CN109187303B - Preparation method of transparent core for directly observing core seepage phenomenon - Google Patents
Preparation method of transparent core for directly observing core seepage phenomenon Download PDFInfo
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- CN109187303B CN109187303B CN201810873627.6A CN201810873627A CN109187303B CN 109187303 B CN109187303 B CN 109187303B CN 201810873627 A CN201810873627 A CN 201810873627A CN 109187303 B CN109187303 B CN 109187303B
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- 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
- G01N1/42—Low-temperature sample treatment, e.g. cryofixation
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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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Abstract
The invention discloses a preparation method of a transparent core for directly observing core seepage phenomenon, which comprises the following steps: preparing a sodium silicate solution, and adding fumed silica; placing a glass plate at the bottom of the container, and pouring a sodium silicate solution containing silicon dioxide into the container; transferring the container into a cold trap, cooling and carrying out constant temperature treatment to obtain frozen glass and ice blocks; transferring the frozen glass and ice blocks into a freeze dryer to obtain a glass plate with a sodium silicate sponge structure growing on the surface of one side; taking two glass plates, overlapping the two glass plates, enabling the smooth surfaces to face outwards, and mutually extruding a sodium silicate sponge structure between the two glass plates by utilizing self gravity; then horizontally placing the overlapped glass plates in a muffle furnace, and heating to make part of sodium silicate enter a molten state; cooling to obtain a glass plate with a large number of gaps in the middle, and obtaining the transparent core. The prepared transparent core can be directly used for recording and observing the movement process of fluid in the pore by optical equipment.
Description
Technical Field
The invention relates to a core material, in particular to a preparation method of a transparent core for directly observing a seepage phenomenon
Background
In the research of oil extraction technology, the flow characteristics of oil in rock are one of the most important research contents. Whether the injection of water into a formation or the study of the effects of chemicals on oil recovery requires fluid seepage characteristics in the rock as an important parameter. However, most of the current research is to judge the rock characteristics through statistics of experimental results. For example, the permeability of rock can only be expressed by the flow rate per unit time under a certain pressure condition. The problems of influence of large and small gaps on the flow direction, fluid adsorption around a rock skeleton and the like in the flow process cannot be described in detail, and due to the opaque characteristics of the rock, the interaction between a plurality of rock gaps and the fluid cannot be observed. For the core needing to know the shape of the internal pores urgently, means such as freezing cutting or grinding are needed, the cost is high, and the original pore characteristics are damaged. This situation still exists in common man-made cores. In order to observe the phenomenon of fluid flow in the pores, the related art mainly uses laser to etch a pattern on the glass, and simulates and observes the seepage characteristics of the fluid in the rock by observing the flow of the fluid in the pattern. In addition to the high cost of laser etching, the geometric characteristics of the patterns are greatly different from the shapes of naturally formed pores, and the recovery degree of the fluid in the flowing process of the pores is not ideal.
Disclosure of Invention
The invention aims to provide a preparation method of a transparent core capable of directly observing core seepage phenomenon. The prepared transparent core can be directly used for recording and observing the movement process of fluid in the pore by optical equipment.
The technical scheme adopted by the invention is as follows:
the preparation method of the transparent core for directly observing the core seepage phenomenon comprises the following steps:
step one, preparing a sodium silicate solution, and adding fumed silica into the solution under the stirring condition;
placing a glass plate at the bottom of the container, pouring a sodium silicate solution containing silicon dioxide into the container, and ensuring that the liquid level is higher than the surface of the glass plate;
transferring the container into a cold trap, cooling and carrying out constant temperature treatment to obtain frozen glass and ice blocks;
transferring the frozen glass and ice blocks into a freeze dryer, and regulating the pressure to 5-10 Pa; keeping the pressure constant for 12 hours to obtain a glass plate with a sodium silicate sponge structure growing on the surface of one side;
step five, two glass plates obtained in the step four are taken and placed in an overlapping mode, the smooth surfaces face outwards, and the sodium silicate sponge structures between the two glass plates are mutually extruded by utilizing the self gravity;
step six, horizontally placing the overlapped glass plates in a muffle furnace, and heating to enable part of sodium silicate to enter a molten state so as to adjust the size of a pore and fix the relative position between the two glass plates;
and step seven, cooling to obtain a glass plate with a large number of gaps in the middle, namely the transparent core capable of directly observing the seepage phenomenon.
