CN113552039A - High-temperature high-pressure water-liquid sulfur two-phase infiltration testing method - Google Patents
High-temperature high-pressure water-liquid sulfur two-phase infiltration testing method Download PDFInfo
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- 239000011593 sulfur Substances 0.000 title claims abstract description 211
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 211
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 200
- 239000007788 liquid Substances 0.000 title claims abstract description 198
- 238000012360 testing method Methods 0.000 title claims abstract description 45
- 230000008595 infiltration Effects 0.000 title claims abstract description 17
- 238000001764 infiltration Methods 0.000 title claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 115
- 230000035699 permeability Effects 0.000 claims abstract description 78
- 238000000034 method Methods 0.000 claims abstract description 46
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 41
- 239000011435 rock Substances 0.000 claims abstract description 40
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000007789 gas Substances 0.000 claims abstract description 17
- 239000012530 fluid Substances 0.000 claims abstract description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 9
- 239000008398 formation water Substances 0.000 claims abstract description 8
- 239000012071 phase Substances 0.000 claims description 114
- 238000002347 injection Methods 0.000 claims description 33
- 239000007924 injection Substances 0.000 claims description 33
- 239000008346 aqueous phase Substances 0.000 claims description 13
- 238000004088 simulation Methods 0.000 claims description 13
- 239000007787 solid Substances 0.000 claims description 12
- 229920006395 saturated elastomer Polymers 0.000 claims description 9
- 238000001514 detection method Methods 0.000 claims description 6
- 238000010998 test method Methods 0.000 claims description 6
- 238000011161 development Methods 0.000 abstract description 6
- 230000007812 deficiency Effects 0.000 abstract description 2
- 238000006073 displacement reaction Methods 0.000 description 13
- 238000004364 calculation method Methods 0.000 description 8
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 6
- 239000011148 porous material Substances 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 238000004140 cleaning Methods 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000003345 natural gas Substances 0.000 description 3
- 238000009738 saturating Methods 0.000 description 3
- GWZOLWLJEJRQMZ-UHFFFAOYSA-N [S].S Chemical compound [S].S GWZOLWLJEJRQMZ-UHFFFAOYSA-N 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
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- 239000005864 Sulphur Substances 0.000 description 1
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- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000003209 petroleum derivative Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
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- 238000006467 substitution reaction Methods 0.000 description 1
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N15/0806—Details, e.g. sample holders, mounting samples for testing
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N15/082—Investigating permeability by forcing a fluid through a sample
- G01N15/0826—Investigating permeability by forcing a fluid through a sample and measuring fluid flow rate, i.e. permeation rate or pressure change
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Abstract
The invention discloses a high-temperature high-pressure water-liquid sulfur two-phase infiltration testing method, which comprises the following steps of: s1: preparing a rock core and an experimental fluid, wherein the experimental fluid comprises nitrogen, simulated formation water and liquid sulfur, and calibrating the dead volume of the phase permeation testing device; s2: establishing a high-temperature high-pressure simulated formation environment; s3: establishing irreducible water saturation, and determining the liquid sulfur permeability under the irreducible water saturation; s4: measuring the effective permeability of the liquid sulfur phase and the water phase by adopting a steady state method, or measuring the relative permeability of the water and the liquid sulfur by adopting an unsteady state method; s5: and (5) finishing the experimental result of the step S4, and calculating and drawing a water-liquid sulfur two-phase permeation curve. The method can accurately, safely and efficiently measure the two-phase permeability of water and liquid sulfur under the formation condition, makes up for the deficiency of the water-liquid sulfur two-phase permeability test technical method in the prior art, and provides reliable data support for the reasonable development of related gas reservoirs.
Description
Technical Field
The invention relates to the technical field of petroleum and natural gas exploration and development, in particular to a high-temperature high-pressure water-liquid sulfur two-phase infiltration testing method.
