CN111610081A - Artificial rock core and manufacturing method thereof - Google Patents
Artificial rock core and manufacturing method thereof Download PDFInfo
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- CN111610081A CN111610081A CN202010390759.0A CN202010390759A CN111610081A CN 111610081 A CN111610081 A CN 111610081A CN 202010390759 A CN202010390759 A CN 202010390759A CN 111610081 A CN111610081 A CN 111610081A
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- glass beads
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- lipophilic
- artificial core
- hydrophilic
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- 238000004519 manufacturing process Methods 0.000 title abstract description 6
- 239000011435 rock Substances 0.000 title description 10
- 239000011521 glass Substances 0.000 claims abstract description 69
- 239000011324 bead Substances 0.000 claims abstract description 67
- 238000000034 method Methods 0.000 claims abstract description 29
- 238000002844 melting Methods 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 230000008018 melting Effects 0.000 claims abstract description 10
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 9
- 238000003825 pressing Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 239000002253 acid Substances 0.000 claims abstract description 5
- 239000007864 aqueous solution Substances 0.000 claims abstract description 5
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910001220 stainless steel Inorganic materials 0.000 claims description 16
- 239000010935 stainless steel Substances 0.000 claims description 16
- 238000009826 distribution Methods 0.000 claims description 9
- 239000004568 cement Substances 0.000 claims 1
- 230000035699 permeability Effects 0.000 abstract description 7
- 238000011049 filling Methods 0.000 abstract description 5
- 238000009736 wetting Methods 0.000 description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 238000001723 curing Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 229910052582 BN Inorganic materials 0.000 description 2
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000004005 microsphere Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000005755 formation reaction Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000013007 heat curing Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/36—Embedding or analogous mounting of samples
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N15/082—Investigating permeability by forcing a fluid through a sample
- G01N15/0826—Investigating permeability by forcing a fluid through a sample and measuring fluid flow rate, i.e. permeation rate or pressure change
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N15/088—Investigating volume, surface area, size or distribution of pores; Porosimetry
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/36—Embedding or analogous mounting of samples
- G01N2001/366—Moulds; Demoulding
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- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Dispersion Chemistry (AREA)
- Fluid Mechanics (AREA)
- Glass Compositions (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention provides a method for manufacturing an artificial core, which comprises the following steps: treating the low-melting-point glass beads with the melting point of 300-400 ℃ with strong acid or strong base to provide hydrophilic glass beads; treating the glass beads with a dichlorodimethylsilane aqueous solution and heating and curing at 250-300 ℃ to provide lipophilic glass beads; mixing the hydrophilic glass beads with the lipophilic glass beads to obtain heterogeneously mixed glass beads; filling the heterogeneously mixed glass beads into a mold with the inner surface coated with a high-temperature-resistant release agent, and heating at the temperature of 300-400 ℃ until the glass beads are softened; pressing the softened glass beads using a mold to deform them to arrange and densify to obtain a stack; the stack is removed from the mold to obtain an artificial core. The prepared artificial core has heterogeneous wettability, porosity and permeability which are closer to those of a natural core.
Description
Technical Field
The invention belongs to the field of oil-gas exploration, development and displacement tests, and particularly relates to an artificial rock core and a manufacturing method thereof.
Background
Wettability is an important parameter in oil and gas exploration and development, and has important influence on oil and gas recovery rate and migration and injection and formation. At present, the method for evaluating the rock wettability in the petroleum industry mainly adopts an Amott and USBM wetting index method, the two methods are complex in testing process and long in time consumption, more importantly, oil washing treatment needs to be carried out on a rock core before testing, the original wettability of the rock is changed, and in the measuring process, oil phase seepage can dissolve and migrate colloid asphaltene, so that the wettability of the rock is changed. Therefore, the development of the artificial rock core with a known wetting state becomes an important way for researching the influence of wetting on seepage. The method for manufacturing the artificial core is generally a pressing method, and the artificial core can be manufactured by mixing a granular material and a cementing agent according to a certain proportion, compacting under high pressure and then solidifying the cementing agent. The common binder is an organic material such as epoxy, so the wettability of the artificial core made by conventional pressing methods exhibits a weakly oleophilic or neutral wetting. The wettability of the artificial core manufactured by the conventional method or the artificial core manufactured according to the requirements of oleophilicity and hydrophilicity is uniform. In addition, the artificial core prepared by the pressing method has no deformation of particles, and the porosity and permeability are obviously higher than those of the natural core.
Disclosure of Invention
An object of the present application is to provide a method of fabricating an artificial core having heterogeneous wettability, porosity and permeability closer to those of natural cores, and an artificial core fabricated by the method.
