of Hardened Cement Paste and refers to Number, by comprehensive for calculated Behavior of Hardened Cement Paste brittleness index IBWith bentonite addition W1With dispersant addition W2Carry out nonlinear fitting, obtain determining the functional relationship Formulas I of the comprehensive brittleness index of Behavior of Hardened Cement PasteB=F (W1, W2);
(3) Behavior of Hardened Cement Paste hydration swelling E test obtained and bentonite addition W1With dispersant addition W2Carry out nonlinear fitting, obtain determining the functional relation E=F (W of Behavior of Hardened Cement Paste hydration swelling1, W2);
(4) functional relation obtained according to analytical calculation, sets up comprcssive strength, comprehensive brittleness index, water respectively Change the graph of a relation between dilatancy compound proportion different from Behavior of Hardened Cement Paste.
In step 5, determine and meet the cement of hard brittle shale stratum characteristic, bentonite, the answering of dispersant The method of proportioning example, comprises the following steps according to sequencing:
(1) according to the hard brittle shale stratum aquation dilatancy tested and the hydration swelling set up and cement Graph of a relation between stone difference compound proportion, determines bentonite addition W1It is 22.0%, as shown in Figure 6.
(2) comprcssive strength according to the hard brittle shale stratum comprcssive strength tested and set up and Behavior of Hardened Cement Paste are not With the graph of a relation between compound proportion, determining bentonite addition W1Under conditions of, determine that dispersant adds Amount W2aIt is 0.70%, as shown in Figure 7.
(3) the comprehensive brittleness index according to the comprehensive brittleness index in hard brittle shale stratum tested and set up and Graph of a relation between Behavior of Hardened Cement Paste difference compound proportion, is determining bentonite addition W1Under conditions of, determine point Powder addition W2bIt is 0.74%, as shown in Figure 8.
(4) determine and meet the dispersion that hard brittle shale stratum comprcssive strength requires and comprehensive brittleness index requires simultaneously Agent addition W2It is 0.72%.
In step 6, the preparation of hard fragility hydration of clay shale artificial core, include following step according to sequencing Rapid:
(1) cement having determined that compound proportion is mixed with bentonite, stir;
(2) it is added to have determined that the dispersant of compound proportion, then adds water, mix, stir, Form mixture;
(3) mixture is watered build up Behavior of Hardened Cement Paste sample, after Behavior of Hardened Cement Paste sample drying molding, i.e. can get hard fragility Hydration of clay shale artificial core.After Behavior of Hardened Cement Paste sample drying molding, need maintenance 28 days.
In the present embodiment, the size of Behavior of Hardened Cement Paste sample is 100mm × 100mm × 100mm, at Behavior of Hardened Cement Paste sample On drill through a diameter of 38mm, height is the standard cylindrical artificial core of 50mm.
The method utilizing the present embodiment prepares hard fragility hydration of clay shale artificial core, and it is carried out rock mechanics Test and hydration swelling are tested, and the material properties of rock of test result with formation at target locations mud shale are compared Relatively analyze, to evaluate the artificial core quality of the present embodiment, as shown in Figure 9.Concrete evaluation result is shown in Table 2.1.
Table 2.1 actual formation and the Evaluating Mechanical Properties result of artificial core
Hydration swelling (%/h) Comprcssive strength (MPa) Comprehensive brittleness index
Actual formation 0.40 53.5 1.49
Artificial core 0.405 52.4 1.476
Relative error 1.25% 2.06% 0.94%
Embodiment three:
A kind of preparation method of hard fragility hydration of clay shale artificial core, its preparation process, principle, useful effect Fruits etc. are identical with embodiment one, except for the difference that:
In step one, make 15 pieces of standard specimens, test clay mineral component, comprcssive strength, water respectively Change dilatancy, then calculate comprehensive brittleness index respectively.Averaging test result and result of calculation, this is put down Average can show the features such as the clay mineral component on this stratum, hydration swelling, intensity, brittleness.
Use the clay mineral component on X-ray diffraction experimental test hard brittle shale stratum, 15 groups of data Averaging, result shows that the clay mineral content on this stratum is 23.0%, based on montmorillonite.
