CN114935486A - Heterogeneous core material based on corn straw core and preparation method thereof - Google Patents
Heterogeneous core material based on corn straw core and preparation method thereof Download PDFInfo
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- 239000011162 core material Substances 0.000 title claims abstract description 167
- 239000010902 straw Substances 0.000 title claims abstract description 97
- 240000008042 Zea mays Species 0.000 title claims abstract description 85
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 title claims abstract description 85
- 235000002017 Zea mays subsp mays Nutrition 0.000 title claims abstract description 85
- 235000005822 corn Nutrition 0.000 title claims abstract description 85
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 39
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 claims abstract description 32
- VZTDIZULWFCMLS-UHFFFAOYSA-N ammonium formate Chemical compound [NH4+].[O-]C=O VZTDIZULWFCMLS-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000001035 drying Methods 0.000 claims abstract description 17
- 239000005051 trimethylchlorosilane Substances 0.000 claims abstract description 16
- 238000002791 soaking Methods 0.000 claims abstract description 15
- 239000012173 sealing wax Substances 0.000 claims abstract description 13
- 238000004108 freeze drying Methods 0.000 claims abstract description 8
- 238000011156 evaluation Methods 0.000 claims abstract description 5
- 239000002253 acid Substances 0.000 claims abstract description 4
- 238000012544 monitoring process Methods 0.000 claims abstract description 4
- 238000007598 dipping method Methods 0.000 claims abstract description 3
- NASVITFAUKYCPM-UHFFFAOYSA-N ethanol;tetraethyl silicate Chemical compound CCO.CCO[Si](OCC)(OCC)OCC NASVITFAUKYCPM-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000001993 wax Substances 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 28
- UUYKGYZJARXSGB-UHFFFAOYSA-N ethanol;ethoxy(trihydroxy)silane Chemical compound CCO.CCO[Si](O)(O)O UUYKGYZJARXSGB-UHFFFAOYSA-N 0.000 claims description 20
- 230000032683 aging Effects 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 7
- 235000019441 ethanol Nutrition 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 230000002378 acidificating effect Effects 0.000 claims description 3
- 230000003301 hydrolyzing effect Effects 0.000 claims description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 3
- 230000007062 hydrolysis Effects 0.000 claims 1
- 238000006460 hydrolysis reaction Methods 0.000 claims 1
- 239000012530 fluid Substances 0.000 abstract description 13
- 230000008859 change Effects 0.000 abstract description 6
- 239000000126 substance Substances 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 238000004088 simulation Methods 0.000 abstract description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 14
- 239000011435 rock Substances 0.000 description 13
- 230000014759 maintenance of location Effects 0.000 description 10
- 239000007787 solid Substances 0.000 description 10
- 239000011148 porous material Substances 0.000 description 9
- 239000006004 Quartz sand Substances 0.000 description 8
- 238000009826 distribution Methods 0.000 description 7
- 239000002245 particle Substances 0.000 description 7
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 description 6
- 239000000499 gel Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 238000001879 gelation Methods 0.000 description 5
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- 239000013067 intermediate product Substances 0.000 description 5
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- 229920000647 polyepoxide Polymers 0.000 description 4
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- 239000000835 fiber Substances 0.000 description 3
- 230000002209 hydrophobic effect Effects 0.000 description 3
- 239000011859 microparticle Substances 0.000 description 3
- 230000000877 morphologic effect Effects 0.000 description 2
- 238000010979 pH adjustment Methods 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 238000003892 spreading Methods 0.000 description 2
- 230000007480 spreading Effects 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- ILRRQNADMUWWFW-UHFFFAOYSA-K aluminium phosphate Chemical compound O1[Al]2OP1(=O)O2 ILRRQNADMUWWFW-UHFFFAOYSA-K 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000002734 clay mineral Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
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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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Abstract
The invention discloses a heterogeneous core material based on corn straw cores and a preparation method thereof, belongs to the field of new material-related services, and particularly relates to a motion change evaluation and monitoring technology of fluids and chemical substances in a porous environment. The preparation method of the heterogeneous core material based on the corn straw core comprises the following steps: dipping the corn straw cores by using an ammonium formate solution, and freeze-drying; the freeze-dried corn straw core is transversely placed, the end part of the freeze-dried corn straw core is sealed with wax, tetraethoxysilane ethanol sol is laterally soaked, the freeze-dried corn straw core is kept stand in a water bath, gel is formed under the weak acid condition, and the freeze-dried corn straw core is kept stand and aged in a sealed water bath; removing the end sealing wax, removing surface gel, soaking with a trimethylchlorosilane solution, and drying at high temperature to obtain the heterogeneous core material based on the corn straw core. The heterogeneous core prepared by the invention has an excellent natural core simulation effect by utilizing the characteristics of similar axial direction environment and radial direction gap change of a water transportation channel structure specific to a natural straw core.
