CN111157310A - Rock casting body slice die-casting preparation method - Google Patents
Rock casting body slice die-casting preparation method Download PDFInfo
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- CN111157310A CN111157310A CN201911425444.9A CN201911425444A CN111157310A CN 111157310 A CN111157310 A CN 111157310A CN 201911425444 A CN201911425444 A CN 201911425444A CN 111157310 A CN111157310 A CN 111157310A
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- 239000011435 rock Substances 0.000 title claims abstract description 107
- 238000004512 die casting Methods 0.000 title claims abstract description 85
- 238000005266 casting Methods 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 26
- 239000003822 epoxy resin Substances 0.000 claims abstract description 25
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 25
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 19
- 239000012295 chemical reaction liquid Substances 0.000 claims abstract description 18
- 238000005406 washing Methods 0.000 claims abstract description 15
- 239000003085 diluting agent Substances 0.000 claims abstract description 14
- 239000007788 liquid Substances 0.000 claims abstract description 12
- 239000000243 solution Substances 0.000 claims abstract description 11
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims abstract description 10
- UHOVQNZJYSORNB-UHFFFAOYSA-N benzene Substances C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000002904 solvent Substances 0.000 claims abstract description 5
- 239000011259 mixed solution Substances 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 239000003921 oil Substances 0.000 claims description 33
- 235000019198 oils Nutrition 0.000 claims description 33
- 238000000227 grinding Methods 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 239000002253 acid Substances 0.000 claims description 8
- 235000012343 cottonseed oil Nutrition 0.000 claims description 8
- 239000002385 cottonseed oil Substances 0.000 claims description 8
- 238000005520 cutting process Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 5
- 239000010445 mica Substances 0.000 claims description 4
- 229910052618 mica group Inorganic materials 0.000 claims description 4
- 238000005498 polishing Methods 0.000 claims description 4
- IEQIEDJGQAUEQZ-UHFFFAOYSA-N phthalocyanine Chemical compound N1C(N=C2C3=CC=CC=C3C(N=C3C4=CC=CC=C4C(=N4)N3)=N2)=C(C=CC=C2)C2=C1N=C1C2=CC=CC=C2C4=N1 IEQIEDJGQAUEQZ-UHFFFAOYSA-N 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- 238000011160 research Methods 0.000 abstract description 2
- 239000000975 dye Substances 0.000 description 12
- 239000011148 porous material Substances 0.000 description 11
- 239000003814 drug Substances 0.000 description 9
- 239000000758 substrate Substances 0.000 description 9
- 238000007789 sealing Methods 0.000 description 6
- 238000001802 infusion Methods 0.000 description 5
- 229920005989 resin Polymers 0.000 description 5
- 239000011347 resin Substances 0.000 description 5
- 238000009755 vacuum infusion Methods 0.000 description 5
- 239000012298 atmosphere Substances 0.000 description 4
- 238000011049 filling Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 238000004043 dyeing Methods 0.000 description 3
- 238000005530 etching Methods 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 238000011068 loading method Methods 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 239000004973 liquid crystal related substance Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 230000005587 bubbling Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
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- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 230000010412 perfusion Effects 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 238000012360 testing method Methods 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
-
- 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
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
-
- 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
- G01N1/32—Polishing; Etching
-
- 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
- G01N1/34—Purifying; Cleaning
-
- 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
-
- 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
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2873—Cutting or cleaving
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- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Engineering & Computer Science (AREA)
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- Molecular Biology (AREA)
- Casting Or Compression Moulding Of Plastics Or The Like (AREA)
Abstract
The invention provides a method for preparing a rock casting body slice by die casting, which comprises the following steps: washing the rock sample with chloroform solvent or alcohol-benzene mixed solution until the rock sample does not contain oil; mixing epoxy resin, a diluent, a curing agent and a dye to obtain a reaction solution; putting the rock sample subjected to the oil washing operation into a vacuum kettle for vacuumizing, then injecting the reaction liquid into the vacuum kettle, and stopping injecting when the liquid level at the upper end of the reaction liquid is more than 10mm higher than the top of the rock sample; injecting die-casting oil into a die-casting cylinder, then putting a rock sample into the die-casting cylinder, pressurizing the rock sample into the die-casting cylinder, and simultaneously injecting the die-casting oil into the die-casting cylinder in the pressurizing process so as to remove gas in the die-casting cylinder until the pressure in the die-casting cylinder reaches a set value; the die-casting preparation method of the rock casting body slice solves the problem that the research of the rock casting body slice prepared by the rock casting body slice in the prior art on the glutenite reservoir with large grain diameter and strong heterogeneity is inaccurate.
