CN118362464A - Gas-liquid synergistic imbibition experimental device and experimental method under shale reservoir condition - Google Patents
Gas-liquid synergistic imbibition experimental device and experimental method under shale reservoir condition Download PDFInfo
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- 238000005213 imbibition Methods 0.000 title claims abstract description 46
- 238000002474 experimental method Methods 0.000 title claims abstract description 16
- 230000002195 synergetic effect Effects 0.000 title claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 134
- 238000012360 testing method Methods 0.000 claims abstract description 83
- 239000003921 oil Substances 0.000 claims abstract description 52
- 238000000034 method Methods 0.000 claims abstract description 40
- 239000010779 crude oil Substances 0.000 claims abstract description 39
- 239000004094 surface-active agent Substances 0.000 claims abstract description 36
- 238000005481 NMR spectroscopy Methods 0.000 claims abstract description 33
- 238000001069 Raman spectroscopy Methods 0.000 claims abstract description 33
- 238000002347 injection Methods 0.000 claims abstract description 33
- 239000007924 injection Substances 0.000 claims abstract description 33
- 238000001237 Raman spectrum Methods 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000012544 monitoring process Methods 0.000 claims abstract description 20
- 239000011435 rock Substances 0.000 claims abstract description 16
- 238000005259 measurement Methods 0.000 claims abstract description 15
- 238000001228 spectrum Methods 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 238000006073 displacement reaction Methods 0.000 claims description 28
- 238000003860 storage Methods 0.000 claims description 26
- 239000011148 porous material Substances 0.000 claims description 16
- 238000007599 discharging Methods 0.000 claims description 13
- 238000011084 recovery Methods 0.000 claims description 9
- 238000004458 analytical method Methods 0.000 claims description 7
- 238000004364 calculation method Methods 0.000 claims description 7
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- 238000010521 absorption reaction Methods 0.000 claims 1
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- G01N13/00—Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
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- G01N21/65—Raman scattering
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- G01N5/025—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by absorbing or adsorbing components of a material and determining change of weight of the adsorbent, e.g. determining moisture content for determining moisture content
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Abstract
The invention provides a gas-liquid synergistic imbibition experimental device and an experimental method thereof under the condition of a shale reservoir, wherein the experimental device comprises a reaction kettle, a nuclear magnetic resonance instrument can detect a nuclear magnetic spectrum in the reaction kettle, the reaction kettle is arranged in a heating cavity of a hot oil furnace, a liquid supply unit and a liquid injection unit are mutually communicated with the inner side of the reaction kettle, the liquid supply unit can supply gas and crude oil in the reaction kettle or vacuumize the reaction kettle, the liquid injection unit can supply a surfactant in the reaction kettle, a rock core can be placed in the reaction kettle, a Raman test unit can carry out Raman spectrum measurement on the rock core in the reaction kettle, a conductivity test unit can carry out water content measurement on the rock core in the reaction kettle, and the nuclear magnetic resonance instrument, the Raman test unit and the conductivity test unit are in signal connection with a data monitoring unit. The invention has the characteristics of accurate measurement, comprehensive simulation development process, repeatability, various simulation conditions, simple instrument, simple operation and the like.
Description
Technical Field
The invention relates to the technical field of oil and gas exploitation, in particular to a gas-liquid collaborative imbibition experimental device and method under the condition of a shale reservoir.
Background
In recent years, the status of unconventional oil reservoirs with difficult reserves such as shale oil and the like in the oil and gas resource exploration and development field in China is more and more important. However, due to the characteristics of ultralow permeability and low porosity, the oil reservoirs have high exploitation difficulty and low recovery ratio. Research shows that imbibition is an important mechanism for improving the extraction degree of crude oil in a tight oil reservoir, and imbibition mediums comprise fracturing fluid, gas, surfactant solution and the like. In the development process of unconventional oil reservoirs such as shale oil, a high-speed seepage channel is provided by injecting fracturing fluid into a fracturing stratum; the energy of stratum is supplemented by injecting CO 2 and other gases, and crude oil is replaced and reduced in viscosity by utilizing the extraction and dissolution effects; and the crude oil in the micro-nano pores is subjected to imbibition displacement by injecting a surfactant, so that the yield and recovery ratio of the crude oil are improved. Therefore, quantitative characterization of the synergistic imbibition extraction effect of the injected gas and the surfactant in the unconventional oil reservoir exploitation process has great significance on the unconventional shale oil reservoir exploitation effect.