Background
High sulfur-containing gas reservoirs are distributed all over the world, and with the continuous development of oil exploration technology, more and more high sulfur-containing gas reservoirs are successively discovered and developed worldwide. In the process of natural gas exploitation, along with the production of gas and the reduction of formation temperature and pressure, the solubility of sulfur in natural gas is reduced, and the sulfur is gathered and precipitated, and exists in the form of liquid sulfur when the temperature is higher than 120 ℃, so that water-sulfur-containing hydrogen sulfide-sulfur multiphase flow can be formed in a reservoir at the moment, and the flow characteristics and seepage rules of the water-sulfur-containing hydrogen sulfide-sulfur multiphase flow are complex.
At present, in the field of oil development, research on water-gas-sulfur multiphase flow of a gas reservoir is mostly concentrated on the aspect of gas-water and gas-liquid sulfur flow rules, the water-liquid sulfur co-flow rule is not involved, and a phase permeation test in the oil industry only provides a method for measuring oil-water and gas-liquid relative permeability according to a standard GB/T28912-2012 'method for measuring relative permeability of two-phase fluid in rock', and a core water-liquid sulfur two-phase permeation experiment is not described much.
Disclosure of Invention
Aiming at the problems, the invention aims to provide a high-temperature high-pressure water-liquid sulfur two-phase infiltration testing method.
The technical scheme of the invention is as follows:
a high-temperature high-pressure water-liquid sulfur two-phase infiltration test method comprises the following steps:
s1: preparing a rock core and an experimental fluid, wherein the experimental fluid comprises nitrogen, simulated formation water and liquid sulfur, and calibrating the dead volume of the phase permeation testing device;
s2: establishing a high-temperature high-pressure simulated formation environment;
s3: establishing irreducible water saturation, and determining the liquid sulfur permeability under the irreducible water saturation;
s4: measuring the effective permeability of the liquid sulfur phase and the water phase by adopting a steady state method, or measuring the relative permeability of the water and the liquid sulfur by adopting an unsteady state method;
s5: and (5) finishing the experimental result of the step S4, and calculating and drawing a water-liquid sulfur two-phase permeation curve.
Preferably, in step S1, when preparing liquid sulfur, corresponding solid sulfur is selected from the core, and when in use, the solid sulfur is heated and melted into liquid sulfur, and the viscosity of the liquid sulfur at the simulated formation temperature is calculated.
Preferably, when the simulated formation temperature is less than 160.5 ℃, the viscosity of the liquid sulfur is calculated by the following formula:
in the formula: mu.ssViscosity of liquid sulfur, mPa · s; t is the formation simulation temperature, DEG C.
Preferably, when the simulated formation temperature is greater than or equal to 160.5 ℃ and less than or equal to 187.575 ℃, the viscosity of the liquid sulfur is calculated by the following formula:
in the formula: mu.ssViscosity of liquid sulfur, mPa · s; t is the formation simulation temperature, DEG C.
Preferably, when the simulated formation temperature is greater than 187.575 ℃ and less than 314 ℃, the viscosity of the liquid sulfur is calculated by the following formula:
in the formula: mu.ssViscosity of liquid sulfur, mPa · s; t is the formation simulation temperature, DEG C.
Preferably, in step S4, the effective permeabilities of the liquid sulfur phase and the aqueous phase are determined at different water saturations when the effective permeabilities of the liquid sulfur phase and the aqueous phase are determined using a steady state method.
Preferably, in step S4, when the relative permeability of water and liquid sulfur is measured by the unsteady state method, the core is saturated with liquid sulfur, and then water flooding is performed to measure the relative permeability of water and liquid sulfur.