Description
Technical Field
The invention relates to the field of geological survey, in particular to a method for preparing a rock casting body slice through die casting.
Background
The rock casting sheet is a method for researching the size distribution of real pores in rock, but the existing casting sheet ground by a rock sample with the diameter of 25mm and 38mm has poor representativeness when researching a glutenite reservoir with large particle size and strong heterogeneity, can not accurately reflect the real pore type and pore throat structural characteristics of the reservoir, and causes larger error of judgment result.
Disclosure of Invention
The invention mainly aims to provide a die-casting preparation method of a rock casting slice, and aims to solve the problem that the rock casting slice prepared from the rock casting slice in the prior art is inaccurate in research on conglomerate reservoirs with large particle size and strong heterogeneity.
In order to achieve the above object, according to one aspect of the present invention, there is provided a method for preparing a rock cast body slice by die casting, comprising: s1: washing the rock sample with chloroform solvent or alcohol-benzene mixed solution until the rock sample does not contain oil; s2: mixing epoxy resin, a diluent, a curing agent and a dye to obtain a reaction solution; s3: putting the rock sample subjected to the oil washing operation into a vacuum kettle, vacuumizing, then injecting the reaction liquid into the vacuum kettle, stopping injecting when the liquid level at the upper end of the reaction liquid is more than 10mm higher than the top of the rock sample, and vacuumizing again until the reaction liquid does not bubble; s4: injecting die-casting oil into a die-casting cylinder, then putting a rock sample into the die-casting cylinder, pressurizing the rock sample into the die-casting cylinder, and simultaneously injecting the die-casting oil into the die-casting cylinder in the pressurizing process so as to remove gas in the die-casting cylinder until the pressure in the die-casting cylinder reaches a set value; s5: heating the temperature in the die casting cylinder to 100-200 ℃, and keeping the temperature above 100 ℃ in a first preset time period; s6: and stopping heating the die-casting cylinder, naturally cooling the rock sample to room temperature in the die-casting cylinder, and taking out the sample.
Further, S1 includes: s11: after oil washing is carried out on the rock sample, the rock sample is put into an ultrasonic cleaner and cleaned by water; s12: and drying the cleaned sample.
Further, S1 further includes: s13: and numbering the cut rock samples, sequentially placing the rock samples into a container after numbering, and isolating the rock samples by using mica sheets.
Further, in preparing the reaction liquid, the epoxy resin, the diluent, the curing agent, and the dye, which are prepared in a predetermined ratio, are mixed at a temperature of 50 to 90 ℃ to sufficiently dissolve the epoxy resin.
Further, the predetermined ratio is: the epoxy resin, the diluent and the curing agent are prepared according to the weight ratio of 10:1:1.2, and the dye comprises oil-soluble blue and oil-soluble green.
Further, the predetermined ratio is: the epoxy resin, the diluent and the curing agent are prepared according to the weight ratio of 10:0.8:1, and the dye comprises phthalocyanine green color paste.
Further, in S4, cottonseed oil is used as the die casting oil.
Further, S5 includes: s51: the temperature is heated to 100 ℃ in a first predetermined period of time, then kept constant at 100 ℃ for 1 hour, and then heated to 160 ℃ in a second predetermined period of time and kept constant at 160 ℃ for 4 hours.
Further, the preparation method of the rock casting body slice by die casting also comprises the following steps: s7: cutting the sample processed by the S6, and enabling the thickness of the cut sample to be not less than 2 times of the thickness of the sample; s8: and grinding the cut sample of S7 until the thickness of the sample reaches a preset value.
