Device and method for crystallization of developer in pores for imaging hydrophilic pores in rocks

Through the method of crystal precipitation of imaging agents in the hydrophilic pores of rocks and combined with a variety of imaging technologies, the problem of difficulty in characterizing the distribution of hydrophilic pores in the rocks in the existing technology is solved, and high-resolution display of hydrophilic pores inside the rocks is achieved. Study on image and distribution characteristics.

CN114813495BActive Publication Date: 2025-02-14CHINA PETROLEUM & CHEMICAL CORP +1
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Patent Information

Application Number
CN202110059420.7
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2021-01-18
Publication Date
2025-02-14
Estimated Expiration
2041-01-18

AI Technical Summary

Technical Problem

The prior art is difficult to accurately characterize the distribution and wettability of hydrophilic pores inside rocks, especially in low-pore-low permeability rocks.

Method used

The device and method of crystallization of imaging agents in pores is used to study the distribution of hydrophilic pores inside rocks through imaging agent solutions, combined with X-ray CT scanning, microscope sheet observation and scanning electron microscope observation. feature.

Benefits of technology

The study of high-resolution imaging and distribution characteristics of hydrophilic pores inside the rock has been achieved, which can be suitable for fresh and long-term rock samples and supports multiple repeated observations.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention discloses a device and method for crystallizing a developer in pores for imaging hydrophilic pores of rocks, wherein the method comprises the following steps: step 1, selecting a developer; step 2, preparing a developer solution; step 3, preparing and installing a sample; step 4, connecting a device; step 5, controlling crystallization conditions; step 6, after crystallization is completed, the rock sample is removed for standby use. The developer can be crystallized into tiny crystals in the hydrophilic pores of the rock by local rapid evaporation and / or heating-cooling methods, so as to observe and describe the distribution characteristics of the hydrophilic pores inside the rock by X-ray CT scanning imaging, microscope thin section observation, scanning electron microscope observation and the like. The method can be applied to both fresh rock samples and samples that have been placed for a long time, and can be repeatedly observed and described.
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Description

Technical Field

[0001] The invention relates to the technical field of geological exploration and oil layer physics, in particular to a device and method for crystallizing a developer in pores for imaging hydrophilic pores of rocks. Background Art

[0002] The wettability of rock pores (oil-wetting or water-wetting) directly affects the contact mode between the rock pore surface and the fluid, the oil-water interfacial tension, etc., and indirectly affects the development potential of rock fluids and the measures taken. In rocks, especially low-porosity and low-permeability rocks, the rock mineral composition and pore types are complex, resulting in complex and variable wettability of the pore surface. In addition, the oil-wetting or water-wetting property of rock pores is also related to the fluid that the rock has been immersed in for a long time, and there is a wettability reversal. At present, the main methods for testing the oil-wetting and water-wetting properties of rocks include the self-imbibition method and the contact angle measurement method. The self-imbibition method measures the oil-wetting and water-wetting properties of the entire rock, and the contact angle measurement method can only measure the wettability of the macroscopic smooth surface of the rock. The above two methods cannot characterize the distribution of hydrophilic pores inside the rock. The X-ray CT scanning method and the focused ion beam-scanning electron microscope method can finely observe the pore structure characteristics and spatial distribution inside the rock. However, it is impossible to judge the wettability of the internal pore space or pore surface. In view of the above problems, the present invention provides a device and method for crystallizing a developer in pores for imaging hydrophilic pores in rocks.

