CN112857934A - Preparation method of high-permeability homogeneous nonmagnetic core - Google Patents

Preparation method of high-permeability homogeneous nonmagnetic core Download PDF

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Publication number
CN112857934A
CN112857934A CN202110087475.9A CN202110087475A CN112857934A CN 112857934 A CN112857934 A CN 112857934A CN 202110087475 A CN202110087475 A CN 202110087475A CN 112857934 A CN112857934 A CN 112857934A
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core
salt
quartz sand
permeability
particle size
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顾春元
狄勤丰
秦荣胜
邱润东
李泳霖
华帅
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University of Shanghai for Science and Technology
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University of Shanghai for Science and Technology
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q

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Abstract

The invention relates to a preparation method of a high-permeability non-magnetic core, which comprises the steps of screening non-magnetic quartz sand and inorganic granular salt which is determined in particle size and is easy to dissolve in water; then fully stirring and uniformly mixing the quartz sand and the cementing agent; then adding inorganic granular salt which is easy to dissolve in water, fully stirring, uniformly filling the inorganic granular salt in the interparticle pores of the quartz sand to play a supporting role, ensuring that the pores do not collapse during pressing, and fully contacting and bonding the quartz sand; and finally, after the core is pressed and dried, soaking in hot water to dissolve salt, enlarging pores, wherein the dissolved pores are positioned at the position of a flow passage, so that the effective porosity and permeability can be increased, and the high-permeability non-magnetic core is prepared. The content and the particle size of the inorganic particle salt are determined according to the physical properties.