Further, the sample processed by the S6 is cut into a plurality of square blocks, the square blocks are polished, and the square blocks are placed into an acid solution to be dissolved after polishing, so that rocks on the surfaces of the square blocks are dissolved, and epoxy resin is exposed.
The method for preparing the rock casting slice by die casting comprises a sample preparation step S1, a reaction liquid preparation step S2, a vacuum infusion step S3, a pressure infusion step S4, a temperature rise step S5 and a sample separation step, wherein in addition, after the rock sample is taken out, the rock sample is ground to obtain the full-diameter rock casting slice.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 shows a schematic flow diagram of a method for the die-casting preparation of a thin sheet of rock casing according to the invention; and
fig. 2 shows a schematic view of an embodiment of the method of the invention for the die-casting preparation of a thin sheet of rock casing.
Wherein the figures include the following reference numerals:
11. a vacuum pump; 12. die casting a cylinder; 13. an electric pump; 14. a liquid storage tank; 15. a temperature control instrument; 16. a vacuum kettle; 17. a drying oven; 21. a first on-off valve; 22. a second on-off valve; 23. a third on-off valve; 24. a fourth switching valve; 25. a fifth on-off valve; 26. a sixth switching valve; 27. and a seventh on-off valve.
Detailed Description
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings.
The invention provides a method for preparing a rock casting body slice by die-casting, and please refer to fig. 1 and fig. 2, which comprises the following steps: s1: washing the rock sample with chloroform solvent or alcohol-benzene mixed solution until the rock sample does not contain oil; s2: mixing epoxy resin, a diluent, a curing agent and a dye to obtain a reaction solution; s3: putting the rock sample subjected to the oil washing operation into a vacuum kettle, vacuumizing, then injecting the reaction liquid into the vacuum kettle, stopping injecting when the liquid level at the upper end of the reaction liquid is more than 10mm higher than the top of the rock sample, and vacuumizing again until the reaction liquid does not bubble; s4: injecting die-casting oil into a die-casting cylinder, then putting a rock sample into the die-casting cylinder, pressurizing the rock sample into the die-casting cylinder, and simultaneously injecting the die-casting oil into the die-casting cylinder in the pressurizing process so as to remove gas in the die-casting cylinder until the pressure in the die-casting cylinder reaches a set value; s5: heating the temperature in the die casting cylinder to 100-200 ℃, and keeping the temperature above 100 ℃ in a first preset time period; s6: and stopping heating the die-casting cylinder, naturally cooling the rock sample to room temperature in the die-casting cylinder, and taking out the sample.
The invention develops a novel die-casting preparation method of a rock casting body slice, which comprises a sample preparation step S1, a reaction liquid preparation step S2, a vacuum infusion step S3, a pressure infusion step S4, a temperature rise step S5 and a sample separation step, wherein after the rock sample is taken out, the rock sample is ground to obtain a full-diameter rock casting body slice.
S1 includes: s11: after oil washing is carried out on the rock sample, the rock sample is put into an ultrasonic cleaner and cleaned by water; s12: and drying the cleaned sample.
The preparation method of the cast rock slice comprises selecting representative part of rock, cutting to obtain the rock sample, and washing oil in oil washing equipment until the rock sample contains no oil, wherein chloroform solvent or 1: 4 mixed alcohol benzene solution is used. And putting the rock sample subjected to oil washing into an ultrasonic cleaner, and carrying out ultra-washing for about 4 minutes by using water. Then the sample is put in a drying oven 17 for 4 hours, the temperature is controlled between 105 ℃ and 110 ℃, the moisture is dried, and the sample is put in a dryer for standby after natural cooling.
S1 further includes: s13: and numbering the cut rock samples, sequentially placing the rock samples into a container after numbering, and isolating the rock samples by using mica sheets. In the preparation of the reaction solution, epoxy resin, a diluent, a curing agent and a dye, which are prepared in a predetermined ratio, are mixed at a temperature of 50 ℃ to 90 ℃ to sufficiently dissolve the epoxy resin.