The Chinese patent CN115992700A proposes an experimental device and a method for simulating the pressure-stewing-discharging-collecting of a low-permeability compact oil reservoir, which simulate the dynamic imbibition displacement process of water and oil after fracturing the low-permeability compact oil reservoir, and the distribution condition and the effect of the imbibition displacement of the oil and the water under different conditions can be obtained by collecting discharged liquid, but an experimental instrument can only relate to the simulation of the displacement imbibition process, the early gas extraction process cannot be considered, and the error of the method for metering the imbibition quantity by means of oil-water separation is larger.
Chinese patent CN115901573a provides a core seepage and suction device, a experimental device for simulating crack fluid pressure seepage and suction and an experimental method, which can simulate the real condition of a reservoir to simulate the seepage and suction and reverse discharge processes, but has the advantages of more instruments, complex operation and incapability of simulating the gas injection process.
Chinese patent CN113820249a discloses a device and a method for evaluating wettability of a sediment based on imbibition nuclear magnetic resonance, which uses an online nuclear magnetic technique to characterize occurrence and migration rules of fracturing fluid in a rock core and wettability evaluation under various pressure and temperature conditions, and the invention can perform dynamic test of a rock core T2 map by using the online nuclear magnetic technique, but does not consider simulation of synergistic effect of gas and the fracturing fluid.
The following problems exist in summary of the prior art means:
(1) The common metering method comprises a imbibition bottle volume imbibition method and a balance weighing method, so that imbibition results can be visually seen, the law of fluid movement in a rock core cannot be analyzed, and the high-temperature and high-pressure conditions of an underground real fracturing and stewing well cannot be simulated; another common method is nuclear magnetic resonance T2 mapping, in which the core undergoes a process from high pressure to normal pressure in the test process, and a large error exists;
(2) The numerical simulation method can study the influence of injection gas types, injection methods, injection rounds, injection speed, temperature, pressure, surfactant properties and the like on extraction degree, the mathematical model of the method is built based on idealized conditions, and the built core model is simple and cannot replace actual core structural characteristics;
(3) In the imbibition process, the content and type of organic matters in the core, the mineral components in the core, the crystal structure of the core and the water content of the core have important influences on occurrence and migration of shale oil and physical and chemical properties of the core, and the existing test method cannot monitor the change of physical parameters of the core in the imbibition process.
Disclosure of Invention
In view of the above, the invention provides a gas-liquid collaborative imbibition experimental device and an experimental method under the condition of a shale reservoir, which are used for researching the core extraction degree in the gas injection combined liquid injection extraction process and an indoor simulation model of the crude oil utilization rules and characteristics of pores of various sizes in a core.
The technical scheme of the invention is realized as follows: the invention provides a gas-liquid collaborative imbibition experimental device under shale reservoir conditions, which comprises: the nuclear magnetic resonance device comprises a reaction kettle, a hot oil furnace, a liquid supply unit, a liquid injection unit, a nuclear magnetic resonance instrument and a data monitoring unit, wherein the nuclear magnetic resonance instrument can detect nuclear magnetic patterns in the reaction kettle, the reaction kettle is arranged in a heating cavity of the hot oil furnace, the liquid supply unit and the liquid injection unit are communicated with the inner side of the reaction kettle, the liquid supply unit can provide gas and crude oil in the reaction kettle or vacuumize the reaction kettle, the liquid injection unit can provide a surfactant in the reaction kettle, a rock core can be placed in the reaction kettle, and the nuclear magnetic resonance instrument is in signal connection with the data monitoring unit.
In some embodiments, the device further comprises a raman test unit, the test end of the raman test unit is communicated with the inner side of the reaction kettle, the raman test unit can perform raman spectrum measurement on the core in the reaction kettle, and the raman test unit is in signal connection with the data monitoring unit.
In some embodiments, the device further comprises a conductivity testing unit, wherein a testing end of the conductivity testing unit is communicated with the inner side of the reaction kettle, the conductivity testing unit can measure the water content of the core in the reaction kettle, and the conductivity testing unit is in signal connection with the data monitoring unit.
In some embodiments, the liquid supply unit comprises a gas storage intermediate container, a displacement pump and a vacuum pump, wherein an outlet of the gas storage intermediate container is communicated with the top opening of the reaction kettle, an outlet of the displacement pump is selectively communicated with an inlet of the gas storage intermediate container and an inlet of the gas storage intermediate container respectively through a multi-way valve, and the vacuum pump is communicated with the top opening of the reaction kettle.