Using the tensile strength on rock mechanics experiment test hard brittle shale stratum, 15 groups of data are averaged Value, result shows that the comprcssive strength on this stratum is 40.5MPa, and elastic modulus E is 2.4GPa, Poisson's ratio v It is 0.40.
Using the hydration swelling on linear expansion instrument test hard brittle shale stratum, 15 groups of data are averaged Value, result shows that the hydration swelling on this stratum is 0.45%/h.
The stress-strain diagram obtained during according to test comprcssive strength calculates the most crisp of hard brittle shale stratum Sex index.15 groups of data are averaged, and result shows that the comprehensive brittleness index on this stratum is 1.40.
In step 2, selecting lumnite cement, its comprcssive strength is 52.5MPa.This stratum clay mineral The content of middle montmorillonite is higher, so selecting sodium bentonite.By X-ray diffraction experimental test Behavior of Hardened Cement Paste The content of middle hydrated calcium silicate (CSH), what in final hydrated product, CSH content was high is sulfonated phenylethylene- Copolymer-maleic anhydride, so selecting Sulfonated Copolymer of Styrene and Maleic Anhydride as the dispersant of artificial core.
In step 3, preparing the Behavior of Hardened Cement Paste of 24 kinds of different compound proportions altogether, its compound proportion is as follows:
Comprise only cement, when not containing bentonite, the addition of dispersant is the 0.5% of cement weight, 0.6%, 0.7%, 0.8%, 0.9%, 1.0%, prepare six kinds of Behavior of Hardened Cement Pastes.
When cement and bentonitic weight ratio are 9:1, the addition of dispersant is cement and bentonite weight sum 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1.0%, prepare six kinds of Behavior of Hardened Cement Pastes.
When cement and bentonitic weight ratio are 8:2, the addition of dispersant is cement and bentonite weight sum 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1.0%, prepare six kinds of Behavior of Hardened Cement Pastes.
When cement and bentonitic weight ratio are 7:3, the addition of dispersant is cement and bentonite weight sum 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1.0%, prepare six kinds of Behavior of Hardened Cement Pastes.
In step 4, comprcssive strength, comprehensive brittleness index, hydration swelling compound proportion different from Behavior of Hardened Cement Paste Between the foundation of graph of a relation, comprise the following steps according to sequencing:
(1) Behavior of Hardened Cement Paste comprcssive strength C test obtained and bentonite addition W1With dispersant addition W2 Carry out nonlinear fitting, obtain determining the functional relation C=F (W of Behavior of Hardened Cement Paste comprcssive strength1, W2);
(2) stress-strain diagram obtained time according to test Behavior of Hardened Cement Paste comprcssive strength calculates the comprehensive fragility of Behavior of Hardened Cement Paste and refers to Number, by comprehensive for calculated Behavior of Hardened Cement Paste brittleness index IBWith bentonite addition W1With dispersant addition W2Carry out nonlinear fitting, obtain determining the functional relationship Formulas I of the comprehensive brittleness index of Behavior of Hardened Cement PasteB=F (W1, W2);
(3) Behavior of Hardened Cement Paste hydration swelling E test obtained and bentonite addition W1With dispersant addition W2Carry out nonlinear fitting, obtain determining the functional relation E=F (W of Behavior of Hardened Cement Paste hydration swelling1, W2);
(4) functional relation obtained according to analytical calculation, sets up comprcssive strength, comprehensive brittleness index, water respectively Change the graph of a relation between dilatancy compound proportion different from Behavior of Hardened Cement Paste.
In step 5, determine and meet the cement of hard brittle shale stratum characteristic, bentonite, the answering of dispersant The method of proportioning example, comprises the following steps according to sequencing:
(1) according to the hard brittle shale stratum aquation dilatancy tested and the hydration swelling set up and cement Graph of a relation between stone difference compound proportion, determines bentonite addition W1It is 24.0%.
(2) comprcssive strength according to the hard brittle shale stratum comprcssive strength tested and set up and Behavior of Hardened Cement Paste are not With the graph of a relation between compound proportion, determining bentonite addition W1Under conditions of, determine that dispersant adds Amount W2aIt is 0.82%.