Description
Technical Field
The invention belongs to the field of new material related services, relates to a heterogeneous core material based on a corn straw core and a preparation method thereof, and particularly relates to a motion change evaluation and monitoring technology of fluids and chemical substances in a porous environment.
Background
In the field of oilfield chemistry, rock cores are required to be used for testing the motion change rules of various fluids and chemical substances in a porous environment. The artificial core can overcome the problem of high sampling cost and has excellent experimental repeatability. The artificial rock core is generally provided with three types of quartz sand epoxy resin cementation, quartz sand filling tubes and quartz sand aluminum phosphate cementation, and a quartz sand epoxy resin cementation model is the most widely applied at present.
CN204532344U discloses an artificial rock core, is formed by silica sand epoxy resin cement, and it includes that the cross section is square and is rectangular form core body, be equipped with a blind hole along its length direction on the core body, be filled with the quartz sand in the blind hole, the particle size of quartz sand is between 35-40 meshes. CN102628761B discloses an artificial long rock core and a preparation method thereof, wherein the rock core is composed of quartz sand and cement, the quartz sand and the cement are weighed according to requirements, mixed evenly and put into a square steel mould, pressed and dried by a pressure tester, slotted by a cutting machine, and finally cast and sealed by epoxy resin on the external surfaces of the slotted and rock core to obtain the rock core with the permeability of 1 mD-10000 mD, the slotted rock core is in a strip shape, the length of 200 cm-3000 cm, and the sectional area of 6.25cm 2 ～144cm 2 Total pore volume of strip core is 1000cm 3 ～50000cm 3 . However, such artificial cores have in common that they are isotropic. When the retention problem of micro particles or the spreading problem of fluid are researched, the isotropic characteristics of the common artificial rock core cannot reflect the particle retention and fluid distribution characteristics.
Controlling the similarity of pore structure, adding clay minerals, controlling wettability, reducing the influence of temperature, humidity and artificial operating factors during the manufacturing process of the model, which are problems that the preparation of the artificial core must face. In the prior art, the simulated rock core in the seepage characteristic evaluation is usually similar in seepage environment in the horizontal direction and obviously changed in permeability and voidage in the vertical direction, which are the structural characteristics of the rock core caused by the sedimentation process. Therefore, how to provide a core material can better simulate the retention of micro particles or the spreading problem of fluid, and has important significance for the research of the motion change rule of various fluids and chemical substances in the porous environment in the field of oilfield chemistry.
Disclosure of Invention
The invention aims to solve the problem that the isotropic characteristic of a common artificial rock core cannot reflect the characteristics of particle retention and fluid distribution when the retention problem of micro particles or the sweep problem of fluid are researched.
Based on the purpose, the invention provides a heterogeneous core material based on a corn straw core and a preparation method thereof.
In one aspect, the invention relates to a preparation method of a heterogeneous core material based on corn straw cores, which comprises the following steps: dipping the corn straw cores by using an ammonium formate solution, and freeze-drying; the freeze-dried corn straw core is transversely placed, the end part of the freeze-dried corn straw core is sealed with wax, tetraethoxysilane ethanol sol is laterally infiltrated, and the freeze-dried corn straw core is sealed and subjected to standing aging in a water bath after being subjected to standing in a weak acid condition to form gel; removing end sealing wax, removing surface gel, soaking with trimethylchlorosilane solution, and drying at high temperature to obtain heterogeneous core material based on corn straw core.
