CN106596223B - Preparation method of rock core for dense conglomerate oil displacement - Google Patents
Preparation method of rock core for dense conglomerate oil displacement Download PDFInfo
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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
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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
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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
- G01N1/38—Diluting, dispersing or mixing samples
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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
- G01N1/44—Sample treatment involving radiation, e.g. heat
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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
- G01N2001/364—Embedding or analogous mounting of samples using resins, epoxy
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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
- G01N2001/366—Moulds; Demoulding
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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
- G01N1/38—Diluting, dispersing or mixing samples
- G01N2001/386—Other diluting or mixing processes
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Abstract
The invention discloses a preparation method of a rock core for compact conglomerate oil displacement, which comprises the following steps: mixing quartz sand with a certain particle size, clay mineral and cementing agent powder in proportion; assembling a mould; wetting the mold: before filling sand into the mold, spraying 3mg of target formation water into the lower surface to be contacted with the sand body by using a fine water spray head, and homogenizing: weighing 1/N of quartz sand mixture in the volume of the mold, loading the quartz sand mixture into the mold, moving the quartz sand mixture in the mold back and forth along the horizontal direction by using a strickling tool, and finally pressing the quartz sand mixture by using a pressing block; stabilizing the pressure of the filled mold for 15min, and then releasing the pressure; repeating the steps (3) to (5) until the mold is full, and putting the whole core mold into a constant temperature box for baking; and (6) demolding. The invention prepares the compact rock core with large volume, the rock core has the advantage of small dead pore, optimizes the compact sandstone in the laboratory experiment only by coring experiment without the blank of artificial rock core, and provides help for the development of unconventional oil and gas fields.
Description
Technical Field
The invention relates to a preparation method of a rock core for compact conglomerate oil displacement, and belongs to the technical field of artificial rock cores and preparation thereof.
Background
The energy exploration reserves of unconventional oil and gas reservoirs (tight sandstone) are huge, and the development of the unconventional oil and gas reservoirs is also a main research field of the current topic, which receives great attention. Due to the uniqueness of a reservoir layer, the conventional means cannot effectively and efficiently produce and develop, a reasonable development scheme is the basis of oil and gas field development, and necessary/accurate indoor is the basis in the basis, so that the method is of great importance for the core manufacturing of a foundation-simulated oil reservoir of indoor experimental research.
At present, most of research on core making is not enough, but most of the research is based on core making of conventional oil and gas reservoirs, for example, each type of core making is explained in the literature of 'technology and application of quartz sand epoxy resin cemented artificial core for core making' taught by professor Piezo, and the research is mainly based on the conventional reservoir geological conditions of Daqing oil fields.
The compact sandstone manufacturing design only includes Wushu, a temperature and pressure double-control compact artificial sandstone core and a preparation method thereof, the publication number is CN104931312A, and the core is manufactured by adopting high temperature of 300 ℃ and high pressure of 220MPa, so that the required porosity and permeability of the core can be met. The porosity and permeability required by the design are only the first problems in the preparation of the compact core, and the next important problem is the size of the prepared core. If only the size is
And
under the condition of low permeability of a bottom hole, the pore volume is very limited (for example, the pore volume is only a few ml for a core with the length of 10 cm), so that for an oil displacement experiment, the experimental error of the recovery ratio/the water content can directly influence the conclusion; the injection pressure still appears to increase under full water flooding conditions. Three important parameters that mainly characterize the displacement effect/displacement characteristics cannot be represented effectively at all.
Therefore, a more ideal model and a manufacturing method are needed to be designed for the compact sandstone core for oil displacement.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention provides a preparation method of a core for compact conglomerate oil displacement, which is mainly used for manufacturing an artificial core for the purpose of indoor experimental research on the displacement characteristics of a compact conglomerate oil reservoir and can meet the indoor displacement experimental research on the type of the compact sandstone oil reservoir.