In the first step, the mass concentration of the sodium silicate solution is 0.1-1%.
In the first step, the mass ratio of the sodium silicate to the silicon dioxide is 2: 1-1: 1.
In the second step, the glass plate is quartz glass.
In the second step, the liquid level is 5-10mm higher than the surface of the glass flat plate.
In the third step, the temperature is reduced to-50 ℃.
In the seventh step, the heating treatment is specifically carried out by raising the temperature to 1090 ℃ at the speed of 3 ℃/min and keeping the temperature for 10 min.
In the second step, the glass plate is quartz glass.
Compared with the prior art, the invention has the beneficial effects that:
the core is prepared by growing a sponge structure on the surface of a glass plate by utilizing a freeze drying technology to form natural random gaps. The silicate framework is used for high-temperature melting, and the glass plate bonding work is finished smoothly when the size distribution range of the void degree voids is adjusted. The prepared transparent core can be directly used for recording and observing the movement process of fluid in the pore by optical equipment. The method has the following specific advantages:
1. compared with a natural core and a conventional artificial core, the fluid movement process can be visually observed. And the inner skeleton component of the core is silicate, does not contain organic binder, and has physical and chemical properties close to those of rock components in the stratum.
2. The photoetching technology is utilized to etch lines, when the pressure of injected liquid is higher, a continuous plane space exists on the surface of an original glass plate, the liquid can flow on the plane without obstacles, and the flow is different from a random curve flow path in a gap. Is not conducive to fluid motion analysis. Additional pressure is applied to eliminate the planar space between the glass sheets if this is to be eliminated. The void shapes in the present invention are random and distributed closer to the rock voids. Especially on the surface of the glass plate, a continuous plane space can not be formed, because the silicate on the surface of the glass can be used as a crystal nucleus when the sodium silicate is separated out in the sponge forming process, namely the sponge structure on the surface of the glass grows on the surface of the glass. When fluid flows in a transparent environment, the path shape is closer to the path of motion in the rock.
3. The silicate framework is utilized for fusion bonding, so that organic binders can be prevented from forming organic surfaces to influence the wettability of pore surfaces.
Drawings
FIG. 1 is a smooth bore in a transparent core prepared in example 1;
fig. 2 is an irregular pore canal in a transparent core prepared in example 1.
Detailed Description
The invention relates to a transparent core capable of directly observing core seepage phenomenon, which comprises a glass flat plate as a carrier, a sodium silicate solution and fumed silica. Wherein the mass ratio of the sodium silicate to the silicon dioxide is 2: 1-1: 1. The glass plate used is a quartz glass which remains unmelted when the sodium silicate is melted.
The preparation method of the transparent core capable of directly observing the core seepage phenomenon is realized by the following steps:
step one, preparing and adjusting sodium silicate solution to make the concentration range of the sodium silicate solution be 0.1-1%, and adding fumed silica into the solution under the condition of rapid stirring. The mass ratio of the sodium silicate to the silicon dioxide is 2: 1-1: 1.
And step two, placing a glass plate at the bottom of the container, pouring the sodium silicate solution containing silicon dioxide into the container, and ensuring that the liquid level is 5-10mm higher than the surface of the glass plate.
And step three, transferring the container to a cold trap, and cooling to-50 ℃. Keeping the temperature for 5 hours.
And step four, transferring the frozen glass and ice blocks into a freeze dryer, and adjusting the pressure to 5-10 Pa. Constant pressure for 12 h. And obtaining the glass plate with the sodium silicate sponge structure growing on the surface of one side.
And step five, two glass plates with sponge structures are overlapped, and the smooth surfaces face outwards. The middle sodium silicate sponge structures are mutually extruded by utilizing the self gravity.
And step six, horizontally placing the overlapped glass plates in a muffle furnace, heating to 1090 ℃ at the speed of 3 ℃/min, and keeping the temperature for 10min to ensure that part of sodium silicate enters a molten state so as to adjust the size of the pore and fix the relative position between the two glass plates.