Further, in the preparation method of the heterogeneous core material based on the corn straw core, the preparation method of the ethyl orthosilicate ethanol sol comprises the following steps: hydrolyzing the ethyl orthosilicate ethanol solution under an alkaline condition to obtain the highly-dispersed and stable ethyl orthosilicate ethanol sol.
Further, in the preparation method of the heterogeneous core material based on the corn straw core, the volume ratio of ethyl orthosilicate, ethanol and water in an ethyl orthosilicate ethanol solution is (20-35) to (50-65) to (7-10); the use concentration of the ethyl orthosilicate ethanol solution is 28-35 wt%.
Further, in the preparation method of the heterogeneous core material based on the corn straw core, the alkaline condition is that the pH value is 9-10; hydrolyzing in a constant-temperature water bath at 20-50 ℃ for 40-100 min, wherein the stirring speed is 200-600 r/min; specifically, an ammonia water solution with the mass concentration of 25-28% is selected for pH adjustment.
Further, in the preparation method of the heterogeneous core material based on the corn straw core, the using concentration of the ammonium formate solution is 40 wt%; the weak acidic condition is that the pH value is 6-7; standing in a water bath to form gel at the temperature of 30-60 ℃; standing and aging in a sealed water bath at the temperature of 30-60 ℃ for 1-5 days; preferably, the weakly acidic conditions are pH 7; specifically, acetic acid with a mass concentration of 10% is selected for pH adjustment.
Further, in the preparation method of the heterogeneous core material based on the corn straw core, the trimethylchlorosilane solution is diluted by normal hexane; the usage concentration of the trimethylchlorosilane solution is 10 percent in terms of volume fraction; soaking in a trimethylchlorosilane solution for 1-2 days; removing the surface gel, namely placing the gel in absolute ethyl alcohol for 3 hours, and repeating for 3-5 times; the high-temperature drying temperature is 300-400 ℃, and the drying time is 6-8 h.
In order to better simulate a radial seepage environment, the invention selects the corn straw core as an artificial core main body. The corn straw core is rich in crude fiber, lignin and the like, and has stable chemical properties, and the internal fiber morphological characteristics can fully reflect the particle retention problem. The silicon dioxide gel has hydrophobic and oleophylic characteristics and a dense pore channel structure, is used for enriching the framework inside the corn straw core, and is soaked in a trimethylchlorosilane solution to reform the framework into a partial hydrophobic structure. The heterogeneous core material based on the corn straw core provided by the invention can well reflect the particle retention problem and the fluid distribution characteristics in the core. Therefore, the invention further claims a heterogeneous core material based on the corn straw core, which is prepared by the method; the artificial core is prepared from the heterogeneous core material based on the corn straw core; and the artificial core is applied to seepage characteristic evaluation monitoring and is used for simulating a radial seepage environment.
Compared with the prior art, the invention has the following beneficial effects or advantages:
the invention discloses a heterogeneous core material based on corn straw cores and a preparation method thereof, wherein the heterogeneous core material takes natural corn straw cores as raw materials and has the characteristics of similar axial direction environment and radial direction gap change of a water transportation channel structure; the internal fiber morphological structure and the compact pore canal caused by the silica gel are transformed to obtain a partially hydrophobic framework, so that the particle retention problem and the fluid distribution characteristic in the rock core during oil exploitation can be well reflected; according to the invention, cheap corn straws are used as raw materials, so that the preparation cost of the heterogeneous core material can be reduced, and the recycling of the corn straws is realized.
Drawings
Fig. 1 is a scanning electron microscopy microtopography of the heterogeneous core material prepared in example 1.
Detailed Description
The following examples are given to illustrate the technical aspects of the present invention, but the present invention is not limited to the following examples.
Example 1
The embodiment provides a preparation test of a heterogeneous core material based on a corn straw core.
(1) Putting 200mL of prepared 28 wt% ethyl orthosilicate ethanol solution into a 500mL three-necked flask, dropwise adding 25% ammonia water solution into the flask until the pH value is 9, setting the device, putting the device into a 50 ℃ constant-temperature water bath kettle, setting the stirring speed to be 200r/min, and reacting for 40min to obtain highly dispersed stable sol; according to the volume ratio, 200mL of 28 wt% ethyl orthosilicate ethanol solution is directly prepared according to the proportion of 20:50:7 of ethyl orthosilicate, ethanol and water.