[0003] Publication (announcement) number: CN107614992B, Publication (announcement) date: 2020-11-24 Disclosed is a hot and cold cabinet, comprising: a main body having a door on the front surface; an internal groove arranged in the main body; a temperature-controlled radiator having a bottom plate and a plurality of fins formed on one surface of the bottom plate, and the other surface of the bottom plate is arranged along the back surface of the internal groove; a heater for heating the temperature-controlled radiator; a temperature-controlled fan arranged on the one surface side of the temperature-controlled radiator to blow air in the internal groove to the fins of the temperature-controlled radiator; a shielding plate having a temperature-controlled fan relative portion, the temperature-controlled fan relative portion having a plurality of through holes and being opposite to the temperature-controlled radiator The shielding plate is arranged on the one surface side of the temperature-regulating radiator relative to the fan, so as to shield the area where the temperature-regulating radiator is arranged in a state where air blowing outlets are formed on the upper and lower sides of the internal groove; the radiator is arranged on the outside of the back side of the internal groove; the heat dissipation fan blows the air outside the internal groove to the radiator; the Peltier module connects the heat absorption surface to the temperature-regulating radiator and the heat dissipation surface to the radiator; and the power control unit supplies power to the heater and the temperature-regulating fan when heating the internal groove, and supplies power to the temperature-regulating fan, the heat dissipation fan and the Peltier module when cooling the internal groove.

[0004] Publication (announcement) number: CN205718062U, Publication (announcement) date: 2016-11-23. It relates to a refrigeration and heating box, including a box, a refrigeration system and a heating system; the box is a rectangular box, the refrigeration system and the heating system are installed in the box, the refrigeration system is composed of a compressor, a condenser, a capillary tube, a drying filter, an evaporator copper tube and a fan, and the heating system is composed of a fan and an electric heating wire; the compressor is connected in series with the evaporator copper tube, the capillary tube, the drying filter and the condenser, the evaporator copper tube is installed at the rear end of the fixed frame, the condenser is wound on the fixed frame, the electric heating rod is installed inside the fixed frame, the front section of the fixed frame is provided with a fan motor and a fan, and the control panel installed on the inner side of the front section of the box is connected with the compressor, the condenser, the fan motor and the electric heating rod; the front section of the box is provided with an air outlet corresponding to the fan. The utility model has the characteristics of both refrigeration and heating, simple structure, low cost and portability.

[0005] Publication (announcement) number: CN102530442B, Publication (announcement) date: 2014-03-05 An intelligent heating and refrigeration dual-purpose tank container is disclosed, comprising a main frame, a tank body is arranged inside the main frame, a step ladder is arranged at one end of the main frame, a refrigerant channel is arranged on the tank body, a refrigeration compressor unit is arranged at the lower end of the outer side of the tank body, a liquid inlet pipeline and a liquid return pipeline are respectively connected to the refrigeration compressor unit, a digital recorder and an electric control cabinet are arranged at one end of the tank body, an expansion tank is arranged above the refrigerant channel, the coil channel is divided into a first coil channel and a second coil channel from the liquid inlet pipeline, valves are arranged at the lowest points of the liquid inlet pipeline and the liquid return pipeline, and an insulation layer is arranged at the outer periphery and both ends of the tank body, and the insulation layer covers the coil channel. The invention has the advantages of convenient operation, exquisite structure, capable of realizing refrigeration and heating of the tank body, and capable of meeting the needs of complex transportation environment and diverse transportation items.

[0006] The article "Wettability, Pore Connectivity and Fluid-Tracer Migration of Shahejie Formation Shale Oil Reservoirs in Dongying Depression" (Acta Petrolei Sinica, Issue 3, 2018, author: Hu Qinhong, et al.) was published, which described the polar and non-polar tracers with different molecular sizes and reactivity developed by them, and applied them to capillary self-imbibition (distilled water and n-decane containing tracers) and saturated diffusion (brine containing tracers) experiments. The samples after the experiment were detected by laser ablation-inductively coupled plasma-mass spectrometry to detect the distribution behavior and migration rate of tracers in mixed wettability shales. This method is different from the method of determining the distribution of hydrophilic pores by observing the distribution of developer crystals in the pores of the present invention. This method studies the internal lipophilic or hydrophilic characteristics at different levels by detecting changes in tracer concentration. The self-absorbed samples obtained by this method need to be quickly tested for tracers, otherwise the loss of tracers after being placed for a period of time will lead to large deviations in the results. The samples containing developer crystals obtained by the present invention can be placed for a long time or observed multiple times.