And sequentially placing the numbered samples into a container in sequence, and making a sample loading record in time, wherein each sample is isolated by a mica sheet, so that the sample loading is stopped at a position 3cm away from the container opening in order to separate the samples later.
Preferably, the rock samples are cut into blocks of 18X 6mm or 24X 6mm, or alternatively, they may be drilled with a 2.5cm diameter core drill and cut into about 6mm rock samples with a slicer, with full diameter core production requiring samples of 100mm in diameter. And numbered with drawing ink or red and blue pencils.
Adding the reaction solution, and fully and uniformly stirring; the whole preparation process is carried out in a constant temperature water bath at 70 ℃ to obtain fully dissolved dyeing resin.
According to one embodiment of the invention, the predetermined ratio of the reaction liquid is: the epoxy resin, the diluent and the curing agent are prepared according to the weight ratio of 10:1:1.2, and the dye comprises oil-soluble blue and oil-soluble green.
According to another embodiment of the present invention, the predetermined ratio of the reaction liquid is: the epoxy resin, the diluent and the curing agent are prepared according to the weight ratio of 10:0.8:1, and the dye comprises phthalocyanine green color paste.
Preferably, the preparation method comprises the steps of weighing a certain amount of 8828 epoxy resin on a balance by using a beaker, weighing the diluent 501 in proportion, fully and uniformly stirring by using a glass rod, weighing the curing agent 594 in proportion, fully and uniformly stirring by using the glass rod, adding the dye in proportion to fully and uniformly stir, and carrying out the whole preparation process in a constant-temperature water bath kettle at 70 ℃ to obtain fully dissolved dyeing resin.
In S4, cottonseed oil is used as the die casting oil.
S5 includes: s51: the temperature is heated to 100 ℃ in a first predetermined period of time, then kept constant at 100 ℃ for 1 hour, and then heated to 160 ℃ in a second predetermined period of time and kept constant at 160 ℃ for 4 hours.
The vessel heating switch is turned on and the thermostat 15 is set to 100 c for a first predetermined period of time, and when 100 c, thermostating commences. After keeping the temperature for 1 hour, entering a second preset time period, setting the temperature controller to 160 ℃, and starting to keep the temperature when the temperature is 160 ℃. Keeping the temperature for 4 hours, turning off the power supply and returning the pump to zero. And after natural cooling, opening the end socket and taking out the sample tube.
When the temperature rises, high back pressure is generated, the pressure needs to be reduced at any time, and when the epoxy resin is polymerized, the pressure is continuously reduced, and at the moment, the pressure needs to be continuously supplemented. The upper limit and the lower limit of the control pressure are set by the electric pump, and the electric pump can automatically increase and reduce the pressure.
The preparation method of the rock casting body slice by die casting further comprises the following steps: s7: cutting the sample processed by the S6, and enabling the thickness of the cut sample to be not less than 2 times of the thickness of the sample; s8: and grinding the cut sample of S7 until the thickness of the sample reaches a preset value.
And cutting the sample processed by the S6 into a plurality of square blocks, polishing the square blocks, and putting the square blocks into an acid solution for dissolving after polishing so as to dissolve rocks on the surfaces of the square blocks and expose the epoxy resin.
After the pressurized perfusion sample is peeled off by a small hammer, the sample is separated by a knife according to the sample loading sequence and is placed at a label for grinding or acid etching.
The abraded cast body slice in fig. 1 is an abraded rock cast body slice, and the acid etching of the cast body sample is to perform acid etching on the rock sample.
From the above description, it can be seen that the above-described embodiments of the present invention achieve the following technical effects:
in the step S4, the second on-off valve 22 is opened, the container containing the sample is placed in the vacuum vessel 16 and sealed, the prepared reaction solution is poured into the medicine bottle, and the medicine bottle is placed in the water bath and heated to about 70 ℃.