(2) Removing the skin of the corn straw to obtain corn straw cores, dividing the corn straw cores into parts with the length of 2cm and the diameter of 2.4cm, weighing 100g of solid ammonium formate, dissolving the solid ammonium formate into 150g of water, soaking one part of corn straw cores by using a prepared ammonium formate solution for 6 hours, and putting the corn straw cores into a vacuum freeze dryer for freeze drying; the dosage of the ammonium formate solution is based on the complete immersion of the corn straw cores.
(3) Transversely placing the freeze-dried straw cores obtained in the step (2), sealing wax at two ends, laterally infiltrating the sol obtained in the step (1), adding 10 wt% acetic acid to adjust the pH value to 6, standing in a constant-temperature water bath at 60 ℃, sealing after gelation, continuing to stand in the water bath, and aging for 1 day.
(4) And (4) taking out the intermediate product obtained in the step (3), removing end sealing wax, placing in absolute ethyl alcohol for 3 hours, repeating for 3 times, soaking for 2 days by using a trimethylchlorosilane solution with the volume fraction of 10%, taking out the straw core, drying the surface by using filter paper, and placing in an oven for drying at the high temperature of 300 ℃ for 8 hours to obtain the heterogeneous core material constructed by the corn straw core.
Example 2
The embodiment provides a preparation test of a heterogeneous core material based on a corn straw core.
(1) Putting 200mL of prepared 30 wt% ethyl orthosilicate ethanol solution into a 500mL three-necked flask, dropwise adding 25% ammonia water solution into the flask until the pH value is 9, setting the device, putting the device into a 30 ℃ constant-temperature water bath kettle, setting the stirring speed to be 400r/min, and reacting for 80min to obtain highly dispersed stable sol; according to the volume ratio, 200mL of 30 wt% ethyl orthosilicate ethanol solution is prepared according to the proportion of 30:60:8 of ethyl orthosilicate, ethanol and water.
(2) Removing the skin of the corn straws to obtain corn straw cores, dividing the corn straw cores into parts with the length of 2cm and the diameter of 2.4cm, weighing 100g of solid ammonium formate, dissolving the solid ammonium formate into 150g of water, soaking one part of the corn straw cores by using a prepared ammonium formate solution for 8 hours, and putting the corn straw cores into a vacuum freeze dryer for freeze drying; the dosage of the ammonium formate solution is based on the complete immersion of the corn straw cores.
(3) Transversely placing the freeze-dried straw cores obtained in the step (2), sealing wax at two ends, laterally infiltrating the sol obtained in the step (1), adding 10 wt% acetic acid to adjust the pH value to 7, standing in a constant-temperature water bath at 40 ℃, sealing after gelation, continuing to stand in the water bath, and aging for 3 days.
(4) And (4) taking out the intermediate product obtained in the step (3), removing end sealing wax, placing in absolute ethyl alcohol for 3h, repeating for 4 times, soaking for 2 days by using a trimethylchlorosilane solution with the volume fraction of 10%, taking out the straw core, drying the surface by using filter paper, and placing in an oven for drying at the high temperature of 300 ℃ for 8h to obtain the heterogeneous core material constructed by the corn straw core.
Example 3
The embodiment provides a preparation test of a heterogeneous core material based on a corn straw core.
(1) Putting 150mL of prepared 35 wt% ethyl orthosilicate ethanol solution into a 500mL three-necked flask, dropwise adding 25% ammonia water solution into the flask until the pH value is 9, setting the device, putting the device into a 50 ℃ constant-temperature water bath kettle, setting the stirring speed to be 400r/min, and reacting for 50min to obtain highly dispersed stable sol; according to the volume ratio, 150mL of 35 wt% ethyl orthosilicate ethanol solution is prepared according to the proportion of ethyl orthosilicate, ethanol and water being 35:65: 10.