In some embodiments, the liquid injection unit comprises a surfactant intermediate container, an outlet of which is in communication with the reaction vessel top opening, and an outlet of the displacement pump is selectively in communication with an inlet of the surfactant intermediate container through a multi-way valve.
In a second aspect, the present invention also provides an experimental method based on the experimental apparatus, the experimental method comprising the following steps:
Step one, placing a core into a reaction kettle, vacuumizing the reaction kettle through a liquid supply unit, respectively measuring the water content of the core and the Raman spectrum by using a conductivity test unit and a Raman test unit, and recording data;
Step two, injecting crude oil into the reaction kettle through a liquid supply unit, pressurizing and saturating the oil;
Step three, discharging crude oil in the reaction kettle, after cleaning, measuring the Raman spectrum of the core by using a Raman test unit, and recording data;
Step four, starting a hot oil furnace to heat the reaction kettle, introducing gas into the reaction kettle by a liquid supply unit, pressurizing, discharging the gas for pressure relief after a certain time is kept, performing nuclear magnetic T2 spectrum test on the reaction kettle by a nuclear magnetic resonance instrument during gas pressurization and pressure relief, simultaneously performing Raman spectrum measurement on the rock core by a Raman test unit, and recording data;
step five, repeating the step four to finish the gas throughput of the target round;
Step six, after the gas throughput is finished, the liquid injection unit injects the surfactant into the reaction kettle, pressurizes the reaction kettle to the formation pressure, the hot oil furnace heats the reaction kettle to the oil reservoir temperature, nuclear magnetic T2 spectrum test is carried out on the reaction kettle through a nuclear magnetic resonance instrument, water content and Raman spectrum measurement are respectively carried out on the rock core through the conductivity test unit and the Raman test unit, and data are recorded;
and step seven, after the imbibition is finished, discharging the liquid in the reaction kettle, and analyzing data.
In a third aspect, the present invention also provides another experimental method based on the experimental apparatus, which includes the following steps:
Step one, placing a core into a reaction kettle, vacuumizing the reaction kettle through a liquid supply unit, respectively measuring the water content of the core and the Raman spectrum by using a conductivity test unit and a Raman test unit, and recording data;
Step two, injecting crude oil into the reaction kettle through a liquid supply unit, pressurizing and saturating the oil;
Step three, discharging crude oil in the reaction kettle, after cleaning, measuring the Raman spectrum of the core by using a Raman test unit, and recording data;
Step four, starting a hot oil furnace to heat the reaction kettle, introducing gas into the reaction kettle by a liquid supply unit, maintaining a certain pressure, continuously replacing core crude oil in the reaction kettle by the gas provided by the liquid supply unit, performing nuclear magnetic T2 spectrum test on the reaction kettle by a nuclear magnetic resonance instrument at different replacement moments, performing Raman spectrum measurement on the core by a Raman test unit, and recording data;
Step five, after the gas replacement is finished, the liquid injection unit injects the surfactant into the reaction kettle, pressurizes the reaction kettle to a set pressure to carry out surfactant imbibition, carries out nuclear magnetic T2 spectrum test on the reaction kettle at different moments of imbibition through a nuclear magnetic resonance instrument, carries out water content and Raman spectrum measurement on the rock core through a conductivity test unit and a Raman test unit respectively, and records data;
and step six, after the imbibition is finished, discharging the liquid in the reaction kettle, and analyzing data.
In the experimental device, the Raman test unit is a Raman scattering spectrometer and comprises a laser, a spectrometer, an incident optical fiber and a receiving optical fiber, wherein the incident end of the incident optical fiber is opposite to the core surface in the reaction kettle, the receiving end of the receiving optical fiber is opposite to the core surface in the reaction kettle, the laser emits laser to enter the core surface through the incident optical fiber, and scattered optical signals enter the spectrometer through the receiving optical fiber.
In the experimental device, the conductivity testing unit is a conductivity meter, and the control end of the conductivity meter is electrically connected with the surface of the core in the reaction kettle through a lead.
In the experimental device, the nuclear magnetic resonance apparatus is an online nuclear magnetic resonance apparatus.
In some embodiments, the analysis data includes calculating the extent of extraction of crude oil from the core at different times by:
Wherein: r 1 -imbibition recovery ratio,%; a 1, the area surrounded by the residual crude oil T2 nuclear magnetic curve and the X axis is dimensionless; a 2, the area surrounded by the original saturated oil T2 nuclear magnetic curve and the X axis, is dimensionless.