Connecting a medicine bottle with a valve on a vacuum kettle 16, opening a switch of a vacuum pump 11, vacuumizing, when the difference between the vacuum in the system and the atmospheric pressure in the system is 400pa, evacuating for 1h to 4h according to different lithologies, if the difference cannot be reached, the difference cannot be found by 2mm pump columns at most, otherwise, carefully checking the sealing reason of the process, eliminating the fault, then injecting the dye in the medicine bottle into the sample tube, submerging the sample for more than 10mm, completely filling, continuing evacuating for 15min to 30min, taking out the sample tube for 15min to 30min without bubbling, stopping the pump, opening the valve on the vacuum kettle, connecting the atmosphere, opening the vacuum kettle, heating, taking out the sample tube, and pressurizing and filling.
After the work is finished, the container must be completely dipped and dyed, so that the container is prevented from being bonded on a full-diameter vacuum kettle during heating and curing.
Immediately after the vacuum pump is turned off, the seventh switching valve 27 is opened to turn on the vacuum pump 11 to the atmosphere.
During the operations of pressure infusion and heating solidification:
1. the sample after vacuum infusion in the vacuum kettle is put into a full-diameter die-casting cylinder, the action is slow and accurate during the putting, air is prevented from being pressed into die-casting oil as much as possible, and the dip dyeing agent liquid is prevented from overflowing to any part of the full-diameter die-casting cylinder so as to avoid bonding.
2. And opening a third switch valve 23 and a fourth switch valve 24, opening a vacuum pump to evacuate the full-diameter die-casting cylinder 12, opening a fifth switch valve 25 to suck oil when the pressure in the die-casting cylinder 12 reaches-0.098 Mpa, closing the third switch valve 23 and the fourth switch valve 24 to continuously suck oil, then closing the vacuum pump, and opening a seventh switch valve 27 to enable the vacuum pump to be connected with the atmosphere.
3. Operation of the electric pump: the pressure parameters of the pump are set as follows: RL 1-20 MPa, RL 2-24 MPa, RH 1-1 MPa,
RH2 is 1MPa, when the pump is pumped and pressurized, the pump is automatically stopped when the pump pressure is increased to RL1+ RH1 is 21 MPa;
when the pump pressure is reduced by RL1 to 20MPa, the pump is automatically fed; when the pump pressure is increased to RL2 ═ 24MPa for external reasons, the pump is automatically withdrawn; when the pump is withdrawn, the pressure is reduced, and when the pump pressure is reduced to RL 2-RH 2 which is 23MPa, the pump is automatically stopped; and during liquid suction, opening a valve on the water storage tank, and closing a sixth switch valve 26 from the electric pump to the die-casting cylinder reaction kettle. During liquid drainage, the valve on the liquid storage tank 14 is closed, and the sixth switch valve 26 for pumping the liquid to the reaction kettle is opened.
The vacuum pump in this application is mainly used to evacuate the core in the core holder, so that the resin can smoothly enter the fine pore canal of the pore.
Container and core holder in this application: the main function is to put the filled sample holding tube into the core chamber to pressurize and heat. The viscosity of the injection agent is firstly reduced at a certain temperature, the injection agent is pressed into the micropore channel of the rock core under the high pressure condition, then a certain temperature is added to polymerize and solidify the injection agent, and the whole system takes a tee joint and a cross joint as the center.
The rock casting body slice die-casting preparation method further comprises an electrical control system, and the electrical control system is mainly used for controlling the service time of the instrument, controlling the vacuum pump and the oil pump, performing overpressure power-off and alarm, heating a circuit, measuring the vacuum degree, the pressure, the temperature and the like.
The working pressure of the instrument is high, all high-pressure pipelines must be filled with oil, and a large amount of gas cannot be mixed in, so that before use, gas in the pipelines is discharged through low-pressure oil pumping, and then the pipelines are completely filled with oil through an oil tank valve. The vacuum system is kept clean without affecting the vacuum level.