In order to achieve the purpose, the invention provides the following technical scheme:
(1) a method for making an artificial core, the method comprising the steps of:
treating the low-melting-point glass beads with the melting point of 300-400 ℃ with strong acid or strong base to provide hydrophilic glass beads;
treating the glass beads with a dichlorodimethylsilane aqueous solution and heating and curing at 250-300 ℃ to provide lipophilic glass beads;
randomly mixing the hydrophilic glass beads and the lipophilic glass beads or arranging the hydrophilic glass beads and the lipophilic glass beads according to a preset distribution state to obtain glass beads in heterogeneous distribution;
the glass beads in heterogeneous distribution are filled into a mold with the inner surface coated with a high-temperature resistant release agent and heated at the temperature of 300-400 ℃ until the glass beads are softened;
pressing the softened glass beads using a mold to deform them to arrange and densify to obtain a stack;
the stack is removed from the mold to obtain an artificial core.
(2) The method according to (1), wherein the mold comprises a cylinder and a cylinder which can move up and down in the cylinder, and the outer diameter of the cylinder is equal to or slightly smaller than the inner diameter of the cylinder.
(3) The method according to (2), wherein the cylinder and the column are made of high-temperature-resistant stainless steel.
(4) The method according to (1), wherein the low-melting glass beads are lead-containing glass beads.
(5) The method of any one of (1) to (4), wherein the method does not use a consolidating agent.
(6) An artificial core produced using the method according to any one of (1) to (5).
Advantageous effects
According to the invention, the hydrophilic and lipophilic glass beads with low melting points, which are prepared in advance, are randomly mixed or distributed in a preset distribution state, and then the glass beads are softened, melted on the surface and pressed to be consolidated together by heating under the condition of not using a cementing agent, so that the heterogeneous wetting artificial core with the wettability, the porosity and the permeability closer to those of a natural core can be obtained. In addition, two heterogeneous wet artificial cores of spot wetting and mixed wetting can be prepared by changing the stacking mode of the oil-wet and water-wet low-melting-point glass beads, and the heterogeneous wet artificial cores with different porosity and permeability levels can be obtained by adjusting the axial pressure applied to a softened glass bead stacking body.
Drawings
Fig. 1 is a schematic view of an apparatus used in the method according to the present invention.
Detailed Description
The method according to the invention comprises the following steps: treating the low-melting-point glass beads with the melting point of 300-400 ℃ with strong acid or strong base to provide hydrophilic glass beads; treating the glass beads with a dichlorodimethylsilane aqueous solution and heating and curing at 250-300 ℃ to provide lipophilic glass beads; randomly mixing the hydrophilic glass beads and the lipophilic glass beads or arranging the hydrophilic glass beads and the lipophilic glass beads according to a preset distribution state to obtain glass beads in heterogeneous distribution; filling the heterogeneously mixed glass beads into a mold with the inner surface coated with a high-temperature-resistant release agent, and heating at the temperature of 300-400 ℃ until the glass beads are softened; pressing the softened glass beads using a mold to deform them to arrange and densify to obtain a stack; the stack is removed from the mold to obtain an artificial core.
According to the method of the present invention, examples of the strong acid include hydrochloric acid, sulfuric acid and the like, and examples of the strong base include sodium hydroxide, potassium hydroxide and the like. The low-melting glass beads have a melting point of 300-400 deg.C, for example 350 deg.C, and examples include lead-containing glass beads. The heat curing and heat softening may be performed in a muffle furnace. The time for heating and curing can be 24-48 hours.
The die used in the method comprises a cylinder body and a cylinder body which can move up and down in the cylinder body, wherein the outer diameter of the cylinder body is equal to or slightly smaller than the inner diameter of the cylinder body. The cylinder and the column body can be made of high-temperature-resistant stainless steel, such as 301S high-temperature-resistant stainless steel.
Fig. 1 is a schematic view of an apparatus used in the method according to the present invention. As shown in fig. 1, the mixed or prearranged low melting glass microspheres 2 are placed in a mold comprising a stainless steel cylinder 1 and a stainless steel cylinder 3, and the mold is placed in a muffle furnace 4 for heating. The inner diameter of the stainless steel column can be 2.54cm, the wall thickness is 0.3cm, and the depth of the column is 25 cm; the stainless steel column was 2.536cm in diameter and 23cm in length. By adopting the device, the artificial mixed wetting rock core with the length of 2-22 cm can be manufactured.
According to the present invention, examples of the high-temperature resistant release agent include boron nitride. The above-described method according to the invention makes it possible to obtain a heterogeneous wetted artificial core. For example, the artificial core may be spotted or mixed wetted.
Hereinafter, the present invention will be specifically described by some examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the present invention in any way.