(3) the comprehensive brittleness index according to the comprehensive brittleness index in hard brittle shale stratum tested and set up and Graph of a relation between Behavior of Hardened Cement Paste difference compound proportion, is determining bentonite addition W1Under conditions of, determine point Powder addition W2bIt is 0.88%.
(4) determine and meet the dispersion that hard brittle shale stratum comprcssive strength requires and comprehensive brittleness index requires simultaneously Agent addition W2It is 0.85%.
In step 6, the preparation of hard fragility hydration of clay shale artificial core, include following step according to sequencing Rapid:
(1) cement having determined that compound proportion is mixed with bentonite, stir;
(2) it is added to have determined that the dispersant of compound proportion, then adds water, mix, stir, Form mixture;
(3) mixture is watered build up Behavior of Hardened Cement Paste sample, after Behavior of Hardened Cement Paste sample drying molding, i.e. can get hard fragility Hydration of clay shale artificial core.After Behavior of Hardened Cement Paste sample drying molding, need maintenance 28 days.
In the present embodiment, the size of Behavior of Hardened Cement Paste sample is 100mm × 100mm × 100mm, at Behavior of Hardened Cement Paste sample On drill through a diameter of 40mm, height is the standard cylindrical artificial core of 50mm.
The method utilizing the present embodiment prepares hard fragility hydration of clay shale artificial core, and it is carried out rock mechanics Test and hydration swelling are tested, and the material properties of rock of test result with formation at target locations mud shale are compared Relatively analyzing, to evaluate the artificial core quality of the present embodiment, concrete evaluation result is shown in Table 3.1.
Table 3.1 actual formation and the Evaluating Mechanical Properties result of artificial core
Hydration swelling (%/h) Comprcssive strength (MPa) Comprehensive brittleness index
Actual formation 0.45 40.5 1.40
Artificial core 0.44 40.1 1.387
Relative error 2.22% 0.99% 0.93%
It will be apparent to those skilled in the art that the preparation side of the hard fragility hydration of clay shale artificial core of the present invention It is each that method includes shown by the summary of the invention of the invention described above description and detailed description of the invention part and accompanying drawing The combination in any of part, does not has each scheme these combinations constituted as space is limited and for making description simple and clear Describe one by one.All within the spirit and principles in the present invention, any modification, equivalent substitution and improvement done Deng, should be included within the scope of the present invention.

Claims (21)

1. a preparation method for hard fragility hydration of clay shale artificial core, it includes following step according to sequencing Rapid:
Step one: the test clay mineral component on hard brittle shale stratum, comprcssive strength, hydration swelling, meter Calculate the comprehensive brittleness index on hard brittle shale stratum;
Step 2: determine the type of cement, bentonite, dispersant;
Step 3: the type of cement, bentonite, dispersant determined by according to, prepares the swelling of Different adding amount Soil and the Behavior of Hardened Cement Paste of dispersant, and test the comprcssive strength of Behavior of Hardened Cement Paste, comprehensive fragility under different compound proportion and refer to Number, hydration swelling;
Step 4: comprcssive strength, the comprehensive fragility of Behavior of Hardened Cement Paste are referred to by bentonite and the dispersant of analyzing Different adding amount Number, the impact of hydration swelling, set up comprcssive strength, comprehensive brittleness index, hydration swelling and water respectively Graph of a relation between mudstone difference compound proportion;
Step 5: according to comprcssive strength, comprehensive brittleness index, hydration swelling compound proportion different from Behavior of Hardened Cement Paste it Between graph of a relation, determine meet the cement of hard brittle shale stratum characteristic, bentonite, dispersant compounding Ratio;
Step 6: the compound proportion of cement, bentonite, dispersant determined by according to, prepares hard fragility hydration of clay Shale artificial core;
In step 2, determine cement type according to the comprcssive strength on hard brittle shale stratum, determined by water The standard testing intensity of mud is not less than the comprcssive strength on tested hard brittle shale stratum;According to hard fragility The clay mineral component of mud shale stratum determines bentonite type, if the clay mineral on hard brittle shale stratum Middle smectite content is higher, then select sodium bentonite, if in the clay mineral on hard brittle shale stratum she Profit stone content is higher, then select calcium-base bentonite;Content according to hydrated calcium silicate determines the type of dispersant, By the content of hydrated calcium silicate in X-ray diffraction experimental test Behavior of Hardened Cement Paste, select hydrated calcium silicate content high Dispersant.