Preferably, in step S1, the infiltration testing apparatus includes an injection system, a core holder, a back pressure system, a metering system, and a formation simulation system;
the injection system is connected with the input end of the core holder, and a first valve and a first pressure gauge are sequentially arranged on a pipeline connected with the injection system; the injection system comprises a gas phase injection pipeline, a liquid sulfur phase injection pipeline and a water phase injection pipeline which are arranged in parallel, wherein the gas phase injection pipeline comprises a nitrogen cylinder and a valve II which are connected in sequence; the liquid sulfur phase injection pipeline comprises a first input pump, a third valve, a liquid sulfur intermediate container and a fourth valve which are connected in sequence; the water phase injection pipeline comprises an input pump II, a valve V, a water phase intermediate container and a valve VI which are connected in sequence;
two ends of the rock core holder are connected with two detection ends of the resistivity tester;
the back pressure system comprises a second pressure gauge, a back pressure pump and a back pressure valve which are sequentially connected, the input end of the back pressure valve is connected with the output end of the core holder, and a seventh valve and a third pressure gauge are sequentially arranged on a pipeline connected with the back pressure valve;
the metering system comprises a liquid-liquid separator, a liquid-sulfur meter and a water meter, wherein one output end of the liquid-liquid separator is connected with the liquid-sulfur meter, a valve eighth is arranged on a connected pipeline, the other output end of the liquid-liquid separator is connected with the water meter, and a valve ninth is arranged on the connected pipeline;
the stratum simulation system comprises a constant temperature box and a confining pressure pump, the confining pressure pump is connected with a pressure gauge IV, and the output end of the confining pressure pump is connected with the confining pressure input end of the core holder; the liquid sulfur intermediate container, the water phase intermediate container, the first pressure gauge, the rock core holder, the third pressure gauge, the liquid-liquid separator, the liquid sulfur meter and the water meter are all arranged in the thermostat.
Preferably, two ends of the core holder are respectively connected with two detection ends of the pressure difference meter.
Preferably, the first input pump and the second input pump both adopt constant-speed constant-pressure pumps.
The invention has the beneficial effects that:
the method can accurately, safely and efficiently measure the two-phase permeability of water and liquid sulfur under the formation condition, makes up for the deficiency of the water-liquid sulfur two-phase permeability test technical method in the prior art, and provides reliable data support for the reasonable development of related gas reservoirs.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a schematic flow chart of the high temperature and high pressure water-liquid sulfur two-phase permeation test method of the present invention;
FIG. 2 is a schematic structural diagram of a phase permeation testing device of the high-temperature high-pressure water-liquid sulfur two-phase permeation testing method of the present invention;
FIG. 3 is a schematic diagram showing the results of a steady state method water-liquid sulfur two-phase permeation test according to an embodiment of the present invention;
FIG. 4 is a schematic diagram showing the results of a steady-state method water-liquid sulfur two-phase permeation test according to another embodiment of the present invention.
Reference numbers in the figures: 1-nitrogen cylinder, 2-valve II, 3-input pump I, 4-valve III, 5-input pump II, 6-valve V, 7-liquid sulfur intermediate container, 8-water phase intermediate container, 9-valve IV, 10-valve VI, 11-valve I, 12-core holder, 13-confining pump, 14-pressure gauge IV, 15-valve VII, 16-valve VIII, 17-liquid sulfur meter, 18-valve IX, 19-water meter, 20-liquid separator, 21-back pressure valve, 22-back pressure pump, 23-pressure gauge II, 24-pressure gauge III, 25-pressure difference gauge, 26-resistivity tester, 27-pressure gauge I and 28-constant temperature box.
Detailed Description
The invention is further illustrated with reference to the following figures and examples. It should be noted that, in the present application, the embodiments and the technical features of the embodiments may be combined with each other without conflict. It is noted that, unless otherwise indicated, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The use of the terms "comprising" or "including" and the like in the present disclosure is intended to mean that the elements or items listed before the term cover the elements or items listed after the term and their equivalents, but not to exclude other elements or items.
As shown in figure 1, the invention provides a high-temperature high-pressure water-liquid sulfur two-phase permeation test method, which adopts a steady state method to perform a water-liquid sulfur two-phase permeation test or adopts an unsteady state method to perform a water-liquid sulfur two-phase permeation test.