In some embodiments, the analysis data includes calculation of the extent of pore crude oil usage of different sizes by:
As the relaxation time in the nuclear magnetism T2 map is larger, the corresponding pore size is represented to be larger, the shale relaxation time can be utilized for pore type division, which is respectively micropore (T2 relaxation time is less than 0.1 ms), small pore (0.1 ms is less than T2 relaxation time is less than 1 ms), mesopore (1 ms is less than T2 relaxation time is less than 10 ms) and large pore (T2 relaxation time is more than 10 ms), the pore utilization degree of each size is respectively calculated, and the calculation method comprises the following steps:
Wherein: i-different pore types, including microporous, small, medium, large, dimensionless; r i -i type pore imbibition recovery,%; a i1 -the area surrounded by the residual crude oil T2 nuclear magnetic curve of the i-type pore and the X axis is dimensionless; a i2, the area surrounded by the original saturated oil T2 nuclear magnetic curve and the X axis, is dimensionless.
In some embodiments, in the two methods, the analyzing the data includes calculating the water content in the core at different times, and the calculating method is as follows:
After the experiment is finished, drying and weighing the core, soaking the core in a surfactant at different moments t i, testing the conductivity sigma i of the core by using a conductivity meter, taking out the core to wipe the surface and testing the mass m i, and calculating the water content W i of the core at moment t i by using a mass method, wherein the calculation method comprises the following steps:
Wherein: mass at m i——ti, g; m-dry weight of core, g;
Fitting the relationship between the water content W i and the core conductivity sigma i, and fitting a common linear function can also see other functional relationships:
Wi＝A*σi+B
Wherein: a is a constant, and is obtained by fitting; b-constant, obtained by fitting.
The corresponding conductivity sigma i is obtained by testing at different moments in the high-temperature high-pressure imbibition experiment process, and the corresponding core water content W i can be calculated by utilizing the relation between W i and sigma i.
Compared with the prior art, the experimental device and the experimental method have the following beneficial effects:
The invention can realize the real process simulation of the field reservoir development and evaluate the synergistic imbibition effect of the gas-surfactant. The invention has the characteristics of accurate measurement, comprehensive simulation development process, repeatability, various simulation conditions, simple instrument, simple operation and the like. The simulation of the gas injection extraction and fracturing fluid permeation extraction processes in actual exploitation provides theoretical basis for crude oil extraction of tight reservoirs, low-permeability reservoirs and the like.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of the experimental apparatus of the present invention;
FIG. 2 is a schematic diagram of the experimental apparatus of the present invention;
FIG. 3 is a nuclear magnetic resonance T2 spectrum of the reaction vessel in example 1;
FIG. 4 is a graph showing the degree of extraction in example 1;
FIG. 5 is a graph showing the degree of porosity used for each size in example 1;
FIG. 6 is a Raman spectrum of example 1;
FIG. 7 is a nuclear magnetic resonance T2 spectrum of the reaction vessel of example 2;
FIG. 8 is a graph showing the degree of extraction in example 2;
FIG. 9 is a graph showing the degree of porosity used for each size in example 2;
fig. 10 is a raman spectrum of example 2.
In the figure: 1-reaction kettle, 2-oil heating furnace, 3-liquid supply unit, 4-liquid injection unit, 5-nuclear magnetic resonance instrument, 6-Raman test unit, 7-conductivity test unit, 8-data monitoring unit, 31-gas storage intermediate container, 32-oil storage intermediate container, 33-displacement pump, 34-vacuum pump, 35-multi-way valve and 41-surfactant intermediate container.
Detailed Description
The following description of the embodiments of the present invention will clearly and fully describe the technical aspects of the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the present invention without making any inventive effort, are intended to fall within the scope of the present invention.
It will be understood that when an element is referred to as being "mounted" or "disposed" on another element, it can be directly on the other element or be indirectly on the other element. When an element is referred to as being "connected to" another element, it can be directly connected to the other element or be indirectly connected to the other element.
It is to be understood that the terms "length," "width," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like are merely for convenience in describing and simplifying the description based on the orientation or positional relationship shown in the drawings, and do not indicate or imply that the devices or elements referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus are not to be construed as limiting the application.
Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more such feature. In the description of the present application, the meaning of "a plurality" is two or more, unless explicitly defined otherwise.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which embodiments of the invention belong. If the definitions set forth in this section are contrary to or otherwise inconsistent with the definitions set forth in the patents, patent applications, published patent applications and other publications incorporated herein by reference, the definitions set forth in this section are preferentially set forth in the definitions set forth herein.