(2) Removing the skin of the corn straw to obtain corn straw cores, dividing the corn straw cores into parts with the length of 2cm and the diameter of 2.4cm, weighing 100g of solid ammonium formate, dissolving the solid ammonium formate into 150g of water, soaking one part of corn straw cores by using a prepared ammonium formate solution for 8 hours, and putting the corn straw cores into a vacuum freeze dryer for freeze drying; the dosage of the ammonium formate solution is based on the complete immersion of the corn straw cores.
(3) Transversely placing the freeze-dried straw cores obtained in the step (2), sealing wax at two ends, laterally infiltrating the sol obtained in the step (1), adding 10 wt% acetic acid to adjust the pH value to 7, standing in a constant-temperature water bath at 40 ℃, sealing after gelation, continuing to stand in the water bath, and aging for 3 days.
(4) And (4) taking out the intermediate product obtained in the step (3), removing end sealing wax, placing in absolute ethyl alcohol for 3 hours, repeating for 3 times, soaking in 10 volume percent trimethylchlorosilane solution for 2 days, taking out the straw core, drying the surface of the straw core by using filter paper, and placing in an oven for drying at 300 ℃ for 8 hours to obtain the heterogeneous core material constructed by the corn straw core.
Example 4
The embodiment provides a preparation test of a heterogeneous core material based on a corn straw core.
(1) Placing 100mL of prepared 35 wt% ethyl orthosilicate ethanol solution in a 500mL three-necked flask, dropwise adding 25% ammonia water solution until the pH value is 9, building a device, placing the device in a 50 ℃ constant-temperature water bath kettle, setting the stirring speed to be 600r/min, and reacting for 100min to obtain highly dispersed stable sol; according to the volume ratio, 100mL of 35 wt% ethyl orthosilicate ethanol solution is prepared according to the proportion of ethyl orthosilicate, ethanol and water being 35:65: 10.
(2) Removing the skin of the corn straws to obtain corn straw cores, dividing the corn straw cores into parts with the length of 2cm and the diameter of 2.4cm, weighing 100g of solid ammonium formate, dissolving the solid ammonium formate into 150g of water, soaking one part of the corn straw cores by using a prepared ammonium formate solution for 8 hours, and putting the corn straw cores into a vacuum freeze dryer for freeze drying; the dosage of the ammonium formate solution is based on the complete immersion of the corn straw cores.
(3) Transversely placing the freeze-dried straw cores obtained in the step (2), sealing wax at two ends, laterally infiltrating the sol obtained in the step (1), adding 10 wt% acetic acid to adjust the pH value to 7, standing in a constant-temperature water bath at 40 ℃, sealing after gelation, continuing to stand in the water bath, and aging for 5 days.
(4) And (4) taking out the intermediate product obtained in the step (3), removing end sealing wax, placing in absolute ethyl alcohol for 3h, repeating for 4 times, soaking for 2 days by using a trimethylchlorosilane solution with the volume fraction of 10%, taking out the straw core, drying the surface by using filter paper, and placing in an oven for drying at the high temperature of 300 ℃ for 8h to obtain the heterogeneous core material constructed by the corn straw core.
Example 5
The embodiment provides a preparation test of a heterogeneous core material based on a corn straw core.
(1) Putting 150mL of prepared 35 wt% ethyl orthosilicate ethanol solution into a 500mL three-necked flask, dropwise adding 25% ammonia water solution into the flask until the pH value is 9, setting the device, putting the device into a 50 ℃ constant-temperature water bath kettle, setting the stirring speed to be 400r/min, and reacting for 60min to obtain highly dispersed stable sol; according to the volume ratio of 35:65:10 of ethyl orthosilicate, ethanol and water, 100mL of 35 wt% ethyl orthosilicate ethanol solution is prepared
(2) Removing the skin of the corn straw to obtain corn straw cores, dividing the corn straw cores into parts with the length of 2cm and the diameter of 2.4cm, weighing 100g of solid ammonium formate, dissolving the solid ammonium formate into 150g of water, soaking one part of corn straw cores by using a prepared ammonium formate solution for 8 hours, and putting the corn straw cores into a vacuum freeze dryer for freeze drying; the dosage of the ammonium formate solution is based on the complete immersion of the corn straw cores.