When a steady state method is adopted to carry out a water-liquid-sulfur two-phase permeability test, firstly, the irreducible water saturation of a rock core needs to be established, and the liquid-sulfur phase permeability under the irreducible water saturation state is determined; under the condition of ensuring that the flow is not changed, simultaneously injecting liquid sulfur and water into the rock core at a constant speed according to a certain proportion, measuring the inlet and outlet of the rock core and the flow rate of the liquid sulfur and the water at the current moment when the flow is stable and the water saturation is not changed, and measuring the water saturation in the rock core through a resistivity measuring instrument to obtain the saturation of the liquid sulfur, so as to calculate the effective permeability and the relative permeability of the water and the liquid sulfur of the rock core; and finally, by changing the injection proportion of the liquid sulfur and the water and repeating the steps, the relative permeability values of the water and the liquid sulfur of the rock core in different water saturation degrees can be obtained, and a water-liquid sulfur two-phase permeability curve of the rock core is drawn according to the relative permeability values.
When an unsteady state method is adopted to carry out a water-liquid-sulfur two-phase permeability test, firstly, the irreducible water saturation of a rock core needs to be established, and the liquid-sulfur phase permeability under the irreducible water saturation state is determined; after the rock core is saturated by liquid sulfur, a prepared stratum water sample is injected into the holder at a constant speed to displace the liquid sulfur in the rock core, the displacement process is an unstable process, the distribution of the water and the liquid sulfur in the rock core is a function of distance and time, the output of each fluid and the change of the pressure difference at two ends of the rock core along with time are recorded at the outlet end of the rock core, the relative permeability of the water and the liquid sulfur are calculated, and a water-liquid sulfur two-phase permeability curve is drawn according to the relative permeability.
When the method is used for testing by a steady state method or an unsteady state method, the viscosity of the liquid sulfur is calculated by the following formula:
when the simulated formation temperature is less than 160.5 ℃:
in the formula: mu.ssViscosity of liquid sulfur, mPa · s; t is the formation simulation temperature, DEG C.
When the simulated formation temperature is greater than or equal to 160.5 ℃ and less than or equal to 187.575 ℃:
when the simulated formation temperature is greater than 187.575 ℃ and less than 314 ℃:
compared with the existing liquid sulfur viscosity formula, the method for calculating the viscosity of the liquid sulfur has the advantages of higher accuracy and less than 3% of overall error.
In one specific embodiment, as shown in fig. 2, a water-liquid-sulfur two-phase infiltration test is performed by using a phase infiltration testing device comprising an injection system, a core holder 12, a back pressure system, a metering system and a formation simulation system;
the injection system is connected with the input end of the core holder 12, and a first valve 11 and a first pressure gauge 27 are sequentially arranged on a pipeline connected with the injection system; the injection system comprises a gas phase injection pipeline, a liquid sulfur phase injection pipeline and a water phase injection pipeline which are arranged in parallel, wherein the gas phase injection pipeline comprises a nitrogen cylinder 1 and a valve II 2 which are connected in sequence; the liquid sulfur phase injection pipeline comprises a first input pump 3, a third valve 4, a liquid sulfur intermediate container 7 and a fourth valve 9 which are connected in sequence; the water phase injection pipeline comprises a second input pump 5, a fifth valve 6, a water phase intermediate container 8 and a sixth valve 10 which are connected in sequence; optionally, the first input pump 3 and the second input pump 5 both adopt constant-speed constant-pressure pumps;
two ends of the core holder 12 are connected with two detection ends of a resistivity tester 26; optionally, two ends of the core holder 12 are further connected to two detection ends of the differential pressure gauge 25, respectively;
the back pressure system comprises a second pressure gauge 23, a back pressure pump 22 and a back pressure valve 21 which are connected in sequence, the input end of the back pressure valve 21 is connected with the output end of the core holder 12, and a seventh valve 15 and a third pressure gauge 24 are arranged on a pipeline connected in sequence;
the metering system comprises a liquid-liquid separator 20, a liquid sulfur meter 17 and a water meter 19, wherein one output end of the liquid-liquid separator 20 is connected with the liquid sulfur meter 17, a valve eight 16 is arranged on a connected pipeline, the other output end of the liquid-liquid separator 20 is connected with the water meter 19, and a valve nine 18 is arranged on the connected pipeline;
the stratum simulation system comprises a constant temperature box 28 and a confining pressure pump 13, the confining pressure pump 13 is connected with a pressure gauge IV 14, and the output end of the confining pressure pump 13 is connected with the confining pressure input end of the core holder 12; the liquid sulfur intermediate container 7, the water phase intermediate container 8, the first pressure gauge 27, the core holder 12, the third pressure gauge 24, the liquid-liquid separator 20, the liquid sulfur meter 17 and the water meter 19 are all arranged in the thermostat 28.