Description

Preparation method of high-permeability homogeneous nonmagnetic core
Technical Field
The invention relates to a preparation method of a high-permeability homogeneous non-magnetic core, which improves the pressing pressure of the prepared core by filling gaps among non-magnetic quartz sand grains with soluble granular salt, ensures that the core is cemented without the gaps being collapsed, achieves the purpose of preparing the high-permeability homogeneous core and belongs to the technical field of petroleum engineering development experiments.
Background
The artificial core is a basic material for developing various injection displacement experiments in the field of petroleum development, and is a high-permeability core with the permeability of more than 4000mD and an ultra-low-permeability core with the permeability of less than 1mD, so that the preparation difficulty is high. The non-magnetic core is a special core which can be used for nuclear magnetic resonance core visualization experiments and common flow experiments.
The permeability of the artificial core is related to the particle size of quartz sand, pressing pressure and the content of glue. Under the condition that other conditions are not changed, the larger the particle size is, the larger the gaps among the particles are, and the larger the permeability is; the smaller the pressure, the greater the permeability. For core preparation to simulate formation geology, the particle size and gel content are often limited by the compositional characteristics of the formation itself (size determination) or the size of the silica sand purchased (or the lack of larger silica sand). After the particle size and the gel content of the quartz stone are determined, the permeability is further improved, only the pressing (overlaying) pressure can be reduced, but the gluing between the quartz sand is influenced when the pressing pressure is too low, the gaps between the quartz sand are reduced when the pressure is too high, and the difficulty is how to control the pressure so that the quartz sand can be glued without reducing the permeability.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a preparation method of a high-permeability homogeneous nonmagnetic core. Under the condition that quartz sand and pressure are limited, in order to continuously obtain the high-permeability nonmagnetic artificial core, the invention adopts a soluble inorganic granular salt pre-filling method to improve the supporting strength and meet higher pressing pressure, thereby preparing the high-permeability nonmagnetic artificial core.
In order to achieve the purpose, the invention adopts the following inventive concept:
the method comprises the steps of screening nonmagnetic quartz sand, fully and uniformly stirring the quartz sand and a cementing agent, filling inorganic granular salt which is easy to dissolve in water into inter-granular pores of the quartz sand to play a supporting role, fully bonding the quartz sand among the granules when the pressure is increased and pressing the quartz sand without collapse, and then soaking and dissolving the salt after a core framework is fixed to expand pores, wherein the dissolved pores are positioned at a runner position, so that the effective porosity and the permeability can be increased. And keeping other manufacturing conditions such as overlying pressure, glue content, baking temperature, quartz sand mesh number and the like unchanged, changing the salt content or the particle size of the granular salt, and preparing the high-permeability non-magnetic artificial core.
According to the inventive concept, the invention adopts the following technical scheme:
a preparation method of a high-permeability homogeneous nonmagnetic core comprises the following steps:
1) preparing a non-magnetic material:
processing and sorting inorganic granular salt according to a given grain diameter, and screening nonmagnetic quartz sand; the quartz sand needs to be cleaned and dried, and the particle size is 10-5000 meshes; the inorganic granular salt does not contain metal and various insoluble impurities, and the material needs to be detected to be nonmagnetic;
2) adding glue and stirring:
pouring the dried quartz sand into a stirring pot of a stirrer, adding a cementing agent according to the mass ratio of the cementing agent to the quartz sand of 1-10%, and stirring in a man-machine staggered mode until no caking adhesive is seen and the whole quartz sand is uniform, wherein the stirring time is 20-30 minutes;
3) adding salt and stirring:
adding the granular salt with the determined particle size according to a given proportion, and fully stirring for 10-15 minutes;
4) pressing a rock sample:
filling the stirred mixture into a die, keeping the sand surface flat, and then pushing into a press; adjusting the numerical value of a pressure limiting table of the pressing machine to a set value, starting the pressing machine, and maintaining the pressure for 30min +/-1 min after the set pressure is reached;
5) drying a rock sample:
closing the press, withdrawing the cylinder, taking out the pressed core together with the mold, and then putting the core into an oven, wherein the temperature of the oven is set to be 120 +/-5 ℃, and the drying time is 18-24 hours;
6) cutting a standard rock sample:
taking out the core block, cutting by a cutting machine to prepare a standard blocky rock sample, or drilling a standard columnar rock core by a rock core drilling machine, and cutting the end face of the sample to be flat by the cutting machine;