(3) Transversely placing the freeze-dried straw cores obtained in the step (2), sealing wax at two ends, laterally infiltrating the sol obtained in the step (1), adding 10 wt% acetic acid to adjust the pH value to 7, standing in a constant-temperature water bath at 50 ℃, sealing after gelation, continuing to stand in the water bath, and aging for 2 days.
(4) And (4) taking out the intermediate product obtained in the step (3), removing end sealing wax, placing in absolute ethyl alcohol for 3h, repeating for 5 times, soaking for 2 days by using a trimethylchlorosilane solution with the volume fraction of 10%, taking out the straw core, drying the surface by using filter paper, and placing in an oven for drying at the high temperature of 300 ℃ for 8h to obtain the heterogeneous core material constructed by the corn straw core.
Example 6
The embodiment provides a performance characterization of a heterogeneous core material based on a corn straw core.
In this example, the properties of the heterogeneous core materials prepared in examples 1 to 5 are represented as shown in table 1.
TABLE 1 porosity distribution of heterogeneous core materials prepared in examples 1-5
The porosity is sequentially increased from inside to outside along the radial direction, the gradient distribution is formed in the range of 40-95%, the highest degree reaches 95%, and the distribution difference on the pores indicates that the obtained heterogeneous core material meets the simulation requirement of detecting the retention degree of the tiny particles among different pores. Under the same pressure condition, polymer solution or other fluids can be retained in different pores after being injected from the cross section, and the seepage capability, the influence range and the like of the fluids under different pores can be described by observing the retention condition in different pores.
As described above, the present invention can be preferably implemented, and the above-mentioned embodiments only describe the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various changes and modifications of the technical solution of the present invention made by those skilled in the art without departing from the design spirit of the present invention shall fall within the protection scope defined by the present invention.
Claims (10)
1. A preparation method of a heterogeneous core material based on corn straw cores is characterized by comprising the following steps:
dipping the corn straw cores by using an ammonium formate solution, and freeze-drying;
the freeze-dried corn straw core is transversely placed, the end part of the freeze-dried corn straw core is sealed with wax, tetraethoxysilane ethanol sol is laterally infiltrated, and the freeze-dried corn straw core is sealed and subjected to standing aging in a water bath after being subjected to standing in a weak acid condition to form gel;
removing the end sealing wax, removing surface gel, soaking with a trimethylchlorosilane solution, and drying at high temperature to obtain the heterogeneous core material based on the corn straw core.
2. The preparation method of the heterogeneous core material based on corn straw cores according to claim 1, wherein the preparation method of the ethyl orthosilicate ethanol sol comprises the following steps: hydrolyzing the ethyl orthosilicate ethanol solution under alkaline conditions to obtain the highly-dispersed and stable ethyl orthosilicate ethanol sol.
3. The method for preparing the heterogeneous core material based on the cornstalk core as claimed in claim 2, wherein the ratio of ethyl orthosilicate, ethanol and water is (20-35): 50-65): 7-10 by volume ratio in the ethyl orthosilicate ethanol solution; the use concentration of the ethyl orthosilicate ethanol solution is 28-35 wt%.
4. The method for preparing the heterogeneous core material based on the corn straw core according to claim 2, wherein the alkaline condition is that the pH value is 9-10;
the hydrolysis is carried out in a constant-temperature water bath at 20-50 ℃ for 40-100 min, and the stirring speed is 200-600 r/min.
5. The method for preparing the heterogeneous core material based on corn straw cores according to claim 1, wherein the ammonium formate solution is used in a concentration of 40 wt%;
the weak acid condition is that the pH value is 6-7;
the temperature for forming gel by standing in the water bath is 30-60 ℃;
the sealed water bath standing aging temperature is 30-60 ℃, and the time is 1-5 days.
6. The method for preparing the heterogeneous core material based on corn straw cores as claimed in claim 5, wherein the weak acidic condition is pH 7.
7. The method for preparing the heterogeneous core material based on cornstalk cores as claimed in claim 1, wherein the trimethylchlorosilane solution is a trimethylchlorosilane solution diluted with n-hexane; the usage concentration of the trimethylchlorosilane solution is 10 percent in volume fraction; the soaking time of the trimethylchlorosilane solution is 1-2 days;
the step of removing the surface gel is to place the gel in absolute ethyl alcohol for 3 hours, and repeat the step for 3-5 times;
the high-temperature drying temperature is 300-400 ℃, and the drying time is 6-8 h.