It should be noted that, in addition to the phase permeation testing apparatus of the above embodiments, the testing method of the present invention can also use other phase permeation testing apparatuses in the prior art to perform a water-liquid sulfur two-phase permeation test.
In a specific embodiment, the steady state method is used for water-liquid sulfur two-phase permeation test, which specifically comprises the following steps:
1. preparing a core: and selecting a corresponding core for extraction, cleaning and drying, and processing and measuring the length, diameter, porosity and permeability of the selected core.
2. Fluid preparation: configuring a corresponding stratum water sample according to the rock core data information, and measuring the viscosity of the stratum water sample under the stratum temperature and the stratum pressure; and selecting corresponding solid sulfur according to the data of the core, heating the solid sulfur to melt the solid sulfur into liquid sulfur when the solid sulfur is used, and calculating the viscosity of the solid sulfur at the formation temperature and under the formation pressure through a liquid sulfur calculation formula.
3. Connection experiment process: connecting the experimental devices, cleaning and checking the connectivity of the pipeline, opening the nitrogen cylinder and checking the air tightness.
4. Calibrating the dead volume: and putting the core into a holder, and calibrating the dead volume in the device.
5. Establishing a high-temperature high-pressure stratum environment: opening a heating device of the thermostat to raise the temperature of the system to 120 ℃ so as to ensure that liquid sulfur cannot be solidified in the pipeline of the device to cause the blockage of the pipeline and the like; and adjusting the confining pressure to a confining pressure value required by a simulated formation through a confining pressure pump so as to establish a temperature pressure environment of the formation.
6. Establishing irreducible water saturation: firstly, opening a second input pump, saturating the selected rock core step by the prepared formation water sample through the second input pump, keeping the confining pressure of each step of saturation to be higher than the internal pressure by 3-5 MPa all the time, stopping when the pressure reaches the target formation pressure, recording the resistivity value on a resistivity tester, and calculating the saturated water quantity under the formation condition; and then closing the second input pump, opening the first input pump, replacing the formation water in the rock core by driving liquid sulfur through the first input pump until no water phase exists in the liquid at the outlet end of the holder, finishing the displacement, recording the resistivity value on the resistivity tester, and calculating the corresponding saturation of the irreducible water.
7. Determination of liquid sulfur permeability at irreducible water saturation: under the condition that the rock core is saturated with water, adjusting the confining pressure pump, adjusting the confining pressure to a target pressure, opening the first input pump, performing liquid sulfur displacement through the first input pump, recording the flow of liquid sulfur after the differential pressure representation number on the rock core holder and the flow of liquid sulfur in the liquid sulfur meter are stable after the volume of displaced liquid sulfur reaches 10 times of the pore volume, and calculating the effective permeability of a liquid sulfur phase; and continuously measuring for three times, finishing the displacement when the relative error is less than 3%, and calculating to determine the effective permeability of the liquid sulfur phase under the saturation of the irreducible water.
8. Determining the effective permeability of the liquid sulphur phase and the aqueous phase at a certain water saturation: under the condition that the rock core is saturated with water, adjusting the confining pressure pump to a target pressure, opening the first input pump and the second input pump, setting different driving speeds, and injecting liquid sulfur and water into the rock core holder in a certain proportion; after the liquid is stabilized, the liquid flows through the holder and then is separated into water and liquid sulfur through a high-temperature and high-pressure resistant liquid-liquid separator, the separated liquid sulfur and water are respectively measured by a fluid meter to determine the flow rate, the inlet pressure and the outlet pressure of the holder and the resistance value of a resistivity tester are recorded, and the displacement is finished; the effective permeability of the aqueous phase, liquid sulfur phase at this water saturation is calculated.