2. the preparation method of hard fragility hydration of clay shale artificial core as claimed in claim 1, it is characterised in that: In described step one, at least choose five pieces of hard brittle shale formation sample, test respectively clay mineral component, Comprcssive strength, hydration swelling, calculate comprehensive brittleness index respectively, makes even test result and result of calculation Average.
3. the preparation method of hard fragility hydration of clay shale artificial core as claimed in claim 2, it is characterised in that: Use the clay mineral component on X-ray diffraction experimental test hard brittle shale stratum.
4. the preparation method of hard fragility hydration of clay shale artificial core as claimed in claim 2, it is characterised in that: Use the tensile strength on rock mechanics experiment test hard brittle shale stratum.
5. the preparation method of hard fragility hydration of clay shale artificial core as claimed in claim 2, it is characterised in that: Use the hydration swelling on linear expansion instrument test hard brittle shale stratum.
6. the preparation method of hard fragility hydration of clay shale artificial core as claimed in claim 2, it is characterised in that: The stress-strain diagram obtained during according to test comprcssive strength calculates the comprehensive fragility on hard brittle shale stratum and refers to Number.
7. the preparation method of hard fragility hydration of clay shale artificial core as claimed in claim 1, it is characterised in that: Determined by cement be any one in Portland cement, composite Portland cement, special cement.
8. the preparation method of hard fragility hydration of clay shale artificial core as claimed in claim 7, it is characterised in that: Described special cement is any one in lumnite cement, oil-well cement, sulfate resisting Portland cement.
9. the preparation method of hard fragility hydration of clay shale artificial core as claimed in claim 1, it is characterised in that: In described step 2, the method determining Dispersant types, comprise the following steps according to sequencing:
Step one: mixed with bentonite by fixed cement, cement and bentonitic weight ratio are 9:1, join Make three parts of identical mixture;
Step 2: add the dissimilar dispersant of identical weight respectively in three parts of mixture, prepares three kinds of cement Stone;
Step 3: use the content of hydrated calcium silicate in three kinds of Behavior of Hardened Cement Pastes of X-ray diffraction experimental test;
Step 4: according to the content of hydrated calcium silicate, determine the type of dispersant.
10. the preparation method of the hard fragility hydration of clay shale artificial core stated such as claim 9, it is characterised in that: Determined by dispersant be in sodium lignin sulfonate, citric acid, Sulfonated Copolymer of Styrene and Maleic Anhydride appoint A kind of.
The preparation method of 11. hard fragility hydration of clay shale artificial cores as claimed in claim 1, it is characterised in that: In described step 3, comprising only cement, when not containing bentonite, the addition of dispersant is cement weight 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1.0%, prepare six kinds of Behavior of Hardened Cement Pastes.
The preparation method of 12. hard fragility hydration of clay shale artificial cores as claimed in claim 11, it is characterised in that: In described step 3, when cement and bentonitic weight ratio are 9:1, the addition of dispersant is cement and swelling Soil the 0.5% of weight sum, 0.6%, 0.7%, 0.8%, 0.9%, 1.0%, prepares six kinds of Behavior of Hardened Cement Pastes.
The preparation method of 13. hard fragility hydration of clay shale artificial cores as claimed in claim 12, it is characterised in that: In described step 3, when cement and bentonitic weight ratio are 8:2, the addition of dispersant is cement and swelling Soil the 0.5% of weight sum, 0.6%, 0.7%, 0.8%, 0.9%, 1.0%, prepares six kinds of Behavior of Hardened Cement Pastes.
The preparation method of 14. hard fragility hydration of clay shale artificial cores as claimed in claim 13, it is characterised in that: In described step 3, when cement and bentonitic weight ratio are 7:3, the addition of dispersant is cement and swelling Soil the 0.5% of weight sum, 0.6%, 0.7%, 0.8%, 0.9%, 1.0%, prepares six kinds of Behavior of Hardened Cement Pastes.