[0007] The article "Research on Microscopic Physical Simulation Experiment of Water-Drive Oil" (Daqing Petroleum Geology and Development, 2002, No. 1, author: Jia Zhongwei, etc.) uses the microscopic oil-drive experimental procedure of the microscopic simulation model to study the seepage law of water-drive oil: the model is emptied and saturated with water, and then the simulated oil is used to drive the water (or the simulated oil is directly emptied). Then the water-drive oil experiment is carried out at an appropriate speed, and the images of the experimental process are recorded by computer and video recorder respectively, so as to study the development characteristics of water-wet or oil-wet pores. This method is only applicable to the development characteristics of water-wet pores that can be observed by the camera on the rock surface, and cannot study the development characteristics of water-wet pores in the internal structure of the rock.

[0008] The public invention application "A new method and device for measuring rock wettability by resistance method" (application number: 201710824893.5, application date: 2017.09.14) discloses a new method and device for measuring rock wettability by resistance method. Provide consistent and stable measurement conditions; monitor the change of rock sample resistance during the entire measurement process; replace the fluid in the sample inlet (lower end) pipeline with the injection fluid (crude oil), keep the oil interface between the sample and the electrode, and form self-priming conditions; monitor the change of rock resistance and the change of liquid level in the metering tube during the self-priming process, and this change of liquid level can be regarded as the liquid level in the Amott method; establish the corresponding resistivity wettability index and wettability discrimination standard. Characterize rock wettability by real-time monitoring the change of rock resistivity during the "self-priming discharge" process, which solves the problem that the existing technology does not consider the influence of sample size and measurement conditions on rock wettability, improves the credibility and measurement accuracy of rock wettability, and provides an experimental basis for reservoir evaluation and transformation. The wettability obtained by this method is the overall comprehensive wettability of the rock, which is not suitable for observing and determining the development characteristics of hydrophilic pores inside the rock.

[0009] In summary, the technical solutions of the above-disclosed technologies, the technical problems to be solved, and the beneficial effects produced are all different from the present invention. Regarding more technical features, technical problems to be solved, and beneficial effects of the present invention, the above-disclosed technical documents do not provide any technical inspiration. Summary of the invention

[0010] In view of the above-mentioned defects in the prior art, the purpose of the present invention is to provide a device and method for crystallization of developer in pores for imaging hydrophilic pores in rocks, which can realize the flow of developer solution through hydrophilic pores and crystallization precipitation in hydrophilic pores. It is convenient to combine with other imaging methods to realize the study of the development law of hydrophilic pores in rocks, and then study the wettability of rocks.

[0011] In order to achieve the above object, the present invention adopts the following technical solutions:

[0012] A device for crystallizing a developer in pores for imaging hydrophilic pores of rocks, comprising a crystallization tube, a wide-mouth evaporator, and a developer solution storage container;

[0013] The upper port of the crystallization tube is connected and communicated with the wide-mouth evaporator, and the lower port of the crystallization tube is connected and communicated with the lower port of the developer solution storage container through a pipeline;

[0014] The wide-mouth evaporator and the developer solution storage container are at the same height, that is, the liquid level of the wide-mouth evaporator and the liquid level of the developer solution storage container are at the same height and are at the same horizontal plane.

[0015] Furthermore, the pipeline is a U-shaped pipeline, and the U-shaped pipeline includes a lower connecting pipe of the crystallization tube and a connecting pipe which are connected to each other as one body, and a two-way valve is installed on the lower connecting pipe of the crystallization tube;

[0016] The upper end of the lower connecting tube of the crystallization tube is connected to the lower port of the crystallization tube;

[0017] The upper end of the connecting pipe is connected to the lower end of the developer solution storage container.

[0018] Further, it also includes a heating-refrigeration box;

[0019] The crystallization tube is placed inside the heating-refrigeration box.