9. Determining the effective permeability of liquid sulfur phase and the effective permeability of water phase under different water saturation degrees: changing the injection proportion of water and liquid sulfur, repeating the experiment step 8, measuring the liquid sulfur and water flow under different water saturation, the inlet and outlet pressure and the resistivity of the clamper, and further calculating to obtain the effective permeability of the water phase and the liquid sulfur phase under different water saturation.
10. And (4) finishing the experimental result, and calculating and drawing a steady-state method water-liquid sulfur two-phase permeation curve.
In this embodiment, the calculation method of each parameter is as follows:
the calculation formula of the water saturation and the liquid sulfur saturation is as follows:
Ss＝1-Sw (5)
in the formula: swThe water saturation of the rock core; ssThe core liquid sulfur saturation is obtained; i is a resistance increase coefficient; rtThe resistivity of the rock core at different water saturation is omega m; r0The resistivity is the resistivity of the rock core at 100% saturated formation water, omega m; b is a constant related to lithology; n is a saturation index;
wherein the n saturation index and the constant b related to the lithology are obtained according to the measured different water saturation and the corresponding resistivity.
Effective permeability of aqueous phase the effective permeability of liquid sulfur phase is calculated by the formula:
in the formula: kwThe effective permeability of the aqueous phase, mD, at each moment; ksThe effective permeability of the liquid sulfur phase at each moment, mD; mu.swIs the viscosity of water at formation conditions, mPa · s; qwIs water flow, cm3/s；QsIs the flow of liquid sulfur, cm3S; l is the core length, cm; a is the cross-sectional area of the core in cm2；P1The pressure at the inlet end of the gripper is MPa; p2The pressure at the outlet end of the gripper is MPa;
the relative permeability of the water phase and the relative permeability of the liquid sulfur phase at each moment are calculated by the following formula:
in the formula: krwRelative permeability of the aqueous phase, mD, at each time; krsRelative permeability of liquid sulfur phase, mD, at each moment; kw(Swi) Absolute permeability of the aqueous phase, mD, at each moment; ks(Ssi) The absolute permeability of the liquid sulfur phase at each time, mD.
In another specific embodiment, the water-liquid sulfur two-phase permeation test is performed by using an unsteady state method, which specifically comprises the following steps:
(1) preparing a core: and selecting a corresponding core for extraction, cleaning and drying, and processing and measuring the length, diameter, porosity and permeability of the selected core.
(2) Fluid preparation: configuring a corresponding stratum water sample according to the rock core data information, and measuring the viscosity of the stratum water sample under the stratum temperature and the stratum pressure; and selecting corresponding solid sulfur according to the data of the core, heating the solid sulfur to melt the solid sulfur into liquid sulfur, and calculating the viscosity of the liquid sulfur at the formation temperature and under the formation pressure by using a liquid sulfur calculation formula.
(3) Connection experiment process: connecting the experimental devices, cleaning and checking the connectivity of the pipeline, opening the nitrogen cylinder and checking the air tightness.
(4) Calibrating the dead volume: and putting the core into a holder, and calibrating the dead volume in the device.
(5) Establishing a high-temperature high-pressure stratum environment: opening a heating device of the thermostat to raise the temperature of the system to 120 ℃ so as to ensure that liquid sulfur cannot be solidified in the pipeline of the device to cause the blockage of the pipeline and the like; and adjusting the confining pressure to a confining pressure value required by a simulated formation through a confining pressure pump so as to establish a temperature pressure environment of the formation.
(6) Establishing irreducible water saturation: firstly, opening a second input pump, saturating the selected rock core step by the prepared formation water sample through the second input pump, keeping the confining pressure of each step of saturation to be higher than the internal pressure by 3-5 MPa all the time, stopping when the pressure reaches the target formation pressure, recording the resistivity value on a resistivity tester, and calculating the saturated water quantity under the formation condition; and then closing the second input pump, opening the first input pump, replacing the formation water in the rock core by driving liquid sulfur through the first input pump until no water phase exists in the liquid at the outlet end of the holder, finishing the displacement, recording the resistivity value on the resistivity tester, and calculating the corresponding saturation of the irreducible water.