The methods used in the examples described below are conventional methods unless otherwise specified. The materials, reagents and apparatus used, unless otherwise specified, are conventional in the art and are commercially available to those skilled in the art.
As shown in fig. 1-2, the experimental device for gas-liquid co-permeation under shale reservoir conditions of the invention comprises: the reactor comprises a reactor 1, a hot oil furnace 2, a liquid supply unit 3, a liquid injection unit 4, a nuclear magnetic resonance instrument 5, a Raman test unit 6, a conductivity test unit 7 and a data monitoring unit 8, wherein the reactor 1 is arranged in the reactor 1 and can be used for carrying out nuclear magnetic spectrum detection on a core in the reactor 1, the reactor 1 is arranged in a heating cavity of the hot oil furnace 2, the liquid supply unit 3 and the liquid injection unit 4 are both communicated with the inner side of the reactor 1, the liquid supply unit 3 can be used for providing gas and crude oil in the reactor 1, the liquid supply unit 3 can be used for vacuumizing the reactor 1, the liquid injection unit 4 can be used for providing a surfactant in the reactor 1, the core can be placed in the reactor 1, the test end of the Raman test unit 6 is communicated with the inner side of the reactor 1, the conductivity test unit 7 can be used for carrying out water content measurement on the core in the reactor 1, and the Raman test unit 6 and the conductivity test unit 7 are both connected with the data monitoring unit 8 in a signal mode.
In some embodiments, the liquid supply unit 3 includes a gas storage intermediate container 31, a oil storage intermediate container 32, a displacement pump 33 and a vacuum pump 34, wherein an outlet of the gas storage intermediate container 31 is communicated with a top opening of the reaction kettle 1, an outlet of the oil storage intermediate container 32 is communicated with the top opening of the reaction kettle 1, an outlet of the displacement pump 33 is selectively communicated with an inlet of the gas storage intermediate container 31 and an inlet of the oil storage intermediate container 32 respectively through a multi-way valve 35, and the vacuum pump 34 is communicated with the top opening of the reaction kettle 1.
In some embodiments, the liquid injection unit 4 includes a surfactant intermediate container 41, an outlet of the surfactant intermediate container 41 is communicated with an opening at the top of the reaction kettle 1, and an outlet of the displacement pump 33 is selectively communicated with an inlet of the surfactant intermediate container 41 through a multi-way valve 35.
In the experimental device, corresponding interfaces are arranged on the upper end surface and the lower end surface of the reaction kettle 1, valves can be installed at the interfaces, valves can be installed at the openings of the gas storage intermediate container 31, the displacement pump 33 and the reaction kettle 1, valves can be installed at the openings of the oil storage intermediate container 32, valves can be installed at the openings of the surfactant intermediate container 41, and the multi-way valve 35 can selectively open or close any one or more channels as required to realize the communication of pipelines required in the experimental process.
The experimental device further comprises an air supply container which is communicated with the air storage intermediate container 31, and the air supply container can supplement air required by the experiment into the air storage intermediate container.
Example 1
(1) Placing the core into a reaction kettle 1, vacuumizing the reaction kettle 1 for 8 hours through a vacuum pump 34, respectively measuring the water content and the Raman spectrum of the core by using a conductivity test unit 7 and a Raman test unit 6, and collecting data through a data monitoring unit 8;
(2) Injecting crude oil in the oil storage intermediate container 32 into the reaction kettle 1 by the displacement pump 33, and pressurizing to 20MPa in the reaction kettle 1 by the displacement pump 33 and saturating the oil for 7d;
(3) Discharging crude oil in the reaction kettle 1, cleaning the reaction kettle 1, measuring the Raman spectrum of the core by using a Raman test unit 6, and collecting data by using a data monitoring unit 8;
(4) Injecting CO 2 gas in the gas storage intermediate container 32 into the reaction kettle 1 through the displacement pump 33, pressurizing to 5MPa at room temperature, keeping the pressure in the reaction kettle 1 for 30min, discharging the gas in the reaction kettle 1, testing a nuclear magnetic resonance T2 map of the reaction kettle 1 through the nuclear magnetic resonance instrument 5 in the process, testing a Raman spectrum of a core through the Raman testing unit 6, collecting data through the data monitoring unit 8, repeatedly completing gas throughput of five rounds and collecting data of the five rounds;
(5) After the throughput is finished, the surfactant in the surfactant intermediate container 41 is injected into the reaction kettle 1 from the bottom of the reaction kettle 1 through the displacement pump 33 until the reaction kettle 1 is full of the surfactant, then other outlets of the reaction kettle 1 are closed, the reaction kettle 1 is pressurized to 20MPa through a channel of the displacement pump 33-the surfactant intermediate container 41-the reaction kettle 1, the hot oil furnace 2 is heated to 60 ℃ for the imbibition of the surfactant under the high temperature condition, the nuclear magnetic T2 map of the reaction kettle 1 is tested at different moments of imbibition by using the nuclear magnetic resonance instrument 5, the calculated water content and the Raman spectrum of the core are measured and calculated by using the conductivity test unit 7 and the Raman test unit 6 respectively, and the data is collected by the data monitoring unit 8.