[0020] Further, it also includes a heating-refrigeration box controller;

[0021] The heating-refrigeration box is electrically connected to the heating-refrigeration box controller.

[0022] Furthermore, it also includes a developer solution storage bottle;

[0023] The developer solution storage bottle has a liquid outlet, the developer solution storage container has a liquid inlet, and the liquid outlet of the developer solution storage bottle is communicated with the liquid inlet of the developer solution storage container.

[0024] Further, it also includes a developer solution filter;

[0025] The inlet of the developer solution filter is communicated with the liquid outlet of the developer solution storage bottle, and the outlet of the developer solution filter is communicated with the liquid inlet of the developer solution storage container.

[0026] In order to achieve the above object, the present invention adopts the following technical solutions:

[0027] A method for crystallizing using a device for crystallizing an imaging agent in a pore for imaging hydrophilic pores of rocks comprises the following steps:

[0028] Step 1: Select the developer: Select the developer that needs to crystallize in the hydrophilic pores of the rock;

[0029] Step 2, preparation of developer solution: preparing the developer into a saturated or nearly saturated solution and placing it into a developer solution storage bottle;

[0030] Step 3: Sample preparation and installation: The rock sample is made into a cylindrical shape and installed in a crystallization tube, and an impermeable material is filled between the crystallization tube and the rock sample;

[0031] Step 4, solution introduction: introduce the solution into the entire device so that the liquid levels in the solution storage bottle, the solution storage container and the wide-mouth evaporator are at the same height;

[0032] Step 5: Control of crystallization conditions: On the one hand, a wide-mouth evaporator is used to naturally volatilize the developer solution; on the other hand, a heating-cooling box is used to control the temperature of the crystallization tube so that the solution flowing through the pores of the rock reaches a saturated state and crystallizes.

[0033] Furthermore, it also includes:

[0034] Step 6. After crystallization is completed, remove the rock sample and set aside.

[0035] Furthermore, the temperature control range of the heating-refrigeration box is 0-90°C, and the temperature control accuracy is ±0.1°C.

[0036] Compared with the prior art, the present invention has the following beneficial effects:

[0037] The device and method for crystallizing developer in pores for imaging hydrophilic pores in rocks provided by the present invention can utilize local rapid evaporation or heating-cooling methods to make the developer crystallize into tiny crystals in the hydrophilic pores of rocks, so as to observe and describe the distribution characteristics of hydrophilic pores in rocks by X-ray CT scanning imaging, microscope thin section observation, scanning electron microscope observation, etc. The method can be applied to both fresh rock samples and samples that have been placed for a long time, and can perform repeated observation and description for many times. BRIEF DESCRIPTION OF THE DRAWINGS

[0038] Figure 1 The present invention is a schematic structural diagram of a device for crystallizing a developer in pores for imaging hydrophilic pores in rocks.

[0039] In the figure: 1-crystallization tube; 2-rock sample; 3-wide-mouth evaporator; 4-heating-refrigeration box; 5-heating-refrigeration box controller; 6-connecting pipe under the crystallization tube; 7-two-way valve; 8-connecting pipe; 9-solution intermediate storage; 10-solution filter; 11-solution storage bottle. DETAILED DESCRIPTION

[0040] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0041] Embodiment 1:

[0042] See also Figure 1 , the present invention provides a technical solution:

[0043] The device for crystallizing a developer in pores for imaging hydrophilic pores of rocks comprises: a crystallization tube 1; a rock sample 2; a wide-mouth evaporator 3; a heating-refrigeration box 4; a heating-refrigeration box controller 5; a connecting pipe 6 under the crystallization tube; a two-way valve 7; a connecting pipe 8; a solution storage device 9; a solution filter 10; and a solution storage bottle 11.

[0044] The crystallization tube 1 is used to crystallize the solution in the pores of the rock sample. It is placed in a heating-refrigeration box 4, and the rock sample 2 to be measured is placed inside the crystallization tube 1. The upper part of the crystallization tube 1 is connected to a wide-mouth evaporator 3, and the lower part of the crystallization tube 1 is connected to a lower connecting tube 6 of the crystallization tube.