(7) Determination of liquid sulfur permeability at irreducible water saturation: under the condition that the rock core is saturated with water, adjusting the confining pressure pump, adjusting the confining pressure to a target pressure, opening the first input pump, performing liquid sulfur displacement through the first input pump, recording the flow of liquid sulfur after the differential pressure representation number on the rock core holder and the flow of liquid sulfur in the liquid sulfur meter are stable after the volume of displaced liquid sulfur reaches 10 times of the pore volume, and calculating the effective permeability of a liquid sulfur phase; and continuously measuring for three times, finishing the displacement when the relative error is less than 3%, and calculating to determine the effective permeability of the liquid sulfur phase under the saturation of the irreducible water.
(8) Saturated liquid sulfur of the core: taking out the rock core of which the liquid sulfur permeability under the irreducible water saturation is measured in the rock core holder, washing sulfur and drying, and then putting back the rock core holder; and opening the first input pump, saturating the selected rock core step by the first input pump, keeping the confining pressure of each step of saturation to be higher than the internal pressure by 3-5 MPa all the time, and stopping when the pressure reaches the target formation pressure.
(9) Determination of the relative permeability of water and liquid sulfur: adjusting the confining pressure pump, adjusting the confining pressure of the clamp to the target pressure, opening the input pump II, and starting displacement at the set displacement speed by using a constant speed method; timing is started when the outlet end of the holder begins to discharge liquid, the water discharge amount, the liquid discharge sulfur amount and the pressure value of a pressure gauge are recorded at regular intervals, the metering is encrypted at the initial stage of water leakage, the recording time interval is changed according to the liquid discharge sulfur amount, and the recording time interval is gradually lengthened along with the continuous decrease of the liquid discharge sulfur amount; when the water content of the effluent reaches 99.5 percent or water is injected for 30 times of pore volume, measuring the water phase permeability under the residual liquid sulfur at the moment, and finishing the displacement; the effective permeability of the aqueous phase, liquid sulfur phase at this water saturation is calculated.
(10) And (4) finishing the experimental result, and calculating and drawing an unsteady-state method water-liquid sulfur two-phase permeation curve.
In this embodiment, the calculation method of each parameter is as follows:
water drive speed calculation formula:
Lμwvw≥1 (10)
in the formula: v iswIs the displacement speed, cm/min;
calculating formulas of water phase relative permeability, liquid sulfur phase relative permeability and water saturation:
in the formula: f. ofs(Sw) Is the liquid sulfur content, expressed in decimal;
the non-dimensional accumulated sulfur yield is expressed by the times of pore volume;
dimensionless cumulative fluid production expressed as a multiple of pore volume; i' is the relative injection capacity, also known as flow capacity ratio; q (t) is the flow rate of the liquid produced at the outlet end face at time t, and Q (t) is Q in the constant-speed tests，cm3/s；Q'sThe sulfur flow rate of the produced liquid in cm is the end face of the core outlet at the initial moment3/s；Δp0Initial driving pressure difference, MPa; Δ p (t) is the displacement pressure difference at time t, MPa; sweThe water saturation of the end face of the core outlet is represented by decimal; swsThe fractional number represents the number of irreducible water saturations.
