CN115165952B - Gas-water two-phase saturated rock core high-temperature high-pressure nuclear magnetic resonance experimental measurement method and device - Google Patents
Gas-water two-phase saturated rock core high-temperature high-pressure nuclear magnetic resonance experimental measurement method and device Download PDFInfo
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Abstract
The invention discloses a high-temperature high-pressure nuclear magnetic resonance experimental measurement method and device. The high-temperature high-pressure nuclear magnetic resonance experiment measuring method beneficial to the device can accurately control the gas-water saturation, can apply and control pore pressure and avoid the change of the gas-water saturation when the nuclear magnetic resonance high-temperature high-pressure experiment is carried out, and meets the requirement of carrying out the physical simulation experiment of the natural gas reservoir in a room.
Description
Technical Field
The invention belongs to the technical field of petroleum and natural gas matched exploration, relates to a petrophysical nuclear magnetic resonance experimental method, and particularly relates to a high-temperature high-pressure nuclear magnetic resonance experimental measurement method and device for a gas-water two-phase saturated core.
Background
Nuclear magnetic resonance is an effective means for obtaining parameters such as physical properties, pore structure, T2 cut-off value and the like of rock samples. In order to obtain the nuclear magnetic resonance response characteristics of the hydrocarbon reservoir under the formation temperature, pressure and oil-water saturation conditions, the existing high-temperature and high-pressure nuclear magnetic resonance generally applies confining pressure and temperature conditions to the core, and simultaneously adopts an oil flooding or water flooding mode to change the oil-water saturation of the core and collect nuclear magnetic resonance signals, and in this case, the outlet end is allowed to be opened to the atmosphere (the atmospheric pressure is 0.1 MPa), namely, no back pressure is added for experimental measurement, as shown in fig. 1.
Because natural gas and crude oil have great difference in hydrogen index, oil-water two-phase saturated rock core cannot be used for measuring nuclear magnetic resonance response characteristics of a gas reservoir. Meanwhile, due to the problems of good compressibility of gas and volume expansion after heating, nuclear magnetic resonance signals of a natural gas reservoir under high temperature and high pressure conditions cannot be obtained by directly using the existing device for measurement (shown in fig. 1). On the one hand, when the gas saturation is changed by displacing formation water with gas, high pore pressures cannot be established to simulate formation pressure because the outlet port is vented to atmosphere (atmospheric pressure is 0.1 MPa) without back pressure. On the other hand, venting the outlet end to atmosphere can cause the gas volume to expand during warming and change the gas saturation. The two problems cause that the method and the device for driving water by oil cannot be used for carrying out nuclear magnetic resonance signal measurement under the high-temperature and high-pressure condition of the natural gas reservoir, so that a new experimental method and a new experimental device are needed to be established, so that the nuclear magnetic resonance signal of the gas-water two-phase core under the high-temperature and high-pressure condition can be accurately obtained, and an accurate petrophysical experimental foundation is provided for the explanation and evaluation work of nuclear magnetic resonance logging of the natural gas reservoir.
Disclosure of Invention
In order to solve the technical problems, the invention provides a high-temperature high-pressure nuclear magnetic resonance experiment measurement method and device, which can accurately control the gas-water saturation, can apply and control pore pressure and avoid the change of the gas-water saturation when carrying out nuclear magnetic resonance high-temperature high-pressure experiments, and meet the needs of carrying out physical simulation experiments of natural gas reservoirs indoors.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a high-temperature high-pressure nuclear magnetic resonance experiment measuring device comprises a computer, a nuclear magnetic resonance measuring instrument, a magnet box with a non-magnetic core holder, a core sample, a confining pressure intermediate container, a confining pressure pump, a pore intermediate container, a pore pressure pump, a feedback control pressure pump and a measuring cylinder;
one side of the nuclear magnetic resonance measuring instrument is connected with a computer, and the other side of the nuclear magnetic resonance measuring instrument is connected with a non-magnetic core holder in the magnet box;
the non-magnetic core holder is internally provided with a core sample;
the two sides of the nonmagnetic core holder are respectively connected with a confining pressure intermediate container through confining pressure valves, and the confining pressure intermediate container is connected with a confining pressure pump;
the inlet end and the outlet end of the nonmagnetic core holder are respectively connected with a pore middle container through a pore pressure valve, and the pore middle container is connected with a pore pressure pump;
the outlet end of the nonmagnetic core holder is connected with a feedback pressure pump through a feedback pressure valve, and the feedback pressure valve is connected with a measuring cylinder.