[0045] The lower part of the wide-mouth evaporator 3 is connected to the crystallization tube 1. The wide-mouth evaporator 3 is a shallow and wide-mouthed vessel used to evaporate the reagent so that the solution in the hydrophilic pores in the rock is saturated and crystallized.

[0046] The heating-cooling box 4 is used to heat or cool the crystallization tube 1, and utilizes the temperature change to promote the crystallization of the developer in the solution in the hydrophilic pores inside the rock. The temperature control range is 0-90°C, and the temperature control accuracy is ±0.1°C.

[0047] The heating-refrigerating box controller 5 is used to control the temperature of the heating-refrigerating box 4. The heating-refrigerating box 4 and the heating-refrigerating box controller 5 are well-known technologies in the art, and the present invention can directly use them without further description, and those skilled in the art will understand.

[0048] A two-way valve 7 is connected to the lower connecting pipe 6 of the crystallization tube.

[0049] The connecting pipe 8 is connected between the lower connecting pipe 6 of the crystallization tube and the solution storage container 9 , and is used to dynamically balance the liquid levels of the wide-mouth evaporator 3 and the solution storage container 9 .

[0050] The solution storage container 9 is used to store the solution so as to continuously replenish the solution into the crystallization tube 1 and the wide-mouth evaporator 3 .

[0051] The solution filter 10 is connected between the solution storage container 9 and the solution storage bottle 11, and is used to filter solid impurities in the solution flowing from the solution storage bottle 11 to the solution storage container 9 to ensure that the solution entering the crystallization tube 1 is free of impurities.

[0052] The solution storage bottle 11 is used to contain and store the solution of the reagents required for the preparation of the experiment.

[0053] The working principle and mechanism of the device for crystallization of developer in pores for imaging hydrophilic pores of rocks of the present invention can be described as follows:

[0054] A saturated or nearly saturated aqueous solution of the developer is passed through a solution filter into a solution storage container. The liquid levels in the solution storage bottle, the solution storage container, and the wide-mouth evaporator are the same. The developer solution flowing through the hydrophilic pores of the rock is promoted to crystallize in two ways: one is to slowly evaporate the reagent through a wide-mouth evaporator, causing the developer in the crystallization tube to be saturated and crystallized; the other is to promote the supersaturation of the developer solution in the rock sample in the crystallization tube by changing and controlling the temperature of the crystallization tube (cooling or heating) and causing crystallization. The reduction in the developer concentration in the solution caused by solvent evaporation or developer crystallization can be continuously replenished by the diffusion of the solution solute in the solution storage container and the solution storage bottle.

[0055] After the rock sample has been subjected to developer crystallization in the hydrophilic pores, the distribution of the hydrophilic pores in the rock can be observed using a variety of methods, including: (1) performing X-ray CT scanning on the rock sample to determine the hydrophilic pores of the rock by observing the development sites of the developer particles; (2) making thin sections of the rock sample to study the characteristics of the hydrophilic pores by observing the distribution of the developer particles on the thin sections; and (3) using a focused ion beam-scanning electron microscope to observe the developer particles to determine the development characteristics of the hydrophilic pores.

[0056] A method for crystallizing a developer in a pore for imaging hydrophilic pores in rocks comprises the following steps:

[0057] Step 1: Select the developer: select the reagent that needs to crystallize in the hydrophilic pores of the rock, select the developer reagent that does not exist in the rock mineral components or rock fluids, has a large specific gravity, and can form tiny particle crystals, preferably analytically pure manganese chloride as the developer.

[0058] Step 2, preparation of developer solution: according to the experimental conditions, temperature and solubility data of the developer, the developer is configured into a saturated or nearly saturated solution and loaded into a solution storage bottle. A preferred embodiment uses a uniform mixture of analytically pure manganese chloride and water as the developer solution. The mass ratio of analytically pure manganese chloride to water is: 42.4% analytically pure manganese chloride, 57.6% distilled water.