(6) After the imbibition is finished, the displacement pump 33 is closed, the liquid in the reaction kettle is discharged, a pipeline is cleaned, nuclear magnetism T2 map data are analyzed, a nuclear magnetism T2 map shown in figure 3 is drawn, the extraction degree is calculated, the result of calculating the utilization degree of crude oil with various sizes is shown in figure 4, the raman spectrum data are analyzed, the mineral composition is obtained, the mineral composition is shown in figure 6, conductivity data are analyzed, and the water content of the rock core is calculated as shown in the following table:
| Imbibition time/h | Conductivity/(s/m) | Moisture content/% |
| 0 | 0.002 | 0.356 |
| 0.5 | 0.01 | 1.18 |
| 1 | 0.0125 | 1.4375 |
| 2 | 0.02 | 2.21 |
| 3 | 0.025 | 2.725 |
Example 2
(1) Placing the core into a reaction kettle 1, vacuumizing the reaction kettle 1 for 8 hours through a vacuum pump 34, respectively measuring the water content and the Raman spectrum of the core by using a conductivity test unit 7 and a Raman test unit 6, and collecting data through a data monitoring unit 8;
(2) Injecting crude oil in the oil storage intermediate container 32 into the reaction kettle 1 by the displacement pump 33, and pressurizing to 20MPa in the reaction kettle 1 by the displacement pump 33 and saturating the oil for 7d;
(3) Discharging crude oil in the reaction kettle 1, cleaning the reaction kettle 1, measuring the Raman spectrum of the core by using a Raman test unit 6, and collecting data by using a data monitoring unit 8;
(4) Starting a heating cycle of a hot oil furnace 2, wherein the heating temperature of the hot oil furnace is 50 ℃, injecting CO 2 gas in a gas storage intermediate container 32 into a reaction kettle 1 through a displacement pump 33, pressurizing the gas to 20MPa through the displacement pump 33, keeping the pressure at 20MPa, replacing core crude oil with continuous CO 2 gas, simultaneously testing a nuclear magnetic T2 map of the reaction kettle 1 by using a nuclear magnetic resonance instrument 5 at different replacing moments, measuring a Raman spectrum of the core by using a Raman test unit 6, and collecting data by using a data monitoring unit 8;
(5) After CO 2 gas energization is finished for replacing core crude oil 28d, injecting surfactant in a surfactant intermediate container 41 into the reaction kettle 1 from the bottom of the reaction kettle 1 through a displacement pump 33 until the reaction kettle 1 is full of the surfactant, then closing other outlets of the reaction kettle 1, pressurizing the inside of the reaction kettle 1 to 20MPa through a passage of the displacement pump 33-the surfactant intermediate container 41-the reaction kettle 1, performing imbibition core oil extraction of the surfactant under high temperature conditions, testing a nuclear magnetic T2 map of the reaction kettle 1at different imbibition moments by using a nuclear magnetic resonance instrument 5, respectively measuring and calculating the water content and the Raman spectrum of the core by using a conductivity test unit 7 and a Raman test unit 6, and performing data collection by a data monitoring unit 8;
(6) After the imbibition is finished, the displacement pump 33 is closed, liquid in the reaction kettle is discharged, a pipeline is cleaned, nuclear magnetism T2 map data are analyzed, a nuclear magnetism T2 map shown in fig. 7 is drawn, the extraction degree is calculated, the result of calculating the crude oil utilization degree of each size is shown in fig. 8, the raman spectrum data are analyzed, the mineral composition is shown in fig. 10, conductivity data are analyzed, and the water content of the rock core is calculated as shown in the following table:
The experimental method designs an indoor simulation model for researching the core extraction degree and the pore crude oil utilization rules and characteristics of each size in the core in the gas injection and injection combined injection and extraction process aiming at the characteristics of the gas injection and injection combined fracturing fluid extraction process in the high-temperature and high-pressure development process of the real oil reservoir.