7) water-soluble desalting:
respectively soaking the rock core in hot water at 40-60 ℃ to remove salt, changing 3-4 times of water in the process, weighing the mass of the rock core until the mass is not changed any more, and accumulating for 12-18 h;
8) and (3) drying to finish the preparation of the rock core:
and drying the desalted core at the temperature of 120 +/-5 ℃ for 12-24 hours to obtain a core finished product, and testing by using a hole-seepage joint-testing device to obtain the permeability of the core.
Preferably, in the step 1), a non-magnetic material is prepared, and the selected inorganic granular salt and quartz sand do not contain metals and various insoluble impurities and are non-magnetic through nuclear magnetic detection; meanwhile, the inorganic particle salt has a determined particle size and an addition proportion, the salt is processed in advance and then the particle size is sorted, the particle size and the content are determined according to the physical property, the particle size is 10 mu m-2 mm, and the mass percentage content is 0-30%.
Preferably, in the steps 2) and 3), a given inorganic salt is required to be added to support the framework and increase the permeability, and the inorganic salt is added after the glue and the large-particle-size quartz sand are fully and uniformly stirred and are not agglomerated, so that the salt particles are prevented from being coated by the glue and being incapable of being dissolved.
Compared with the prior art, the invention has the following obvious prominent substantive characteristics and remarkable advantages:
1. firstly, non-magnetic quartz sand and inorganic salt are preselected, then soluble granular salt is added into the quartz sand which is well mixed by adding glue, so that gaps among quartz sand particles are not reduced during pressing, the pressing force is improved, but the gaps among the particles are not reduced, the permeability is changed by adjusting the proportion of the granular salt and the particle size of the particles, and finally the granular salt is removed by water immersion to prepare the high-permeability artificial core;
2. the method is simple to operate, easy to realize and suitable for popularization and application.
Drawings
FIG. 1 is a flow chart of the preparation process of the present invention.
Fig. 2 is a schematic view of an artificial core.
Detailed Description
The preferred embodiments of the present invention will now be described in detail with reference to the accompanying drawings.
The first embodiment is as follows:
referring to fig. 1, a preparation method of a high-permeability homogeneous nonmagnetic core comprises the following steps:
1) preparing a non-magnetic material:
processing and sorting inorganic granular salt according to a given grain diameter, and screening nonmagnetic quartz sand; the quartz sand needs to be cleaned and dried, and the particle size is 10-5000 meshes; the inorganic granular salt does not contain metal and various insoluble impurities, and the material needs to be detected to be nonmagnetic;
2) adding glue and stirring:
pouring the dried quartz sand into a stirring pot of a stirrer, adding a cementing agent according to the mass ratio of the cementing agent to the quartz sand of 1-10%, and stirring in a man-machine staggered mode until no caking adhesive is seen and the whole quartz sand is uniform, wherein the stirring time is 20-30 minutes;
3) adding salt and stirring:
adding the granular salt with the determined particle size according to a given proportion, and fully stirring for 10-15 minutes;
4) pressing a rock sample:
filling the stirred mixture into a die, keeping the sand surface flat, and then pushing into a press; adjusting the numerical value of a pressure limiting table of the pressing machine to a set value, starting the pressing machine, and maintaining the pressure for 30min +/-1 min after the set pressure is reached;
5) drying a rock sample:
closing the press, withdrawing the cylinder, taking out the pressed core together with the mold, and then putting the core into an oven, wherein the temperature of the oven is set to be 120 +/-5 ℃, and the drying time is 18-24 hours;
6) cutting a standard rock sample:
taking out the core block, cutting by a cutting machine to prepare a standard blocky rock sample, or drilling a standard columnar rock core by a rock core drilling machine, and cutting the end face of the sample to be flat by the cutting machine;
7) water-soluble desalting:
respectively soaking the rock core in hot water at 40-60 ℃ to remove salt, changing 3-4 times of water in the process, weighing the mass of the rock core until the mass is not changed any more, and accumulating for 12-18 h;
8) and (3) drying to finish the preparation of the rock core:
and drying the desalted core at the temperature of 120 +/-5 ℃ for 12-24 hours to obtain a core finished product, and testing by using a hole-seepage joint-testing device to obtain the permeability of the core.
In the embodiment, the easily soluble inorganic granular salt pre-filling method is adopted to improve the supporting strength and meet higher pressing pressure, so that the high-permeability non-magnetic artificial core is prepared.
Example two
This embodiment is substantially the same as the first embodiment, and is characterized in that:
in the step 1), preparing a non-magnetic material, wherein the added inorganic granular salt and quartz sand do not contain metal and various insoluble impurities and are non-magnetic through nuclear magnetic detection; meanwhile, the inorganic particle salt has a determined particle size and an addition proportion, the salt is processed in advance and then the particle size is sorted, the particle size and the content are determined according to the physical property, the particle size is 10 mu m-2 mm, and the mass percentage content is 0-30%.
In the steps 2) and 3), given inorganic salt is required to be added to play roles of supporting a framework and increasing the permeability, and the inorganic salt is added after the glue and the large-particle-size quartz sand are fully and uniformly stirred and are free from agglomeration to prevent the glue from wrapping the salt particles to cause the salt particles to be incapable of being dissolved.
In the embodiment, non-magnetic quartz sand and inorganic salt are preselected, then easily-soluble granular salt is added into the quartz sand which is well mixed by adding glue, so that gaps among quartz sand particles are not reduced during pressing, the pressing force is improved, but the gaps among the particles are not reduced, the permeability is changed by adjusting the proportion of the granular salt and the particle size, and finally the granular salt is removed by water immersion to prepare the high-permeability artificial core.
EXAMPLE III
In this embodiment, an artificial core greater than 4500mD is prepared by the following specific steps:
1) preparation of quartz sand and inorganic particulate salt. Processing refined salt purchased from a supermarket, screening according to the particle size, and weighing 250 g; 1500g of clean 40-60 mesh quartz sand was prepared. The salt and the quartz sand are subjected to magnetic detection by a nuclear magnetic resonance instrument, and can be used without magnetism.
2) Adding glue and stirring. Weighing 1320g of dried 40-60-mesh quartz sand in proportion, and pouring the quartz sand into a stirring pot of a stirrer; then 100g of cementing agent is added, and the mixture is stirred in a man-machine cross mode until no caking exists and the whole mixture is uniform, wherein the stirring time is generally 30 minutes;
3) adding salt and stirring. Adding prepared 40-60 mesh salt according to a designed proportion of 15 percent (namely 250g), and fully stirring for 15 minutes;
4) and (5) pressing the rock sample. The stirred mixture is uniformly filled into a die as much as possible and then pushed into a press; adjusting the numerical value of a pressure limiting table of a pressing machine to 10MPa, starting the pressing machine, and maintaining the pressure for 30min after the pressure reaches a set pressure;
5) and (5) drying the rock sample. Closing the press, withdrawing the cylinder, and taking out the pressed core together with the mold; taking down the pressing cover plate, and putting the pressing cover plate into an oven, wherein the temperature of the oven is set to be 120 ℃, and the baking time is 18 hours;
6) and cutting the standard rock sample. Taking out the core, drilling the core with the diameter of 25mm by using a core drilling machine, and cutting two ends flat by using a cutting machine;
7) dissolving in water to remove salt. Soaking the core with 50 deg.C hot water, removing salt, replacing with 4 times of water, and weighing until the core mass is no longer changed for 12 hr;
8) and drying to finish the preparation of the rock core. And (4) putting the soaked core into an oven to be dried for 18 hours to obtain a finally usable core finished product.
Measuring the average permeability of the rock core by using a hole seepage joint measurement device to be 4637 mD; whereas the average permeability of cores prepared by the conventional method without adding salt under the same parameter conditions was 3812 mD.
In the preparation method of the high-permeability non-magnetic core, non-magnetic quartz sand and inorganic granular salt which is determined in particle size and is easily soluble in water are screened firstly; then fully stirring and uniformly mixing the quartz sand and the cementing agent; then adding soluble inorganic granular salt, fully stirring to uniformly fill the inorganic granular salt in the interparticle pores of the quartz sand to play a supporting role, ensuring that the pores do not collapse during pressing, and enabling the quartz sand to be fully contacted and bonded; and finally, after the core is pressed and dried, soaking in hot water to dissolve salt, enlarging pores, wherein the dissolved pores are positioned at the position of a flow passage, so that the effective porosity and permeability can be increased, and the high-permeability non-magnetic core is prepared. The content and the particle size of the inorganic particle salt are determined according to the physical properties.
The embodiments of the present invention have been described with reference to the accompanying drawings, but the present invention is not limited to the embodiments, and various changes and modifications can be made according to the purpose of the invention, and any changes, modifications, substitutions, combinations or simplifications made according to the spirit and principle of the technical solution of the present invention shall be equivalent substitutions, as long as the purpose of the present invention is met, and the present invention shall fall within the protection scope of the present invention without departing from the technical principle and inventive concept of the present invention.