The technical scheme adopted by the invention for solving the technical problems is as follows: a preparation method of a core for dense conglomerate oil displacement comprises the following steps:
(1) mixing quartz sand with certain particle size, clay mineral and cementing agent powder in a certain proportion, and uniformly stirring to obtain a quartz sand mixture;
(2) assembling a mold: the die mainly comprises a bottom plate, a side plate and a pressing block, wherein the bottom plate, the side plate and the pressing block are steel plates, the surface roughness Ra of the inner wall is less than or equal to 0.025 mu m, and the geometric size of the square core die is as follows: length × width × height is 305mm × 92mm × 92 mm;
(3) wetting the mold: before filling sand into the mold, spraying 3mg of target formation water to the lower surface of the sand body to be contacted by a fine water spray head, and uniformly covering;
(4) sand homogenizing: weighing quartz sand mixture with the volume of 1/N of that of the mold, filling the quartz sand mixture into the wetted mold, moving the quartz sand mixture back and forth in the mold along the horizontal direction by using a strickling tool until the surface of the quartz sand mixture is flat, and finally pressing the quartz sand mixture by using a pressing block;
(5) compacting: placing the filled die on a preset four-column hydraulic machine, prepressing for 5min under the condition of the pressing pressure of 80MPa, then controlling the pressure of the press to be 80MPa again, and releasing the pressure after 15min of pressure stabilization;
(6) repeating steps (3) - (5) until the mold is full, wherein the pressure of step (5) is increased by 10MPa when step (5) is repeated every more time;
(7) molding: putting the whole core mould with the pressing block into a constant temperature box, baking under variable temperature and timing conditions, wherein the baking temperature and time are 100 ℃, 240min → 130 ℃, 30min → 210 ℃, 10min → natural cooling;
(8) demolding: and placing the formed core mould on a fixed position of a four-column hydraulic press, and pressing a pressing block to enable the core to be separated from the mould to obtain the core.
Further, the cementing agent in the step (1) mainly comprises the following components in percentage by mass: 9-20% of curing agent, 1-5% of flatting agent, 0.5-1% of barium sulfate and the balance of epoxy resin and polyester, wherein the mass percentage of the epoxy resin to the polyester is 1: 1.
Further, the corresponding relation of the grain size content of the cementing agent in the step (1) is consistent with the grain size proportion of the quartz sand.
Further, in the step (2), a high temperature resistant film is padded between the bottom plate and the side plate of the mold.
Further, in the step (4), after the quartz sand mixture is loaded into the mold, the bridge plug of the quartz sand mixture is released by using a sand homogenizer, so that the quartz sand mixture forms close point contact with each other.
Further, in the step (5), the ultrasonic wave of 90HZ to 150HZ may be simultaneously released to the mold filled with the quartz sand during the process of compacting the quartz sand mixture.
The invention has the beneficial effects that: the invention prepares the compact rock core with large volume, the rock core has the advantage of small dead pore, optimizes the compact sandstone in the laboratory experiment only by coring experiment without the blank of artificial rock core, and provides help for the development of unconventional oil and gas fields.
Detailed Description
The following examples are provided to further illustrate the embodiments of the present invention and are not intended to limit the scope of the present invention.
The invention relates to a preparation method of a rock core for dense conglomerate oil displacement, which comprises the following steps:
(1) mixing quartz sand with certain particle size, clay mineral and cementing agent powder in a certain proportion, and uniformly stirring to obtain a quartz sand mixture; according to the oil reservoir characteristics, filtering screens with different meshes screen quartz sand particles with required sizes, matching with a powder cementing agent (the particle size distribution is 75-100 mu m), and quantitatively weighing clay minerals according to the lithologic mineral content of a sandstone reservoir;
the cementing agent mainly comprises the following components in percentage by mass: 9-20% of curing agent, 1-5% of flatting agent, 0.5-1% of barium sulfate and the balance of epoxy resin and polyester, wherein the mass percentage of the epoxy resin to the polyester is 1: 1. The mass ratio of the quartz sand to the cementing agent is 5-12.5: 1.