Preferably, the magnetic core holder, the confining pressure intermediate container and the confining pressure valve are connected through a metal nonmagnetic pipeline.
Preferably, the confining pressure intermediate container is connected with a temperature controller.
Preferably, the number of the confining pressure intermediate containers is 2, and the confining pressure intermediate containers comprise a No. 1 confining pressure intermediate device and a No. 2 confining pressure intermediate device.
Further preferably, the confining pressure intermediate container is filled with fluorine oil.
Preferably, the pore intermediate container is filled with brine or methane gas.
The invention also provides a high-temperature high-pressure nuclear magnetic resonance experimental measurement method, which adopts the high-temperature high-pressure nuclear magnetic resonance experimental measurement device to measure the core sample.
Preferably, the high-temperature high-pressure nuclear magnetic resonance experimental measurement method comprises the following steps:
s1, filling fluorine oil into a confining pressure intermediate container 1 and a confining pressure container 2, and opening a temperature controller to heat the fluorine oil to the stratum temperature;
s2, placing the pretreated core sample into a non-magnetic core holder in a magnet box, adjusting the pressure of a confining pressure pump, and applying confining pressure to the core sample;
s3, adjusting the back control pressure pump to enable the back control pressure valve to reach preset pressure, and enabling water or gas in the pipeline at the outlet end to flow into the measuring cylinder through the pipeline.
S4, filling saline into the pore intermediate container, opening a pore pressure valve, adjusting a pore pressure pump, applying pressure to two ends of the core sample until the pressure reaches a preset pressure, and closing the pore pressure valve.
S5, adjusting pressure values of the confining pressure pump No. 1, the confining pressure pump No. 2 and the pore pressure pump, applying confining pressure to the core sample by using fluorine oil, applying pore pressure to the core sample by using brine, keeping the pressure difference between the confining pressure and the pore pressure to be less than 10Mpa, and gradually increasing the pressure to the formation pressure P;
s6, adjusting the pressure P1 of the confining pressure pump No. 1 to enable the confining pressure pump No. 1 and the confining pressure pump No. 2 to generate confining pressure difference delta P, and driving the liquid in the confining pressure intermediate container No. 2 to enter the confining pressure intermediate container No. 1 through the confining pressure cavity of the nonmagnetic core holder;
s7, after all the fluorine oil in the confining pressure intermediate container No. 2 enters the confining pressure intermediate container No. 1, adjusting the pressure of the confining pressure pump No. 1 to be the formation pressure P, setting the pressure of the confining pressure pump No. 2 to be P2', and enabling the fluorine oil in the confining pressure intermediate container No. 1 to enter the confining pressure intermediate container No. 2 through the confining pressure cavity of the nonmagnetic core holder under the action of pressure difference;
s8, repeating the steps S6 and S7, so that the temperature in the confining pressure cavity of the non-magnetic core holder is always kept at the stratum temperature;
s9, collecting high-temperature high-pressure nuclear magnetic resonance parameters of a core sample in a saturated saline state;
s10, white oil is filled in the measuring cylinder;
s11, filling methane gas into a pore intermediate container, opening an inlet pore pressure valve, closing an outlet pore pressure valve, adjusting a back control pressure pump to proper pressure, opening the back control pressure valve, and enabling water or gas in an outlet end pipeline to flow into a measuring cylinder through a pipeline;
s12, adjusting a pore pressure pump to a proper displacement pressure according to physical properties of the core, driving methane gas in a pore middle container to displace the core sample to a proper water saturation or gas saturation, and calculating the water saturation or gas saturation of the core according to water yield or gas yield in a measuring cylinder;
s13, repeating the steps S5, S6 and S7, recovering the temperature, the confining pressure and the pore pressure to the stratum condition, and collecting the high-temperature high-pressure nuclear magnetic resonance parameters of the gas-water two-phase saturated core.