Claims (3)

1. A preparation method of a high-permeability homogeneous nonmagnetic core is characterized by comprising the following steps:
1) preparing a non-magnetic material:
processing and sorting inorganic granular salt according to a given grain diameter, and screening nonmagnetic quartz sand; the quartz sand needs to be cleaned and dried, and the particle size is 10-5000 meshes; the inorganic granular salt does not contain metal and various insoluble impurities, and the material needs to be detected to be nonmagnetic;
2) adding glue and stirring:
pouring the dried quartz sand into a stirring pot of a stirrer, adding a cementing agent according to the mass ratio of the cementing agent to the quartz sand of 1-10%, and stirring in a man-machine staggered mode until no caking adhesive is seen and the whole quartz sand is uniform, wherein the stirring time is 20-30 minutes;
3) adding salt and stirring:
adding the granular salt with the determined particle size according to a given proportion, and fully stirring for 10-15 minutes;
4) pressing a rock sample:
filling the stirred mixture into a die, keeping the sand surface flat, and then pushing into a press; adjusting the numerical value of a pressure limiting table of the pressing machine to a set value, starting the pressing machine, and maintaining the pressure for 30min +/-1 min after the set pressure is reached;
5) drying a rock sample:
closing the press, withdrawing the cylinder, taking out the pressed core together with the mold, and then putting the core into an oven, wherein the temperature of the oven is set to be 120 +/-5 ℃, and the drying time is 18-24 hours;
6) cutting a standard rock sample:
taking out the core block, cutting by a cutting machine to prepare a standard blocky rock sample, or drilling a standard columnar rock core by a rock core drilling machine, and cutting the end face of the sample to be flat by the cutting machine;
7) water-soluble desalting:
respectively soaking the rock core in hot water at 40-60 ℃ to remove salt, changing 3-4 times of water in the process, weighing the mass of the rock core until the mass is not changed any more, and accumulating for 12-18 h;
8) and (3) drying to finish the preparation of the rock core:
and drying the desalted core at the temperature of 120 +/-5 ℃ for 12-24 hours to obtain a core finished product, and testing by using a hole-seepage joint-testing device to obtain the permeability of the core.
2. The method for preparing the high-permeability homogeneous nonmagnetic core according to claim 1, wherein the method comprises the following steps: in the step 1), preparing a non-magnetic material, wherein the selected inorganic granular salt and quartz sand do not contain metal and various insoluble impurities and do not have magnetism through nuclear magnetic detection; meanwhile, the inorganic particle salt has a determined particle size and an addition proportion, the salt is processed in advance and then the particle size is sorted, the particle size and the content are determined according to the physical property, the particle size is 10 mu m-2 mm, and the mass percentage content is 0-30%.
3. The method for preparing the high-permeability homogeneous nonmagnetic core according to claim 1, wherein the method comprises the following steps: in the steps 2) and 3), given inorganic salt is required to be added to play roles of supporting the framework and increasing the permeability, the glue and the large-particle-size quartz sand are required to be fully stirred uniformly without agglomeration, and then the inorganic salt is added to prevent the glue from wrapping the salt particles, so that the salt particles cannot be dissolved.
CN202110087475.9A 2021-01-22 2021-01-22 Preparation method of high-permeability homogeneous nonmagnetic core Pending CN112857934A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20100324868A1 (en) * 2009-06-22 2010-12-23 Russell Mark C Core Sample Preparation, Analysis, And Virtual Presentation
CN104089806A (en) * 2014-07-17 2014-10-08 中国石油大学(华东) Man-made rock core with multi-pore structure and preparation method of man-made rock core
CN204064753U (en) * 2013-12-26 2014-12-31 中国石油天然气集团公司 A kind of reservoir core sample preparation system
CN105738179A (en) * 2016-04-18 2016-07-06 西南石油大学 Manufacturing method of low-cost sandstone artificial rock core for experimental teaching
CN110361241A (en) * 2019-08-13 2019-10-22 山东科技大学 A kind of rocks in direct tension sample quick preparation device and preparation method

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20100324868A1 (en) * 2009-06-22 2010-12-23 Russell Mark C Core Sample Preparation, Analysis, And Virtual Presentation
CN204064753U (en) * 2013-12-26 2014-12-31 中国石油天然气集团公司 A kind of reservoir core sample preparation system
CN104089806A (en) * 2014-07-17 2014-10-08 中国石油大学(华东) Man-made rock core with multi-pore structure and preparation method of man-made rock core
CN105738179A (en) * 2016-04-18 2016-07-06 西南石油大学 Manufacturing method of low-cost sandstone artificial rock core for experimental teaching
CN110361241A (en) * 2019-08-13 2019-10-22 山东科技大学 A kind of rocks in direct tension sample quick preparation device and preparation method

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
臧士宾等: "核磁共振技术在储层评价中的应用研究――以青海柴达木盆地为例", 《青海石油》 *

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