The application comprises the following steps: and (3) placing the test tube filled with the sample into a vacuum drying oven, sealing, pouring the prepared reaction liquid into a medicine bottle, placing the medicine bottle into a water bath kettle, and heating to about 70 ℃ to enable the medicine bottle to flow easily. And (4) connecting the vacuum drying box and the medicine bottle with a vacuum pump, opening a vacuum pump switch, vacuumizing, and vacuumizing for 15-30 min after the atmospheric pressure of the current day is reached. If the pressure does not reach the preset pressure, the pump column can not be 2mm at most, otherwise, the sealing reason of the process is carefully checked, the fault is eliminated, then the dye in the medicine bottle is injected into the sample tube, the sample is submerged for more than 10mm, the filling is finished, the evacuation is continued for 15min to 30min, the pump is stopped until no bubbles are generated, the three-way plug valve is rotated to connect the atmosphere, and the vacuum drier is opened to take out the sample tube for pressurization and heating filling.
The pressurized infusion and elevated temperature curing of the present application includes:
(1) injecting cottonseed oil: the pressurizing and heating medium cottonseed oil is slowly injected into the full-diameter die casting cylinder, so that the oil level just reaches the sealing surface.
(2) Placing a rock sample: and (3) putting the sample subjected to vacuum infusion into the full-diameter die-casting cylinder, wherein the action is slow and accurate during the placing, air is prevented from being pressed into oil liquid to the greatest extent, and the dip dyeing liquid is prevented from overflowing to any part of the full-diameter die-casting cylinder so as not to be bonded.
(3) Pressurizing: opening a valve on the sealing head of the full-diameter die-casting cylinder, covering the sealing head on the full-diameter die-casting cylinder, screwing a nut, discharging air from a valve opening, opening a pressure pump, supplementing cottonseed oil into the full-diameter die-casting cylinder, discharging air, closing the valve when the cottonseed oil is discharged from the valve outlet, and increasing the pressure. The upper limit of the pressure value is controlled by an electrode point pressure gauge, and the pump automatically stops when the pressure is needed.
(4) And (3) heating: the temperature controller is set to 100 ℃, the container heating switch is turned on, and the constant temperature is started when the temperature reaches 100 ℃. The time is recorded, after keeping the temperature for 1 hour, the temperature controller is set to 160 ℃, and the temperature is kept at 160 ℃. Recording time, keeping the temperature for 4 hours, turning off the power supply at the time, and returning the pump to zero. And naturally cooling overnight, opening the end socket, and taking out the sample tube.
(5) Heating and maintaining: the data show that the sample is kept at 100 ℃ for 1 hour in a full diameter die casting cylinder, the core is pressed into the epoxy resin as far as possible at the lowest viscosity, the temperature is 145 ℃ to 160 ℃, the red light is on (indicating continuous temperature rise), and the temperature is kept for 4 hours at 160 ℃ when the yellow light is on, so that the epoxy resin is polymerized and cured. The actual operation is as follows: the power switch is turned on and the voltage regulator is rotated to a voltage of 220V. Adjusting the temperature controller to 100 ℃, wherein a red light (warming light) is on to indicate that the warming is started; when a yellow lamp (constant temperature lamp) is on, the constant temperature of 100 ℃ is started; recording time, keeping the temperature for 1 hour, adjusting the temperature controller to 160 ℃, then, turning on a red light (indicating that the temperature is continuously heated), and when a yellow light is turned on, indicating that the constant temperature of 160 ℃ is started, recording time; keeping the temperature for 4 hours, turning off the power supply at the moment, and returning the pump to zero. After natural cooling overnight, the pressure tank is opened and the sample tube is taken out. Inverted in a beaker and the cottonseed oil was drained.
Grinding and scanning a rock casting sheet:
(1) grinding a rock casting sheet: the method is basically the same as grinding common rock slices. Because the pores are filled with the epoxy resin to play a role in solidifying the specimen, loose rock samples are not required to be boiled and processed, coarse, fine and fine grinding can be directly carried out on a sheet grinding machine, and the impregnating agents except the rock samples are cut or ground off optimally, and because the impregnating agents are easy to generate bubbles when adhering the sheets and are easy to generate degumming phenomenon during grinding. The clay sheets and subsequent coarse, fine, and thickness standards are the same as for conventional rock sheets.