The corresponding relationship of the grain size content of the cementing agent is consistent with the grain size ratio of the quartz sand (for example, the sand body has a size of 20 meshes, 120 meshes, 5:1, 80 meshes, 180 meshes), because the cementing agent under the condition has stronger adhesive/consolidation capability, because the grain size of part of the sand body of the quartz sand is larger, the adhesive of the conventional formula can not adhere to the sand body necessarily, the proper grain size ratio can be matched and contacted more reasonably, and the dead pores are increased because the whole size is too small.
(2) Assembling a mold: the die mainly comprises a bottom plate, a side plate and a pressing block, wherein the bottom plate, the side plate and the pressing block are steel plates, the surface roughness Ra of the inner wall is less than or equal to 0.025 mu m, and the geometric size of the square core die is as follows: length × width × height is 305mm × 92mm × 92 mm; a high-temperature resistant film is padded between the bottom plate and the side plate of the die, so that the damage to the bottom of the core in the demolding process is avoided;
the side plate in the die is an integral annular wall and has integrity, and the side plate, the bottom plate and the pressing block are all polished rough on the surface so as to promote the fit of core particles and the die; and the pressing surface of the pressing block is provided with an exhaust hole, so that produced gas in the rock core cavity in the filling process is prevented from impacting rock core particles and cemented particles, and the contact relation of the particles after uniform mixing is changed.
(3) Wetting the mold: before filling sand into the mold, spraying 3mg of target formation water to the lower surface of the sand body to be contacted by a fine water spray head, and uniformly covering; the method aims to adsorb the quartz sand mixture to be filled, reduce the contact between the surface cementing agent and the briquetting and finally avoid the formation of dead pores due to the mass aggregation on the contact surface;
(4) sand homogenizing: weighing quartz sand mixture with the volume of 1/N of that of the mold, filling the quartz sand mixture into the wetted mold, releasing a bridge plug of the quartz sand mixture by using a sand evening device to enable the quartz sand mixture to form close point contact with each other, moving the quartz sand mixture back and forth in the mold along the horizontal direction by using a scraping tool until the surface of the quartz sand mixture is flat, and finally pressing the quartz sand mixture by using a pressing block;
(5) compacting: placing the filled die on a preset four-column hydraulic machine, prepressing for 5min under the condition of the pressing pressure of 80MPa, then controlling the pressure of the press to be 80MPa again, and releasing the pressure after 15min of pressure stabilization; in the process of compacting the quartz sand mixture, 90-150 Hz ultrasonic waves can be released to a mold filled with quartz sand at the same time, and under high pressure, the ultrasonic waves with the wavelength can effectively promote the vertical migration among particles to force the contact to be tighter;
(6) repeating the steps (3) to (5) until the mould is full, wherein when the step (5) is repeated every time, the pressure of the step (5) is increased by 10MPa, the briquetting is fused into a high-temperature oven on the mould, and the gradient pressurization under the pressure condition is the experimental result of multiple rounds in order to keep the straightness in the vertical direction; the cementing agent attached to the surface of the pressed block can be also arranged on the surface of the uppermost rock core after being filled and pressed for many times, so that the cementing agent in each layer is relatively uniform and has uniformity vertically upwards;
(7) molding: putting the whole core mould with the pressing block into a constant temperature box, baking under variable temperature and timing conditions, wherein the baking temperature and time are 100 ℃, 240min → 130 ℃, 30min → 210 ℃, 10min → natural cooling;
(8) demolding: and (3) placing the molded core mold on a fixed position of a four-column hydraulic press, pressing a pressing block to enable the core to be separated from the mold to obtain the core, further modifying the core by adopting a liquid nitrogen cutting machine to set the size of the core to be 300mm multiplied by 89mm, and thus obtaining the artificial core with the core size smaller than 305mm multiplied by 92 mm.
The compact core with the freeze frame of 300mm multiplied by 89mm is prepared by the method, the core has the advantages of large volume and small dead pore, the compact sandstone is optimized only by a coring experiment in an experimental laboratory experiment without the blank of an artificial core, and the method provides help for the development of unconventional oil and gas fields.