8. A heterogeneous core material based on corn straw cores, characterized by being prepared by the method of any one of claims 1 to 7.
9. An artificial core prepared from the heterogeneous core material based on cornstalk cores of claim 8.
10. Use of the artificial core according to claim 9 for evaluation and monitoring of seepage characteristics, wherein the artificial core is used to simulate a radial seepage environment.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210628776.2A CN114935486B (en) | 2022-06-06 | 2022-06-06 | Heterogeneous core material based on corn straw core and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210628776.2A CN114935486B (en) | 2022-06-06 | 2022-06-06 | Heterogeneous core material based on corn straw core and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114935486A true CN114935486A (en) | 2022-08-23 |
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Citations (21)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1664547A (en) * | 2005-03-30 | 2005-09-07 | 大庆石油学院 | Quartz sand epoxide-resin agglutinated rock core and method for making same |
| CN102628761A (en) * | 2012-04-10 | 2012-08-08 | 东北石油大学 | Artificial long core and preparation method thereof |
| CN103411804A (en) * | 2013-07-03 | 2013-11-27 | 中国石油天然气股份有限公司 | Heterogeneous cementing core model with high-permeability layer and preparation method thereof |
| 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 |
| CN104111189A (en) * | 2014-07-31 | 2014-10-22 | 中国石油天然气股份有限公司 | Rock core preparation method |
| CN104390825A (en) * | 2014-11-20 | 2015-03-04 | 中国石油大学(北京) | Artificial core containing controllable and movable fluid, and manufacturing method of artificial core |
| CN104458383A (en) * | 2014-12-19 | 2015-03-25 | 西南石油大学 | Method for making artificial rock core |
| CN204532344U (en) * | 2015-03-19 | 2015-08-05 | 丹诺(北京)石油技术服务有限公司 | Artificial core |
| CN105547778A (en) * | 2015-12-17 | 2016-05-04 | 石家庄经济学院 | Preparation method of artificial core in petroleum geology research and application of artificial 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 |
| WO2017024701A1 (en) * | 2015-08-11 | 2017-02-16 | 深圳朝伟达科技有限公司 | Method for preparing drill core |
| CN108426753A (en) * | 2018-01-17 | 2018-08-21 | 中国地质大学（武汉） | A kind of artificial shale core preparation method based on inorganic glue proportioning |
| CN108593385A (en) * | 2018-06-11 | 2018-09-28 | 李战伟 | A kind of artificial mud stone rock core and its preparation method and application |
| CN108956224A (en) * | 2018-05-30 | 2018-12-07 | 中国石油大学(华东) | A kind of artificial core preparation method and device for petroleum geology exploration |
| CN109187303A (en) * | 2018-08-02 | 2019-01-11 | 陕西科技大学 | For directly observing the preparation method of the transparent rock core of rock core percolation phenomenon |
| CN110320076A (en) * | 2019-07-04 | 2019-10-11 | 中国海洋石油集团有限公司 | A kind of artificial carbonate rock rock core and preparation method thereof for developing secondary pore |
| CN111122270A (en) * | 2020-01-02 | 2020-05-08 | 陕西科技大学 | Silicate high-porosity artificial core and preparation method thereof |
| CN111610081A (en) * | 2020-05-09 | 2020-09-01 | 中国科学院地质与地球物理研究所 | Artificial rock core and manufacturing method thereof |
| AU2020103924A4 (en) * | 2020-12-07 | 2021-02-11 | Northeast Petroleum University | Artificial core preparation method for rock drillability test |
| CN112857935A (en) * | 2021-01-22 | 2021-05-28 | 上海大学 | Preparation method of large-grade-difference heterogeneous nonmagnetic core |