(2) The diameter of the die casting cylinder is 140mm to 150mm, the pressure bearing range is 0 to 15Mpa, and the number of conventional samples for single die casting is about 3 times of the original number;
(3) slides of specification 145mm 140mm 1.2mm were made and full diameter cores were ground to 0.03mm thick cast sheets.
(4) Sticking, slicing, grinding and covering:
cutting the substrate to a thickness of about 5mm by using a cutting machine with higher precision after adhering the substrate by using 502, grinding the substrate to a thickness of 0.03mm by using a post grinding machine, and covering the substrate by using a liquid crystal display screen with 110mm by 110 mm.
Grinding the substrate by directly grinding the substrate on a grinding disc after adhering the substrate 502 for about one week, and protecting the substrate by using a 110mm liquid crystal screen to cover the substrate when the thickness reaches 0.03 mm.
Grinding a full-diameter core of about 5mm in thickness to 0.03mm takes three days, and for the currently advantageous method, a special slicer is used to cut the sample to 2mm and then the sample is ground with the slicer.
Scanning the rock casting slice: cutting the poured rock sample into blocks of 11X 3mm, performing coarse and fine grinding on a sheet grinding machine and coarse and fine grinding on a glass plate, and performing acid dissolution on the ground sample. The lithology is different, the acid is different, and 5% hydrochloric acid is used for carbonate rock; and for sandstone, a reagent prepared by hydrofluoric acid and distilled water according to a volume ratio of 1:1 is used for corrosion, a layer of rock on the surface can be dissolved out, epoxy resin in pores is protruded, acidified residues are cleaned by distilled water, and a photo reflecting the pores and the throat can be shot under an electron microscope after film coating.
The preparation method suitable for the full-diameter rock casting body slice is established, and the problem that the actual state of the reservoir cannot be accurately reflected by the pore type and the pore throat structural characteristics when the casting body slice is analyzed in conglomerate reservoir evaluation is solved, so that the reservoir evaluation structure is more real and reliable.
1. During vacuum infusion, the difference between the reading on the vacuum meter and the atmospheric pressure of the current day is less than 2mm of mercury and meets the standard;
2. the pressure is not lower than 280kg/cm2 when the pressure is used for pressure infusion, so that the resin can be ensured to be infused into the rock pores;
3. the cured resin is hard and free of bubbles and cracks in rock samples.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments according to the present application. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
The relative arrangement of the components and steps, the numerical expressions and numerical values set forth in these embodiments do not limit the scope of the present invention unless specifically stated otherwise. Meanwhile, it should be understood that the sizes of the respective portions shown in the drawings are not drawn in an actual proportional relationship for the convenience of description. Techniques, methods, and apparatus known to those of ordinary skill in the relevant art may not be discussed in detail but are intended to be part of the specification where appropriate. In all examples shown and discussed herein, any particular value should be construed as merely illustrative, and not limiting. Thus, other examples of the exemplary embodiments may have different values. It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, further discussion thereof is not required in subsequent figures.
In the description of the present invention, it is to be understood that the orientation or positional relationship indicated by the orientation words such as "front, rear, upper, lower, left, right", "lateral, vertical, horizontal" and "top, bottom", etc. are usually based on the orientation or positional relationship shown in the drawings, and are only for convenience of description and simplicity of description, and in the case of not making a reverse description, these orientation words do not indicate and imply that the device or element being referred to must have a specific orientation or be constructed and operated in a specific orientation, and therefore, should not be considered as limiting the scope of the present invention; the terms "inner and outer" refer to the inner and outer relative to the profile of the respective component itself.
Spatially relative terms, such as "above … …," "above … …," "above … …," "above," and the like, may be used herein for ease of description to describe one device or feature's spatial relationship to another device or feature as illustrated in the figures. It will be understood that the spatially relative terms are intended to encompass different orientations of the device in use or operation in addition to the orientation depicted in the figures. For example, if a device in the figures is turned over, devices described as "above" or "on" other devices or configurations would then be oriented "below" or "under" the other devices or configurations. Thus, the exemplary term "above … …" can include both an orientation of "above … …" and "below … …". The device may be otherwise variously oriented (rotated 90 degrees or at other orientations) and the spatially relative descriptors used herein interpreted accordingly.