The method has the advantages that the error problem caused by pressure release during conventional offline nuclear magnetic testing is solved by using the reaction kettle and the online nuclear magnetic resonance instrument, the characterization of parameters such as core moisture content, mineral composition and the like under the high-temperature high-pressure and nuclear magnetic resonance environment is realized by using the conductivity testing unit and the Raman testing unit, the effect of gas and liquid on the core is realized, and the recovery degree, the core crude oil utilization condition, the core physical property change rule and the characteristic detection and analysis are improved.
In the method, the pressure, the temperature, the conductivity, the Raman spectrum and the nuclear magnetism T2 picture are accurately measured, the simulation development process is comprehensive, the experimental device is easy to assemble and repeatable, the gas, the liquid, the temperature and the pressure can be simulated, the conditions of the pressure are various, and the parameters are easy to measure.
The simulation of the gas injection extraction and fracturing fluid permeation extraction processes in actual exploitation provides theoretical basis for crude oil extraction of tight reservoirs, low-permeability reservoirs and the like.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (11)
1. The utility model provides a gas-liquid cooperated imbibition experimental apparatus under shale reservoir condition which characterized in that includes: the nuclear magnetic resonance device comprises a reaction kettle (1), a hot oil furnace (2), a liquid supply unit (3), a liquid injection unit (4), a nuclear magnetic resonance instrument (5) and a data monitoring unit (8), wherein the nuclear magnetic resonance instrument (5) can detect nuclear magnetic patterns in the reaction kettle (1), the reaction kettle (1) is arranged in a heating cavity of the hot oil furnace (2), the liquid supply unit (3) and the liquid injection unit (4) are communicated with the inner side of the reaction kettle (1), the liquid supply unit (3) can provide gas, crude oil or vacuumize the reaction kettle (1), the liquid injection unit (4) can provide surfactant in the reaction kettle (1), the nuclear magnetic resonance instrument (5) is in signal connection with the data monitoring unit (8).
2. The experimental device for gas-liquid co-permeation under the condition of shale reservoirs according to claim 1, wherein the liquid supply unit (3) comprises a gas storage intermediate container (31), an oil storage intermediate container (32), a displacement pump (33) and a vacuum pump (34), an outlet of the gas storage intermediate container (31) is communicated with a top opening of the reaction kettle (1), an outlet of the oil storage intermediate container (32) is communicated with the top opening of the reaction kettle (1), an outlet of the displacement pump (33) is selectively communicated with an inlet of the gas storage intermediate container (31) and an inlet of the oil storage intermediate container (32) respectively through a multi-way valve (35), and the vacuum pump (34) is communicated with the top opening of the reaction kettle (1).
3. The experimental device for gas-liquid co-permeation under shale reservoir conditions according to claim 2, wherein the liquid injection unit (4) comprises a surfactant intermediate container (41), an outlet of the surfactant intermediate container (41) is communicated with a top opening of the reaction kettle (1), and an outlet of the displacement pump (33) is selectively communicated with an inlet of the surfactant intermediate container (41) through a multi-way valve (35).
4. The gas-liquid collaborative imbibition experimental device under the shale reservoir condition according to claim 1, further comprising a raman test unit (6), wherein a test end of the raman test unit (6) is communicated with the inner side of the reaction kettle (1), the raman test unit (6) can perform raman spectrum measurement on a core in the reaction kettle (1), and the raman test unit (6) is in signal connection with the data monitoring unit (8).
5. The gas-liquid collaborative imbibition experimental device under the shale reservoir condition according to claim 1, further comprising a conductivity testing unit (7), wherein a testing end of the conductivity testing unit (7) is communicated with the inner side of the reaction kettle (1), the conductivity testing unit (7) can measure the water content of a rock core in the reaction kettle (1), and the conductivity testing unit (7) is in signal connection with a data monitoring unit (8).