And seventhly, cooling to obtain the glass plate with a large number of gaps in the middle, namely the transparent core capable of directly observing the seepage phenomenon.
The core is made by growing a sponge structure on the surface of a glass plate by using a freeze drying technology to form natural random gaps. The silicate framework is used for high-temperature melting, and the glass plate bonding work is finished smoothly when the size distribution range of the void degree voids is adjusted.
Example 1
100ml of a sodium silicate solution having a concentration of 1% was prepared, and 1g of fumed silica was added to the solution under rapid stirring. After uniform dispersion, 50ml of dispersion liquid is poured on the surface of 10 multiplied by 10cm quartz glass by using a baffle, transferred to a cold trap, cooled to minus 50 ℃ to form ice blocks with the thickness of 0.5cm on the surface of the glass, the glass with the ice blocks is transferred to a freeze dryer, the pressure is adjusted to be 5Pa, the constant pressure time is 12 hours, and the glass plate with the sponge structure growing on the single surface is obtained. Two glass plates with sponges growing on the single surfaces are stacked, the smooth surfaces are outside, the glass plates are transferred to a muffle furnace, the temperature is increased to 1090 ℃ at the speed of 3 ℃/min, the temperature is kept for 10min, part of sodium silicate enters a molten state, and therefore the size of the pore is adjusted and the relative position between the two glass plates is fixed. And cooling to obtain the transparent core capable of directly observing the core seepage phenomenon. The morphology of the channels in the transparent core is shown in fig. 1 and fig. 2, and different types of seepage channels in the core can be reflected.
Example 2
200ml of a sodium silicate solution having a concentration of 0.1% was prepared, and 0.1g of fumed silica was added to the solution under rapid stirring. After uniform dispersion, 100ml of dispersion liquid is poured on the surface of quartz glass with the thickness of 10 multiplied by 10cm by using a baffle, the quartz glass is transferred to a cold trap, the temperature is reduced to minus 50 ℃, ice blocks with the thickness of 1cm are formed on the surface of the glass, the glass with the ice blocks is transferred to a freeze dryer, the pressure is adjusted to 10Pa, the constant pressure time is 12 hours, and the glass plate with the sponge structure growing on the single surface is obtained. Two glass plates with sponges growing on the single surfaces are stacked, the smooth surfaces are outside, the glass plates are transferred to a muffle furnace, the temperature is increased to 1090 ℃ at the speed of 3 ℃/min, the temperature is kept for 10min, part of sodium silicate enters a molten state, and therefore the size of the pore is adjusted and the relative position between the two glass plates is fixed. And cooling to obtain the transparent core capable of directly observing the core seepage phenomenon.
Example 3
100ml of a sodium silicate solution having a concentration of 0.5% was prepared, and 1.0g of fumed silica was added to the solution under rapid stirring. After uniform dispersion, 50ml of dispersion liquid is poured on the surface of 10 multiplied by 10cm quartz glass by using a baffle, transferred to a cold trap, cooled to minus 50 ℃ to form ice blocks with the thickness of 0.5cm on the surface of the glass, the glass with the ice blocks is transferred to a freeze dryer, the pressure is adjusted to be 8Pa, the constant pressure time is 12 hours, and the glass plate with the sponge structure growing on the single surface is obtained. Two glass plates with sponges growing on the single surfaces are stacked, the smooth surfaces are outside, the glass plates are transferred to a muffle furnace, the temperature is increased to 1090 ℃ at the speed of 3 ℃/min, the temperature is kept for 10min, part of sodium silicate enters a molten state, and therefore the size of the pore is adjusted and the relative position between the two glass plates is fixed. And cooling to obtain the transparent core capable of directly observing the core seepage phenomenon.