[0059] Among them, the developer is configured into a saturated or nearly saturated solution according to the experimental conditions, temperature and solubility data of the developer. This is a routine technique of those skilled in the art and can be directly used in the present invention without further elaboration, which is clear to those skilled in the art.

[0060] Step 3: Sample preparation and installation: Make the rock sample into a cylindrical shape with a diameter slightly smaller than the inner diameter of the crystallization tube. Place the rock sample in the crystallization tube, and fill the space between the crystallization tube and the rock sample with impermeable materials, such as waterproof glue and sealing rubber.

[0061] The impermeable material is not used to block the crystallization tube. For example, a relatively viscous and quickly solidified waterproof glue is used to fill only the space between the rock sample and the wall of the crystallization tube. Due to its rapid solidification, it will not penetrate into the interior of the rock, thereby maintaining the vertical connectivity of the hydrophilic pores of the rock, ensuring that the solution in the developer solution storage container can replenish the solution in the wide-mouth evaporator.

[0062] Step 4: Solution introduction: introduce the solution into the entire device so that the liquid levels in the solution storage bottle, the solution storage container and the wide-mouth evaporator are at the same height.

[0063] Step 5: Control of crystallization conditions: On the one hand, a wide-mouth evaporator is used to naturally volatilize the developer solution; on the other hand, the temperature of the crystallization tube is controlled so that the solution flowing through the pores of the rock reaches a saturated state and crystallizes.

[0064] Step 6. After crystallization is completed, remove the rock sample and set aside.

[0065] The device and method for crystallizing developer in pores for imaging hydrophilic pores in rocks provided by the present invention can utilize local rapid evaporation or heating-cooling methods to make the developer crystallize into tiny crystals in the hydrophilic pores of rocks, so as to observe and describe the distribution characteristics of hydrophilic pores in rocks by X-ray CT scanning imaging, microscope thin section observation, scanning electron microscope observation, etc. The method can be applied to both fresh rock samples and samples that have been placed for a long time, and can perform repeated observation and description for many times.

[0066] Embodiment 2:

[0067] See also Figure 1 , the present invention provides a technical solution:

[0068] A method for crystallizing a developer in a pore for imaging hydrophilic pores in rocks comprises the following steps:

[0069] Step 1: Select the developer: select the reagent that needs to crystallize in the hydrophilic pores of the rock, select the developer reagent that does not exist in the rock mineral components or rock fluids, has a large specific gravity, and can form tiny particle crystals, preferably analytically pure manganese chloride as the developer.

[0070] Step 2, preparation of developer solution: according to the experimental conditions, temperature and solubility data of the developer, the developer is configured into a saturated or nearly saturated solution and loaded into a solution storage bottle. A preferred embodiment uses a uniform mixture of analytically pure manganese chloride and water as the developer solution. The mass ratio of analytically pure manganese chloride to water is: 42.4% analytically pure manganese chloride, 57.6% distilled water.

[0071] Among them, the developer is configured into a saturated or nearly saturated solution according to the experimental conditions, temperature and solubility data of the developer. This is a routine technique of those skilled in the art and can be directly used in the present invention without further elaboration, which is clear to those skilled in the art.

[0072] Step 3, sample preparation and installation: Make the rock sample into a cylindrical shape with a diameter slightly smaller than the inner diameter of the crystallization tube. Place the rock sample in the crystallization tube, and fill the space between the crystallization tube and the rock sample with impermeable materials, such as waterproof glue and sealing rubber. The impermeable material is not used to block the crystallization tube. For example, a relatively viscous and fast-solidifying waterproof glue is used to fill the space between the rock sample and the wall of the crystallization tube. Due to the fast solidification, it will not penetrate into the interior of the rock, so that the hydrophilic pores of the rock can be maintained from top to bottom, ensuring that the solution in the developer solution storage container can replenish the solution in the wide-mouth evaporator.