6. An experimental method adopting the experimental device for gas-liquid collaborative imbibition under the condition of a shale reservoir as set forth in any one of claims 1-5, which is characterized by comprising the following steps:
Step one, putting a core into a reaction kettle (1), vacuumizing the reaction kettle (1) through a liquid supply unit (3), respectively measuring the water content of the core and the Raman spectrum, and recording data;
step two, injecting crude oil into the reaction kettle (1) through a liquid supply unit (3), pressurizing and saturating the oil;
Step three, discharging crude oil in the reaction kettle (1), measuring the Raman spectrum of the core after cleaning, and recording data;
step four, starting a hot oil furnace (2) to heat the reaction kettle (1), introducing gas into the reaction kettle (1) by a liquid supply unit (3) and pressurizing, discharging the gas for pressure relief after a certain time, performing nuclear magnetic T2 spectrum test on the reaction kettle (1) by a nuclear magnetic resonance instrument (5) during gas pressurization and pressure relief, and simultaneously performing Raman spectrum measurement on a rock core and recording data;
step five, repeating the step four to finish the gas throughput of the target round;
Step six, after the gas throughput is finished, the liquid injection unit (4) injects the surfactant into the reaction kettle (1), the reaction kettle (1) is pressurized to the formation pressure, the hot oil furnace (2) heats the reaction kettle (1) to the oil reservoir temperature, nuclear magnetic T2 spectrum test is carried out on the reaction kettle (1) through the nuclear magnetic resonance instrument (5), water content and Raman spectrum measurement are respectively carried out on the rock core, and data are recorded;
and step seven, after the imbibition is finished, discharging the liquid in the reaction kettle, and analyzing data.
7. An experimental method adopting the experimental device for gas-liquid collaborative imbibition under the condition of a shale reservoir as set forth in any one of claims 1-5, which is characterized by comprising the following steps:
Step one, putting a core into a reaction kettle (1), vacuumizing the reaction kettle (1) through a liquid supply unit (3), respectively measuring the water content of the core and the Raman spectrum, and recording data;
step two, injecting crude oil into the reaction kettle (1) through a liquid supply unit (3), pressurizing and saturating the oil;
Step three, discharging crude oil in the reaction kettle (1), measuring the Raman spectrum of the core after cleaning, and recording data;
Step four, starting a hot oil furnace (2) to heat the reaction kettle (1), introducing gas into the reaction kettle (1) by a liquid supply unit (3) and keeping a certain pressure, continuously replacing core crude oil in the reaction kettle (1) by the gas provided by the liquid supply unit (3), performing nuclear magnetic T2 spectrum test on the reaction kettle (1) by a nuclear magnetic resonance instrument (5) at different replaced moments, performing Raman spectrum measurement on the core, and recording data;
step five, after the gas replacement is finished, the liquid injection unit (4) injects the surfactant into the reaction kettle (1), pressurizes the reaction kettle (1) to a set pressure to carry out surfactant imbibition, carries out nuclear magnetic T2 spectrum test on the reaction kettle (1) through the nuclear magnetic resonance instrument (5) at different moments of imbibition, carries out water content and Raman spectrum measurement on the rock core respectively, and records data;
And step six, after the imbibition is finished, discharging the liquid in the reaction kettle (1), and analyzing data.
8. The method for testing a gas-liquid co-permeation testing device under shale reservoir conditions according to claim 6 or 7, wherein in the sixth step, the analysis data comprises calculation of crude oil permeation recovery ratio in the core at different moments, the calculation method comprises the following steps: Wherein R 1 is the imbibition recovery ratio,%; a 1 is the area surrounded by the T2 nuclear magnetic curve and the X axis of the residual crude oil, and the dimension is zero; a 2 is the area surrounded by the original saturated oil T2 nuclear magnetic curve and the X axis, and is dimensionless.
9. The method for testing a gas-liquid co-permeation testing device under shale reservoir conditions according to claim 6 or 7, wherein in the sixth step, the analysis data comprises calculating the permeation recovery ratio of crude oil with different sizes in the core, and the calculation method comprises the following steps: Wherein i is different pore types including micropores, small pores, mesopores and macropores, and is dimensionless; r i is the i-type pore absorption recovery ratio,%; a i1 is the area surrounded by the residual crude oil T2 nuclear magnetic curve of the i-type pore and the X axis, and the dimension is zero; a i2 is the area surrounded by the original saturated oil T2 nuclear magnetic curve and the X axis, and is dimensionless.
10. The experimental method of a gas-liquid synergistic imbibition experimental device under shale reservoir conditions as claimed in claim 6 or 7, wherein in the sixth step, the analysis data comprises the steps of calculating the water content in the core at different moments, and the calculation method comprises the following steps: Wherein m i is the mass at time t i, g; m is the dry weight of the core, g.
11. The method of claim 10, wherein in step six, the analysis data includes fitting a relationship between water content and core conductivity, the fitting relationship being: w i＝A*σi +b, wherein W i is water content,%; σ i is the core conductivity, s/m; a is a constant, and is obtained by fitting; b is a constant, obtained by fitting.
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