Further preferably, the preprocessing of the core sample in step S2 is: and (3) after washing oil and drying the core sample, vacuumizing and pressurizing saturated brine, and calculating the pore volume, the total volume and the porosity of the core according to the dry weight, the wet weight and the floating weight of the core sample.
Further preferably, in step S6, the calculation formula of the pressure P1 of the confining pressure pump No. 1 is: p1=p-0.5 Mpa.
Further preferably, in step S6, the calculation formula of the confining pressure difference Δp is: Δp=p2-P1, where P2 is the pressure of the No. 2 confining pressure pump.
Further preferably, the calculation formula of P2' in step S7 is: p2' =p-0.5 Mpa.
The beneficial effects of the invention are as follows:
aiming at the situation that no feasible high-temperature high-pressure nuclear magnetic resonance experimental measurement method capable of avoiding the change of the gas-water saturation exists at present, the invention provides the high-temperature high-pressure nuclear magnetic resonance experimental measurement method and the device capable of controlling the gas-water saturation of the core, the pore pressure and the temperature and avoiding the change of the gas-water two-phase saturated core. The method comprises the steps of selecting a sandstone plunger sample from a certain depth section, based on a high-temperature high-pressure nuclear magnetic resonance experiment of a gas-water two-phase saturated core, utilizing the characteristic that fluorine oil does not contain hydrogen and does not generate nuclear magnetic signals, adopting fluorine oil as confining pressure application and a heat transfer medium, heating two intermediate containers at two ends of a distributed core, realizing heating control temperature of the core through reciprocating motion of the heated fluorine oil in the two intermediate containers, adopting methane gas as a pore pressure application medium, realizing simultaneous application of high pore pressure at two ends of the core by setting a back control pressure valve pressure limit, and finally measuring to obtain a nuclear magnetic T2 spectrogram of the rock sample under the conditions of high temperature, high pressure and different gas saturation.
Drawings
FIG. 1 is a diagram of a conventional oil-water two-phase saturated core high-temperature high-pressure nuclear magnetic resonance experimental device in the prior art;
wherein, 1, enclosing the pressure pump; 2. a pore pressure pump; 3. a confining pressure valve; 4. a pore pressure valve; 5. a metal pipeline; 6. a magnet box; 7. a core sample; 8. a measuring cylinder; 9. a data link line; 10. a computer; 11. nuclear magnetic resonance measuring instrument.
FIG. 2 is a diagram of an experimental apparatus of the present invention;
wherein, the enclosed pressure pumps of the numbers 1 and 1; 2. a No. 2 confining pressure pump; 3. a pore pressure pump; 4. a middle container 1; 5. a number 2 intermediate container; 6. a void intermediate container; 7. a number 1 confining pressure valve; 8. a No. 2 confining pressure valve; 9. an inlet pore pressure valve; 10. an outlet pore pressure valve; 11. a back-control pressure valve; 12. a measuring cylinder; 13. a metal nonmagnetic pipeline; 14. a magnet box; 15. a core sample; 16. a data link line; 17. a computer; 18. nuclear magnetic resonance measuring instrument; 19. a temperature controller; 20. and (5) back-controlling the pressure pump.
Fig. 3 is a flow chart of the method of the present invention.
FIG. 4 is a diagram of a T2 spectrum of an embodiment of the present invention.
Detailed Description
Other advantages and effects of the present invention will become apparent to those skilled in the art from the following disclosure, which describes embodiments of the present invention in conjunction with specific embodiments. The invention may be practiced or carried out in other embodiments that depart from the specific details, and the details of the present description may be modified or varied from the spirit and scope of the present invention.
Before the embodiments of the invention are explained in further detail, it is to be understood that the invention is not limited in its scope to the particular embodiments described below; it is also to be understood that the terminology used in the examples of the invention is for the purpose of describing particular embodiments only, and is not intended to limit the scope of the invention.