Example 1
And (3) respectively cleaning 60-mesh lead-containing glass beads (with the melting point of 350 ℃) by using 5% hydrochloric acid and sodium hydroxide to remove surface impurities, rinsing by using clear water and airing to obtain the water-wet low-melting-point wet glass beads. Soaking part of the low-melting-point glass beads in 0.1% dichlorodimethylsilane aqueous solution, filtering to dry, heating at 280 ℃ for 48 hours in a muffle furnace, and cooling to room temperature to prepare the oil-wet low-melting-point glass beads. And (3) coating boron nitride on the inner surface of the stainless steel barrel. Oil-and water-wetted low melting glass microspheres were mixed according to 2: 3, and mixing the mixture sufficiently. Selecting a mixture of proper amount of oil-wetted and water-wetted low-melting-point glass beads, filling the mixture into a stainless steel column (301S high-temperature stainless steel) with a filling height of 8cm, leveling the upper surfaces of the glass beads, and filling the glass beads into a stainless steel column (301S high-temperature stainless steel) on the upper surfaces. The stainless steel cylinder filled with the glass beads is placed in a muffle furnace and is kept at the constant temperature of 370 ℃ for three hours. And taking out the stainless steel cylinder filled with the glass beads, and axially pressing (the size is 100N) through the stainless steel cylinder to ensure that the softened glass beads are extruded and deformed to be arranged and densified. And after cooling, taking out the high-temperature consolidated glass bead columnar accumulation body to obtain the artificial mixed wetting rock core with the oil wetting and the water wetting being 2: 3.
The porosity of the resulting mixed wet core was measured by gas measurement to be 12.8%, the permeability was 9.74mD, which is close to the average porosity of 12% and the average permeability of 8.05mD for natural cores (10 samples).
The above-described embodiments are merely illustrative of the present invention and are not intended to limit the present invention. It will be appreciated by those skilled in the art that modifications and variations to the embodiments of the present invention are within the scope of the present invention without departing from the spirit and scope of the invention. And the scope of the invention should be determined from the appended claims.
Claims (6)
1. A method for making an artificial core, the method comprising the steps of:
treating the low-melting-point glass beads with the melting point of 300-400 ℃ with strong acid or strong base to provide hydrophilic glass beads;
treating the glass beads with a dichlorodimethylsilane aqueous solution and heating and curing at 250-300 ℃ to provide lipophilic glass beads;
randomly mixing the hydrophilic glass beads and the lipophilic glass beads or arranging the hydrophilic glass beads and the lipophilic glass beads according to a preset distribution state to obtain glass beads in heterogeneous distribution;
the glass beads in heterogeneous distribution are filled into a mold with the inner surface coated with a high-temperature resistant release agent and heated at the temperature of 300-400 ℃ until the glass beads are softened;
pressing the softened glass beads using the mold to deform them to arrange and densify to obtain a stack;
and taking the stack out of the mold to obtain the artificial core.
2. The method of claim 1, wherein the mold comprises a barrel and a cylinder movable up and down within the barrel, the cylinder having an outer diameter equal to or slightly less than an inner diameter of the barrel.
3. The method of claim 2, wherein the cylinder and the column are made of high temperature resistant stainless steel.
4. The method according to claim 1, wherein the low melting point glass beads are lead-containing glass beads.
5. The method of any one of claims 1 to 4, wherein no cement is used.
6. An artificial core made using the method according to any one of claims 1 to 5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010390759.0A CN111610081B (en) | 2020-05-09 | 2020-05-09 | Artificial rock core and manufacturing method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010390759.0A CN111610081B (en) | 2020-05-09 | 2020-05-09 | Artificial rock core and manufacturing method thereof |
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| CN111610081A true CN111610081A (en) | 2020-09-01 |
| CN111610081B CN111610081B (en) | 2021-08-24 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112857935A (en) * | 2021-01-22 | 2021-05-28 | 上海大学 | Preparation method of large-grade-difference heterogeneous nonmagnetic core |
| CN113027431A (en) * | 2021-03-12 | 2021-06-25 | 东北石油大学 | Semi-sealed two-dimensional seepage model and manufacturing method thereof |
| CN114935486A (en) * | 2022-06-06 | 2022-08-23 | 陕西科技大学 | Heterogeneous core material based on corn straw core and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112857935A (en) * | 2021-01-22 | 2021-05-28 | 上海大学 | Preparation method of large-grade-difference heterogeneous nonmagnetic core |
| CN112857935B (en) * | 2021-01-22 | 2022-11-18 | 上海大学 | Preparation method of large-grade-difference heterogeneous nonmagnetic core |
| CN113027431A (en) * | 2021-03-12 | 2021-06-25 | 东北石油大学 | Semi-sealed two-dimensional seepage model and manufacturing method thereof |
| CN113027431B (en) * | 2021-03-12 | 2021-09-07 | 东北石油大学 | Semi-sealed two-dimensional seepage model and manufacturing method thereof |
| CN114935486A (en) * | 2022-06-06 | 2022-08-23 | 陕西科技大学 | Heterogeneous core material based on corn straw core and preparation method thereof |
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| Publication number | Publication date |
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| CN111610081B (en) | 2021-08-24 |
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