Example 4
200ml of a sodium silicate solution having a concentration of 0.8% was prepared, and 0.8g of fumed silica was added to the solution under rapid stirring. After uniform dispersion, 100ml of dispersion liquid is poured on the surface of 10 multiplied by 10cm quartz glass by using a baffle, the quartz glass is transferred to a cold trap, the temperature is reduced to minus 50 ℃, ice blocks with the thickness of 1cm are formed on the surface of the glass, the glass with the ice blocks is transferred to a freeze dryer, the pressure is adjusted to be 6Pa, the constant pressure time is 12 hours, and the glass plate with the sponge structure growing on the single surface is obtained. Two glass plates with sponges growing on the single surfaces are stacked, the smooth surfaces are outside, the glass plates are transferred to a muffle furnace, the temperature is increased to 1090 ℃ at the speed of 3 ℃/min, the temperature is kept for 10min, part of sodium silicate enters a molten state, and therefore the size of the pore is adjusted and the relative position between the two glass plates is fixed. And cooling to obtain the transparent core capable of directly observing the core seepage phenomenon.
The foregoing is a more detailed description of the invention and it is not intended that the invention be limited to the specific embodiments described herein, but that various modifications, alterations, and substitutions may be made by those skilled in the art without departing from the spirit of the invention, which should be construed to fall within the scope of the invention as defined by the appended claims.
Claims (7)
1. The preparation method of the transparent core for directly observing the core seepage phenomenon is characterized by comprising the following steps of: the method comprises the following steps:
step one, preparing a sodium silicate solution, and adding fumed silica into the solution under the stirring condition;
placing a glass plate at the bottom of the container, pouring a sodium silicate solution containing silicon dioxide into the container, and ensuring that the liquid level is higher than the surface of the glass plate;
transferring the container into a cold trap, cooling and carrying out constant temperature treatment to obtain frozen glass and ice blocks;
transferring the frozen glass and ice blocks into a freeze dryer, and regulating the pressure to 5-10 Pa; keeping the pressure constant for 12 hours to obtain a glass plate with a sodium silicate sponge structure growing on the surface of one side;
step five, two glass plates obtained in the step four are taken and placed in an overlapping mode, the smooth surfaces face outwards, and the sodium silicate sponge structures between the two glass plates are mutually extruded by utilizing the self gravity;
step six, horizontally placing the overlapped glass plates in a muffle furnace, and heating to enable part of sodium silicate to enter a molten state so as to adjust the size of a pore and fix the relative position between the two glass plates;
and step seven, cooling to obtain a glass plate with a large number of gaps in the middle, namely the transparent core capable of directly observing the seepage phenomenon.
2. The method for preparing the transparent core for directly observing the core seepage phenomenon according to claim 1, wherein the method comprises the following steps: in the first step, the mass concentration of the sodium silicate solution is 0.1-1%.
3. The method for preparing the transparent core for directly observing the core seepage phenomenon according to claim 1, wherein the method comprises the following steps: in the first step, the mass ratio of the sodium silicate to the silicon dioxide is 2: 1-1: 1.
4. The method for preparing the transparent core for directly observing the core seepage phenomenon according to claim 1, wherein the method comprises the following steps: in the second step, the glass plate is quartz glass.
5. The method for preparing the transparent core for directly observing the core seepage phenomenon according to claim 1, wherein the method comprises the following steps: in the second step, the liquid level is 5-10mm higher than the surface of the glass flat plate.
6. The method for preparing the transparent core for directly observing the core seepage phenomenon according to claim 1, wherein the method comprises the following steps: in the third step, the temperature is reduced to-50 ℃.
7. The method for preparing the transparent core for directly observing the core seepage phenomenon according to claim 1, wherein the method comprises the following steps: in the sixth step, the heating treatment is specifically carried out by raising the temperature to 1090 ℃ at the speed of 3 ℃/min and keeping the temperature for 10 min.
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| CN110733192B (en) * | 2019-10-08 | 2020-07-17 | 中国矿业大学 | Manufacturing method of organic glass tube for sandstone seepage model |
| CN111122270A (en) * | 2020-01-02 | 2020-05-08 | 陕西科技大学 | Silicate high-porosity artificial core and preparation method thereof |
| CN114935486B (en) * | 2022-06-06 | 2023-04-11 | 陕西科技大学 | Heterogeneous core material based on corn straw core and preparation method thereof |
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