Claims (3)
1. A preparation method of a core for dense conglomerate oil displacement is characterized by comprising the following steps:
(1) mixing quartz sand with certain particle size, clay mineral and cementing agent powder in a certain proportion, and uniformly stirring to obtain a quartz sand mixture;
(2) assembling a mold: the die mainly comprises a bottom plate, a side plate and a pressing block, wherein the bottom plate, the side plate and the pressing block are steel plates, the surface roughness Ra of the inner wall is less than or equal to 0.025 mu m, and the geometric size of the square core die is as follows: length × width × height =305mm × 92mm × 92 mm;
(3) wetting the mold: before filling sand into the mold, spraying 3mg of target formation water to the lower surface of the sand body to be contacted by a fine water spray head, and uniformly covering;
(4) sand homogenizing: weighing quartz sand mixture with the volume of 1/N of that of the mold, filling the quartz sand mixture into the wetted mold, moving the quartz sand mixture back and forth in the mold along the horizontal direction by using a strickling tool until the surface of the quartz sand mixture is flat, and finally pressing the quartz sand mixture by using a pressing block;
(5) compacting: placing the filled die on a preset four-column hydraulic machine, prepressing for 5min under the condition of the pressing pressure of 80MPa, then controlling the pressure of the press to be 80MPa again, and releasing the pressure after 15min of pressure stabilization;
(6) repeating steps (3) - (5) until the mold is full, wherein the pressure of step (5) is increased by 10MPa when step (5) is repeated every more time;
(7) molding: putting the whole core mould with the pressing block into a constant temperature box, baking under variable temperature and timing conditions, wherein the baking temperature and time are 100 ℃, 240min → 130 ℃, 30min → 210 ℃, 10min → natural cooling;
(8) demolding: placing the formed core mould on a fixed position of a four-column hydraulic press, and pressing a pressing block to enable the core to be separated from the mould to obtain a core;
the cementing agent in the step (1) consists of the following components in percentage by mass: 9-20% of curing agent, 1-5% of flatting agent, 0.5-1% of barium sulfate and the balance of epoxy resin and polyester, wherein the mass percentage of the epoxy resin to the polyester is 1: 1;
after the quartz sand mixture in the step (4) is filled into a die, a sand homogenizer is used for removing a bridge plug of the quartz sand mixture, so that the quartz sand mixture forms close point contact with each other;
and (5) simultaneously releasing 90-150 Hz of ultrasonic waves to the mold filled with the quartz sand during the process of compacting the quartz sand mixture.
2. The method for preparing the core for compact conglomerate flooding, according to claim 1, is characterized in that the corresponding relation of the grain size content of the cementing agent in the step (1) is consistent with the grain size proportion of quartz sand.
3. The method for preparing the core for compact conglomerate flooding as claimed in claim 2, wherein in the step (2), a high temperature resistant film is padded between the bottom plate and the side plate of the mold.
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| CN108412469B (en) * | 2018-02-14 | 2020-02-07 | 中国石油大学(北京) | Sand filling pipe, preparation method thereof and reservoir seepage simulation method |
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| CN109060484B (en) * | 2018-10-08 | 2021-06-15 | 中国海洋石油集团有限公司 | Large-size rock core for relative permeability curve determination and preparation method thereof |
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| CN111781051B (en) * | 2020-07-09 | 2021-06-25 | 中国石油大学(北京) | Artificial conglomerate core based on lithology and permeability control and preparation method and application thereof |
| CN114428000A (en) * | 2020-10-13 | 2022-05-03 | 中国石油化工股份有限公司 | Natural gas hydrate ore body artificial rock sample material, natural gas hydrate ore body artificial rock sample and preparation method |
| CN113532990B (en) * | 2021-07-15 | 2023-11-14 | 西南石油大学 | Preparation method of compact sandstone oil displacement core with argillaceous interlayer |
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