| CN114486417A (en) * | 2021-12-25 | 2022-05-13 | 中国石油天然气股份有限公司 | High-fidelity heterogeneous conglomerate artificial core and manufacturing method thereof |
-
2022
- 2022-06-06 CN CN202210628776.2A patent/CN114935486B/en active Active
Patent Citations (21)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1664547A (en) * | 2005-03-30 | 2005-09-07 | 大庆石油学院 | Quartz sand epoxide-resin agglutinated rock core and method for making same |
| CN102628761A (en) * | 2012-04-10 | 2012-08-08 | 东北石油大学 | Artificial long core and preparation method thereof |
| CN103411804A (en) * | 2013-07-03 | 2013-11-27 | 中国石油天然气股份有限公司 | Heterogeneous cementing core model with high-permeability layer and preparation method thereof |
| 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 |
| CN104111189A (en) * | 2014-07-31 | 2014-10-22 | 中国石油天然气股份有限公司 | Rock core preparation method |
| CN104390825A (en) * | 2014-11-20 | 2015-03-04 | 中国石油大学(北京) | Artificial core containing controllable and movable fluid, and manufacturing method of artificial core |
| CN104458383A (en) * | 2014-12-19 | 2015-03-25 | 西南石油大学 | Method for making artificial rock core |
| CN204532344U (en) * | 2015-03-19 | 2015-08-05 | 丹诺(北京)石油技术服务有限公司 | Artificial core |
| WO2017024701A1 (en) * | 2015-08-11 | 2017-02-16 | 深圳朝伟达科技有限公司 | Method for preparing drill core |
| CN105547778A (en) * | 2015-12-17 | 2016-05-04 | 石家庄经济学院 | Preparation method of artificial core in petroleum geology research and application of artificial 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 |
| CN108426753A (en) * | 2018-01-17 | 2018-08-21 | 中国地质大学（武汉） | A kind of artificial shale core preparation method based on inorganic glue proportioning |
| CN108956224A (en) * | 2018-05-30 | 2018-12-07 | 中国石油大学(华东) | A kind of artificial core preparation method and device for petroleum geology exploration |
| CN108593385A (en) * | 2018-06-11 | 2018-09-28 | 李战伟 | A kind of artificial mud stone rock core and its preparation method and application |
| CN109187303A (en) * | 2018-08-02 | 2019-01-11 | 陕西科技大学 | For directly observing the preparation method of the transparent rock core of rock core percolation phenomenon |
| CN110320076A (en) * | 2019-07-04 | 2019-10-11 | 中国海洋石油集团有限公司 | A kind of artificial carbonate rock rock core and preparation method thereof for developing secondary pore |
| CN111122270A (en) * | 2020-01-02 | 2020-05-08 | 陕西科技大学 | Silicate high-porosity artificial core and preparation method thereof |
| CN111610081A (en) * | 2020-05-09 | 2020-09-01 | 中国科学院地质与地球物理研究所 | Artificial rock core and manufacturing method thereof |
| AU2020103924A4 (en) * | 2020-12-07 | 2021-02-11 | Northeast Petroleum University | Artificial core preparation method for rock drillability test |
| CN112857935A (en) * | 2021-01-22 | 2021-05-28 | 上海大学 | Preparation method of large-grade-difference heterogeneous nonmagnetic core |
| CN114486417A (en) * | 2021-12-25 | 2022-05-13 | 中国石油天然气股份有限公司 | High-fidelity heterogeneous conglomerate artificial core and manufacturing method thereof |
Non-Patent Citations (9)
| Title |
|---|
| YANG BAI 等: "Based on self-made shale formation simulated artificial cores to evaluate water-based drilling fluids plugging effect technology" * |
| 周春玲 等: "人造岩心的研制及渗透率影响因素研究", 《石油化工应用》 * |
| 徐宏光 等: "特高渗疏松砂岩人造岩心的制作及评价" * |
| 徐洪波 等: "大庆油田砂岩人造岩心制作方法", 《科学技术与工程》 * |
| 徐洪波: "人造天然岩心的制作与性能评价", 《采油工程文集》 * |
| 熊钰 等: "国内人造岩心物理研究进展", 《天然气与石油》 * |
| 王子振 等: "一种多重孔隙结构人造岩心的制备新方法及其应用" * |
| 王玲: "疏松砂岩人造岩心制作方法研究" * |
| 郑明明 等: "一种物性参数可控的人造长岩心制作技术与影响因素分析", 《地质科技通报》 * |
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