As shown in fig. 2, the invention provides a high-temperature high-pressure nuclear magnetic resonance experimental measurement device, which comprises a computer 17, a nuclear magnetic resonance measuring instrument 18, a magnet box 14 with a non-magnetic core holder arranged inside, a core sample 15, a confining pressure intermediate container 4, a confining pressure intermediate container 5, a confining pressure pump 1, a confining pressure pump 2, a pore intermediate container 6, a pore pressure pump 3, a feedback control pressure pump 20 and a measuring cylinder 12;
one side of the nuclear magnetic resonance measuring instrument 18 is connected with the computer 17, and the other side is connected with the non-magnetic core holder in the magnet box 14;
the non-magnetic core holder is internally provided with a core sample 15;
the two sides of the nonmagnetic core holder are respectively connected with a confining pressure intermediate container 4 and a confining pressure intermediate container 5 of No. 1 through a confining pressure valve 7 of No. 1 and a confining pressure valve 8 of No. 2, and the confining pressure intermediate container 4 of No. 1 and the confining pressure intermediate container 5 of No. 2 are connected with a confining pressure pump 1 of No. 1 and a confining pressure pump 2 of corresponding No. 2;
the inlet end and the outlet end of the nonmagnetic core holder are respectively connected with the pore intermediate container 6 through an inlet pore pressure valve 9 and an outlet pore pressure valve 10, and the pore intermediate container 6 is connected with the pore pressure pump 3;
the outlet end of the nonmagnetic core holder is connected with a feedback pressure pump 20 through a feedback pressure valve 11, and the feedback pressure valve 11 is connected with a measuring cylinder 12.
Preferably, the magnetic core holder, the confining pressure intermediate container and the confining pressure valve are connected by a metal nonmagnetic pipeline 13.
Preferably, the confining pressure intermediate container is connected with a temperature controller 19.
Preferably, the confining pressure intermediate container is filled with fluorine oil.
Preferably, the pore intermediate container is filled with brine or methane gas.
The invention also provides a high-temperature high-pressure nuclear magnetic resonance experimental measurement method, which adopts the high-temperature high-pressure nuclear magnetic resonance experimental measurement device to measure the core sample. The method and apparatus of the present invention will now be described in detail with reference to FIG. 3 and the specific embodiment, taking a certain reservoir A well as an example.
Example 1
The high-temperature high-pressure nuclear magnetic resonance experiment measurement method specifically comprises the following steps of:
s1, selecting 5 sandstone plunger samples at a certain depth section, and vacuumizing and pressurizing saturated brine after washing oil and drying the rock samples. Calculating the pore volume, the total volume and the porosity of the core sample according to the dry weight, the wet weight and the floating weight of the rock sample;
s2, filling fluorine oil into the confining pressure intermediate container 4 and the confining pressure intermediate container 5, opening a temperature controller 19, setting the temperature to be 80 ℃ of the stratum, and heating the fluorine oil in the confining pressure intermediate container 4 and the confining pressure intermediate container 5 to the stratum temperature of 80 ℃;
s3, placing a core sample of saturated brine into a holder of the device, adjusting the pressure of a No. 1 confining pressure pump 1 and a No. 2 confining pressure pump 2 to be 3MPa, and driving fluorine oil in an intermediate container to apply 3MPa confining pressure;
s4, adjusting the back control pressure pump 20 to 60MPa, and setting the pressure limit of 60MPa for the back control pressure valve 11;
s5, filling the pore intermediate container 6 with saline water with the same mineralization degree, opening an inlet pore pressure valve 9 and an outlet pore pressure valve 10, adjusting the pressure of the pore pressure pump 3 to 0.5MPa, applying pore pressure to 0.5MPa at two ends of a core sample, and closing the inlet pore pressure valve 9 and the outlet pore pressure valve 10;
s6, adjusting the pressure values of the confining pressure pump 1, the confining pressure pump 2 and the pore pressure pump 3, and increasing the confining pressure to 58MPa and the pore pressure to 50MPa under the condition that the confining pressure and the pore pressure difference are always kept to be smaller than 10 MPa;