[0073] Step 4: Solution introduction: introduce the solution into the entire device so that the liquid levels in the solution storage bottle, the solution storage container and the wide-mouth evaporator are at the same height.

[0074] Step 5: Control of crystallization conditions: Use a wide-mouth evaporator to naturally volatilize the developer solution so that the solution flowing through the pores of the rock reaches a saturated state and crystallizes.

[0075] Embodiment 3:

[0076] See also Figure 1 , the present invention provides a technical solution:

[0077] A method for crystallizing a developer in a pore for imaging hydrophilic pores in rocks comprises the following steps:

[0078] Step 1: Select the developer: select the reagent that needs to crystallize in the hydrophilic pores of the rock, select the developer reagent that does not exist in the rock mineral components or rock fluids, has a large specific gravity, and can form tiny particle crystals, preferably analytically pure manganese chloride as the developer.

[0079] Step 2, preparation of developer solution: according to the experimental conditions, temperature and solubility data of the developer, the developer is configured into a saturated or nearly saturated solution and loaded into a solution storage bottle. A preferred embodiment uses a uniform mixture of analytically pure manganese chloride and water as the developer solution. The mass ratio of analytically pure manganese chloride to water is: 42.4% analytically pure manganese chloride, 57.6% distilled water.

[0080] Among them, the developer is configured into a saturated or nearly saturated solution according to the experimental conditions, temperature and solubility data of the developer. This is a routine technique of those skilled in the art and can be directly used in the present invention without further elaboration, which is clear to those skilled in the art.

[0081] Step 3, sample preparation and installation: Make the rock sample into a cylindrical shape with a diameter slightly smaller than the inner diameter of the crystallization tube. Place the rock sample in the crystallization tube, and fill the space between the crystallization tube and the rock sample with impermeable materials, such as waterproof glue and sealing rubber. The impermeable material is not used to block the crystallization tube. For example, a relatively viscous and fast-solidifying waterproof glue is used to fill the space between the rock sample and the wall of the crystallization tube. Due to the fast solidification, it will not penetrate into the interior of the rock, so that the hydrophilic pores of the rock can be maintained from top to bottom, ensuring that the solution in the developer solution storage container can replenish the solution in the wide-mouth evaporator.

[0082] Step 4: Solution introduction: introduce the solution into the entire device so that the liquid levels in the solution storage bottle, the solution storage container and the wide-mouth evaporator are at the same height.

[0083] Step 5: Control of crystallization conditions: Control the temperature of the crystallization tube by a heating-cooling box so that the solution flowing through the pores of the rock reaches a saturated state and crystallizes.

[0084] Although all the above embodiments use Figure 1 However, as a person skilled in the art can clearly know, there is no need to provide a separate drawing to represent, as long as the missing parts or structural features in the embodiment are removed from the drawing. This is clear to those skilled in the art. Of course, the embodiment with more parts is only the optimal embodiment, and the embodiment with fewer parts is the basic embodiment, but it can also achieve the basic purpose of the present invention, so all these variant embodiments are within the protection scope of the present invention.

[0085] All parts and components not discussed in detail in this application and the connection methods of the parts and components in this application belong to the well-known technology in this technical field and will not be described in detail, such as welding, threaded connection, etc.

[0086] In the present invention, the term "plurality" refers to two or more than two, unless otherwise clearly defined. The terms "installed", "connected", "connected", "fixed" and the like should be understood in a broad sense. For example, "connected" can be a fixed connection, a detachable connection, or an integral connection; "connected" can be a direct connection or an indirect connection through an intermediate medium. For those of ordinary skill in the art, the specific meanings of the above terms in the present invention can be understood according to the specific circumstances.

[0087] In the description of the present invention, it is necessary to understand that the directions or positional relationships indicated by terms such as “upper”, “lower”, “left”, “right”, “front” and “back” are based on the directions or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or unit referred to must have a specific direction, be constructed and operated in a specific orientation, and therefore, cannot be understood as a limitation on the present invention.