The preparation method of 15. hard fragility hydration of clay shale artificial cores as claimed in claim 1, it is characterised in that: In described step 4, comprcssive strength, comprehensive brittleness index, hydration swelling compound proportion different from Behavior of Hardened Cement Paste Between the foundation of graph of a relation, comprise the following steps according to sequencing:
Step one: Behavior of Hardened Cement Paste comprcssive strength C that test is obtained and bentonite addition W1With dispersant addition W2Carry out nonlinear fitting, obtain determining the functional relation C=F (W of Behavior of Hardened Cement Paste comprcssive strength1, W2);
Step 2: the stress-strain diagram obtained during according to test Behavior of Hardened Cement Paste comprcssive strength calculates the most crisp of Behavior of Hardened Cement Paste Sex index, by comprehensive for calculated Behavior of Hardened Cement Paste brittleness index IBWith bentonite addition W1Add with dispersant Amount W2Carry out nonlinear fitting, obtain determining the functional relationship Formulas I of the comprehensive brittleness index of Behavior of Hardened Cement PasteB=F (W1, W2);
Step 3: the Behavior of Hardened Cement Paste hydration swelling E that test is obtained and bentonite addition W1With dispersant addition W2Carry out nonlinear fitting, obtain determining the functional relation E=F (W of Behavior of Hardened Cement Paste hydration swelling1, W2);
Step 4: the functional relation obtained according to analytical calculation, set up respectively comprcssive strength, comprehensive brittleness index, Graph of a relation between hydration swelling compound proportion different from Behavior of Hardened Cement Paste.
The preparation method of 16. hard fragility hydration of clay shale artificial cores as claimed in claim 1, it is characterised in that: In described step 5, determine and meet the cement of hard brittle shale stratum characteristic, bentonite, the answering of dispersant The method of proportioning example, comprises the following steps according to sequencing:
Step one: determine and meet the bentonite addition W that hard brittle shale stratum aquation dilatancy requires1
Step 2: determine and meet the dispersant addition W that hard brittle shale stratum comprcssive strength requires2a
Step 3: determine and meet the dispersant addition W that the comprehensive brittleness index in hard brittle shale stratum requires2b
Step 4: determine that meet hard brittle shale stratum comprcssive strength requires and the requirement of comprehensive brittleness index simultaneously Dispersant addition W2
The preparation method of 17. hard fragility hydration of clay shale artificial cores as claimed in claim 16, it is characterised in that: In described step one, hard brittle shale stratum aquation dilatancy and the aquation set up according to having tested are swollen Graph of a relation between swollen property compound proportion different from Behavior of Hardened Cement Paste, determines bentonite addition W1
The preparation method of 18. hard fragility hydration of clay shale artificial cores as claimed in claim 16, it is characterised in that: In described step 2, according to the hard brittle shale stratum comprcssive strength tested and the comprcssive strength set up Graph of a relation between compound proportions different from Behavior of Hardened Cement Paste, is determining bentonite addition W1Under conditions of, determine Dispersant addition W2a
The preparation method of 19. hard fragility hydration of clay shale artificial cores as claimed in claim 16, it is characterised in that: In described step 3, according to the comprehensive brittleness index in hard brittle shale stratum tested and set up comprehensive Graph of a relation between brittleness index compound proportion different from Behavior of Hardened Cement Paste, is determining bentonite addition W1Condition Under, determine dispersant addition W2b
The preparation method of 20. hard fragility hydration of clay shale artificial cores as claimed in claim 16, it is characterised in that: In described step 4, dispersant addition W2=(W2a+W2b)/2。
The preparation method of 21. hard fragility hydration of clay shale artificial cores as claimed in claim 1, it is characterised in that: In described step 6, the preparation of hard fragility hydration of clay shale artificial core, include following step according to sequencing Rapid:
Step one: the cement having determined that compound proportion is mixed with bentonite;
Step 2: be added to have determined that the dispersant of compound proportion, then add water, mix, is formed Mixture;
Step 3: watered by mixture and build up Behavior of Hardened Cement Paste, after Behavior of Hardened Cement Paste drying and moulding, i.e. can get hard fragility aquation Mud shale artificial core.
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