s7, adjusting the pressure of the confining pressure pump 1 of the No. 1 to 57.5MPa, wherein the pressure difference between the pressure of the confining pressure pump 2 of the No. 2 and the pressure of the confining pressure pump 1 of the No. 1 is 0.5MPa, and the confining pressure pump 2 of the No. 2 starts to drive high-temperature liquid in the confining pressure intermediate container 5 of the No. 2 to enter the confining pressure intermediate container 4 of the No. 1 through a confining pressure cavity of a clamp holder;
s8, after all the fluorine oil in the confining pressure intermediate container 5 of the No. 2 enters the confining pressure intermediate container 4 of the No. 1, recovering the pressure of the confining pressure pump 1 to be 58MPa of the stratum pressure, and setting the pressure of the confining pressure pump 2 of the No. 2 to be 57.5MPa. At the moment, due to the pressure difference effect, the liquid in the confining pressure intermediate container No. 1 enters the confining pressure intermediate container No. 2 5 through the confining pressure cavity of the clamp holder;
s9, repeating the steps S7 and S8, so that the internal temperature of the clamp holder is always kept at the set stratum temperature of 80 ℃;
s10, collecting high-temperature high-pressure nuclear magnetic resonance parameters of a saturated saline state core sample 15;
s11, filling a small amount of white oil into the measuring cylinder 12, so that the white oil is ensured to submerge the outlet end of the displacement pipeline, and gas (salt water) at the outlet end is prevented from diffusing into the air, so that inaccurate measurement of the saturation degree of the gas (water) is prevented;
s12, filling methane gas into the gap intermediate container 6, opening an inlet pore pressure valve 9, closing an outlet pore pressure valve 10, adjusting a back control pressure pump 20 to 0.5MPa pressure, opening a back control pressure valve 11, and enabling water (gas) in an outlet end pipeline to flow into a measuring cylinder 12 through a pipeline;
s13, adjusting the displacement pressure of the pore pressure pump 3 to 1MPa, driving methane gas in the pore intermediate container 6 to displace the core sample 15 to proper water (gas) saturation, and calculating the core water (gas) saturation according to the water (gas) outlet in the measuring cylinder 12 at the outlet end of the measuring clamp;
s14, repeating the steps S6, S7 and S8, recovering the temperature, confining pressure and pore pressure to the stratum condition, and collecting the high-temperature high-pressure nuclear magnetic resonance parameters of the gas-water two-phase saturated core, wherein the result is shown in fig. 4.
It should be emphasized that the examples described herein are illustrative rather than limiting, and therefore the invention includes, but is not limited to, the examples described in the detailed description, as other embodiments derived from the technical solutions of the invention by a person skilled in the art are equally within the scope of the invention.
Claims (2)
1. The high-temperature high-pressure nuclear magnetic resonance experimental measurement method is characterized by adopting a high-temperature high-pressure nuclear magnetic resonance experimental measurement device to measure a core sample and comprising the following steps of:
s1, filling fluorine oil into a confining pressure intermediate container 1 and a confining pressure container 2, and opening a temperature controller to heat the fluorine oil to the stratum temperature;
s2, placing the pretreated core sample into a non-magnetic core holder in a magnet box, adjusting the pressure of a confining pressure pump, and applying confining pressure to the core sample;
s3, adjusting a back control pressure pump to enable a back control pressure valve to reach preset pressure, and enabling water or gas in a pipeline at an outlet end to flow into a measuring cylinder through the pipeline;
s4, filling saline into the pore middle container, opening a pore pressure valve, adjusting a pore pressure pump, applying pressure to two ends of the core sample until the pressure reaches a preset pressure, and closing the pore pressure valve;
s5, adjusting pressure values of the confining pressure pump No. 1, the confining pressure pump No. 2 and the pore pressure pump, applying confining pressure to the core sample by using fluorine oil, applying pore pressure to the core sample by using brine, keeping the pressure difference between the confining pressure and the pore pressure to be less than 10Mpa, and gradually increasing the pressure to the formation pressure P;
s6, adjusting the pressure P1 of the confining pressure pump No. 1 to enable the confining pressure pump No. 1 and the confining pressure pump No. 2 to generate confining pressure difference delta P, and driving the liquid in the confining pressure intermediate container No. 2 to enter the confining pressure intermediate container No. 1 through the confining pressure cavity of the nonmagnetic core holder;
the calculation formula of the pressure P1 of the No. 1 confining pressure pump is as follows: p1=p-0.5 Mpa; the calculation formula of the confining pressure difference delta P is as follows: Δp=p2-P1, where P2 is the pressure of the No. 2 confining pressure pump;