[0088] In the description of this specification, the description of the terms "one embodiment", "some embodiments", "specific embodiments", etc. means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representation of the above terms does not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in any one or more embodiments or examples in a suitable manner.

[0089] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. For those skilled in the art, the present invention may have various modifications and variations. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

Claims

1. A device for crystallizing a developer in pores for imaging hydrophilic pores in rocks, characterized in that: It includes a crystallization tube, a wide-mouth evaporator, and a developer solution storage container; The upper port of the crystallization tube is connected and communicated with the wide-mouth evaporator, and the lower port of the crystallization tube is connected and communicated with the lower port of the developer solution storage container through a pipeline; The wide-mouth evaporator and the developer solution storage container are at the same height, that is, the liquid level of the wide-mouth evaporator and the liquid level of the developer solution storage container are the same and are on the same horizontal plane; the connecting pipe is connected between the lower connecting pipe of the crystallization tube and the solution intermediate storage container.

2. The device for crystallization of developer in pores for imaging hydrophilic pores in rocks according to claim 1, characterized in that: The pipeline is a U-shaped pipeline, which includes a lower connecting pipe of the crystallization tube and a connecting pipe which are connected to each other as one body, and a two-way valve is installed on the lower connecting pipe of the crystallization tube; The upper end of the lower connecting tube of the crystallization tube is connected to the lower port of the crystallization tube; The upper end of the connecting pipe is connected to the lower end of the developer solution storage container.

3. The device for crystallization of developer in pores for imaging hydrophilic pores of rocks according to claim 1 or 2, characterized in that: Also included are heating-cooling boxes; The crystallization tube is placed inside the heating-refrigeration box.

4. The device for crystallization of developer in pores for imaging hydrophilic pores in rocks according to claim 3, characterized in that: Also included is a heating-cooling box controller; The heating-refrigeration box is electrically connected to the heating-refrigeration box controller.

5. The device for crystallization of developer in pores for imaging hydrophilic pores of rocks according to claim 4, characterized in that: Also included is a developer solution storage bottle; The developer solution storage bottle has a liquid outlet, the developer solution storage container has a liquid inlet, and the liquid outlet of the developer solution storage bottle is communicated with the liquid inlet of the developer solution storage container.

6. The device for crystallizing developer in pores for imaging hydrophilic pores of rocks according to claim 5, characterized in that: Also included is a developer solution filter; The inlet of the developer solution filter is communicated with the liquid outlet of the developer solution storage bottle, and the outlet of the developer solution filter is communicated with the liquid inlet of the developer solution storage container.

7. A method for crystallizing a developer in pores for imaging hydrophilic pores of rocks using the device for crystallizing a developer in pores of claim 6, characterized in that: The following steps are involved: Step 1: Select the developer: Select the developer that needs to crystallize in the hydrophilic pores of the rock; Step 2, preparation of developer solution: preparing the developer into a saturated or nearly saturated solution and placing it into a developer solution storage bottle; Step 3: Sample preparation and installation: The rock sample is made into a cylindrical shape and placed in a crystallization tube, and an impermeable material is filled between the crystallization tube and the rock sample; Step 4, solution introduction: introduce the solution into the entire device so that the liquid levels in the solution storage bottle, the solution storage container and the wide-mouth evaporator are at the same height; Step 5: Control of crystallization conditions: On the one hand, a wide-mouth evaporator is used to naturally volatilize the developer solution; on the other hand, a heating-cooling box is used to control the temperature of the crystallization tube so that the solution flowing through the pores of the rock reaches a saturated state and crystallizes.

8. The crystallization method according to claim 7, characterized in that Also includes: Step 6. After crystallization is completed, remove the rock sample and set aside.

9. The crystallization method according to claim 7, characterized in that The temperature control range of the heating-refrigeration box is 0-90°C, and the temperature control accuracy is ±0.1°C.

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