It should be noted that the terms "first", "second", and the like are used to define the components, and are only used for convenience of distinguishing the corresponding components, and the terms have no special meanings unless otherwise stated, and therefore, the scope of the present invention should not be construed as being limited.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for preparing a rock casting body slice by die casting is characterized by comprising the following steps:
s1: washing oil on the rock sample by adopting a chloroform solvent or an alcohol benzene mixed solution until the rock sample does not contain oil;
s2: mixing epoxy resin, a diluent, a curing agent and a dye to obtain a reaction solution;
s3: putting the rock sample subjected to oil washing operation into a vacuum kettle, vacuumizing, then injecting the reaction liquid into the vacuum kettle, stopping injecting when the liquid level at the upper end of the reaction liquid is more than 10mm higher than the top of the rock sample, and vacuumizing again until the reaction liquid does not bubble;
s4: injecting die-casting oil into a die-casting cylinder, then putting the rock sample into the die-casting cylinder, pressurizing the rock sample into the die-casting cylinder, and injecting the die-casting oil into the die-casting cylinder during the pressurizing process so as to remove gas in the die-casting cylinder until the pressure in the die-casting cylinder reaches a set value;
s5: heating the temperature in the die casting cylinder to 100-200 ℃, and keeping the temperature above 100 ℃ in a first preset time period;
s6: and stopping heating the die-casting cylinder, naturally cooling the rock sample to room temperature in the die-casting cylinder, and taking out the sample.
2. The method for die-casting a rock casting sheet according to claim 1, wherein S1 includes:
s11: after the oil washing is carried out on the rock sample, the rock sample is put into an ultrasonic cleaner and cleaned by water;
s12: and drying the cleaned sample.
3. The method for die-casting a rock casting sheet according to claim 2, wherein the step S1 further comprises:
s13: numbering the cut rock samples, sequentially placing the rock samples into a container after numbering, and isolating the rock samples by mica sheets.
4. The die-casting preparation method of a rock casting sheet according to claim 1, wherein the epoxy resin, the diluent, the curing agent and the dye are mixed at a temperature of 50 ℃ to 90 ℃ in a predetermined ratio to sufficiently dissolve the epoxy resin when the reaction liquid is prepared.
5. A method for the die-casting preparation of a rock casting sheet according to claim 4, wherein the predetermined ratio is: the epoxy resin, the diluent and the curing agent are prepared according to the weight ratio of 10:1:1.2, and the dye comprises oil-soluble blue and oil-soluble green.
6. A method for the die-casting preparation of a rock casting sheet according to claim 4, wherein the predetermined ratio is: the epoxy resin, the diluent and the curing agent are prepared according to the weight ratio of 10:0.8:1, and the dye comprises phthalocyanine green color paste.
7. The method for die casting a cast rock body flake according to claim 1, wherein in S4, cottonseed oil is used as the die casting oil.
8. The method for die-casting a rock casting sheet according to claim 1, wherein S5 includes:
s51: heating to 100 ℃ in the first preset time period, keeping the temperature of 100 ℃ constant for 1 hour, heating to 160 ℃ in the second preset time period, and keeping the temperature constant at 160 ℃ for 4 hours.
9. The method of die casting rock casing slice as claimed in claim 1, further comprising:
s7: cutting the sample processed by the S6, wherein the thickness of the cut sample is not less than 2 times of the thickness of the sample;
s8: and grinding the sample cut by the S7 until the thickness of the sample reaches a preset value.
10. The die-casting preparation method of the rock casting sheet as claimed in claim 1, wherein the sample treated in S6 is cut into a plurality of square blocks, the square blocks are polished, and after polishing, the square blocks are put into an acid solution to be dissolved so as to dissolve the rocks on the surfaces of the square blocks and expose the epoxy resin.
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Cited By (1)
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| CN115184118A (en) * | 2022-08-15 | 2022-10-14 | 西南石油大学 | Preparation method and preparation system of slice rock sample and core imbibition mechanism research method |
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