s7, after all the fluorine oil in the confining pressure intermediate container No. 2 enters the confining pressure intermediate container No. 1, adjusting the pressure of the confining pressure pump No. 1 to be the formation pressure P, setting the pressure of the confining pressure pump No. 2 to be P2', and enabling the fluorine oil in the confining pressure intermediate container No. 1 to enter the confining pressure intermediate container No. 2 through the confining pressure cavity of the nonmagnetic core holder under the action of pressure difference;
wherein, the calculation formula of the P2' is as follows: p2' =p-0.5 Mpa;
s8, repeating the steps S6 and S7, so that the temperature in the confining pressure cavity of the non-magnetic core holder is always kept at the stratum temperature;
s9, collecting high-temperature high-pressure nuclear magnetic resonance parameters of a core sample in a saturated saline state;
s10, white oil is filled in the measuring cylinder;
s11, filling methane gas into a pore intermediate container, opening an inlet pore pressure valve, closing an outlet pore pressure valve, adjusting a back control pressure pump to proper pressure, opening the back control pressure valve, and enabling water or gas in an outlet end pipeline to flow into a measuring cylinder through a pipeline;
s12, adjusting a pore pressure pump to a proper displacement pressure according to physical properties of the core, driving methane gas in a pore middle container to displace the core sample to a proper water saturation or gas saturation, and calculating the water saturation or gas saturation of the core according to water yield or gas yield in a measuring cylinder;
s13, repeating the steps S5, S6 and S7, recovering the temperature, confining pressure and pore pressure to stratum conditions, and collecting high-temperature high-pressure nuclear magnetic resonance parameters of the gas-water two-phase saturated core;
specifically, the high-temperature high-pressure nuclear magnetic resonance experiment measuring device comprises a computer, a nuclear magnetic resonance measuring instrument, a magnet box with a non-magnetic core holder, a core sample, a confining pressure intermediate container, a confining pressure pump, a pore intermediate container, a pore pressure pump, a feedback control pressure pump and a measuring cylinder;
one side of the nuclear magnetic resonance measuring instrument is connected with a computer, and the other side of the nuclear magnetic resonance measuring instrument is connected with a non-magnetic core holder in the magnet box;
the non-magnetic core holder is internally provided with a core sample;
the two sides of the nonmagnetic core holder are respectively connected with a confining pressure intermediate container through confining pressure valves, and the confining pressure intermediate container is connected with a confining pressure pump;
the inlet end and the outlet end of the nonmagnetic core holder are respectively connected with a pore middle container through a pore pressure valve, and the pore middle container is connected with a pore pressure pump;
the outlet end of the nonmagnetic core holder is connected with a feedback pressure pump through a feedback pressure valve, and the feedback pressure valve is connected with a measuring cylinder;
the magnetic core holder, the confining pressure intermediate container and the confining pressure valve are connected through a metal nonmagnetic pipeline;
the confining pressure intermediate container is connected with a temperature controller;
the confining pressure intermediate container is filled with fluorine oil; the pore intermediate container is filled with brine or methane gas;
the confining pressure middle container comprises a No. 1 confining pressure middle container and a No. 2 confining pressure middle container, one end of the No. 1 confining pressure middle container is connected with a No. 1 confining pressure pump, the other end of the No. 1 confining pressure middle container is connected with a confining pressure cavity of the nonmagnetic core holder through a pipeline, one end of the No. 2 confining pressure middle container is connected with the No. 2 confining pressure pump, and the other end of the No. 2 confining pressure middle container is connected with a confining pressure cavity of the nonmagnetic core holder through a pipeline.
2. The method according to claim 1, wherein the pretreatment of the core sample in step S2 is: and (3) after washing oil and drying the core sample, vacuumizing and pressurizing saturated brine, and calculating the pore volume, the total volume and the porosity of the core sample according to the dry weight, the wet weight and the floating weight of the core sample.
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