In a specific example, a core is taken as an example, and a steady state method is adopted to carry out a water-liquid sulfur two-phase infiltration test. The basic parameters of the core I are shown in the table 1:
TABLE 1 core basic parameters
| Length (cm) | Diameter (cm) | Gas porosity (%) | Gas permeability (mD) |
| 5.89 | 2.513 | 16.67 | 435.07 |
The experimental conditions of the phase permeation test are as follows: the confining pressure is 30 MPa; the experimental temperature is 130 ℃; the liquid sulfur viscosity was 9.6209 mPas (obtained by calculation according to the formula (1) of the present invention), and the results of the phase permeation test are shown in Table 2 and FIG. 3:
TABLE 2 core Permeability test results
| Water saturation (%) | Sulfur-containing saturation (%) | Relative permeability K of sulfur phasers | Relative permeability of the aqueous phase Krw |
| 0.2768 | 0.7232 | 1.0000 | 0.0000 |
| 0.3694 | 0.6306 | 0.5237 | 0.0192 |
| 0.4189 | 0.5811 | 0.3754 | 0.0379 |
| 0.4564 | 0.5436 | 0.2650 | 0.0547 |
| 0.5016 | 0.4984 | 0.1924 | 0.0736 |
| 0.5529 | 0.4471 | 0.1230 | 0.1157 |
| 0.6078 | 0.3922 | 0.0722 | 0.1979 |
| 0.6470 | 0.3530 | 0.0502 | 0.2610 |
| 0.6895 | 0.3105 | 0.0319 | 0.3451 |
| 0.7035 | 0.2965 | 0.0252 | 0.3722 |
| 0.7433 | 0.2567 | 0.0107 | 0.5005 |
| 0.7688 | 0.2312 | 0.0032 | 0.5973 |
In another specific example, taking a core two as an example, a steady state method is adopted to perform a water-liquid sulfur two-phase permeability test. The basic parameters of the core two are shown in table 3:
TABLE 3 core two basic parameters
| Length (cm) | Diameter (cm) | Gas porosity (%) | Gas permeability (mD) |
| 3.62 | 2.509 | 7.75 | 63.29 |
The experimental conditions of the phase permeation test are as follows: the confining pressure is 30 MPa; the experimental temperature is 130 ℃; the liquid sulfur viscosity was 9.6209 mPas (obtained by calculation according to the formula (1) of the present invention), and the results of the phase permeation test are shown in Table 4 and FIG. 4:
TABLE 4 core two-phase permeability test results
As can be seen from FIGS. 3 and 4, the sulfur saturation S is dependent on the sulfur contentsIncrease of (2) liquid sulfur phase relative permeability KrsIncrease and relative permeability K of the aqueous phaserwThe decrease is significant, but the relative permeability K of the liquid sulfur phasersRelative permeability K of rising specific water phaserwThe reduction is more obvious; the reason for this is that the water-liquid sulfur co-flow causes interaction and interference of water-liquid sulfur, and when the flow resistance of the water-liquid sulfur co-flow reaches the maximum, the sum of the two-phase permeability of the water-liquid sulfur will be the lowest value.
In conclusion, the invention can obtain more accurate liquid sulfur viscosity according to the formulas (1) to (3), and then obtain a water-liquid sulfur two-phase relative permeation rule by adopting a steady state method or an unsteady state method, so as to provide a theoretical basis for the development of a high-sulfur-content gas reservoir.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. A high-temperature high-pressure water-liquid sulfur two-phase infiltration test method is characterized by comprising the following steps:
s1: preparing a rock core and an experimental fluid, wherein the experimental fluid comprises nitrogen, simulated formation water and liquid sulfur, and calibrating the dead volume of the phase permeation testing device;
s2: establishing a high-temperature high-pressure simulated formation environment;
s3: establishing irreducible water saturation, and determining the liquid sulfur permeability under the irreducible water saturation;
s4: measuring the effective permeability of the liquid sulfur phase and the water phase by adopting a steady state method, or measuring the relative permeability of the water and the liquid sulfur by adopting an unsteady state method;
s5: and (5) finishing the experimental result of the step S4, and calculating and drawing a water-liquid sulfur two-phase permeation curve.
2. The high-temperature high-pressure water-liquid sulfur two-phase infiltration test method according to claim 1, wherein in step S1, when preparing liquid sulfur, corresponding solid sulfur is selected according to the core, and when in use, the solid sulfur is heated and melted into liquid sulfur, and the viscosity of the liquid sulfur at the simulated formation temperature is calculated.
3. The method of claim 2, wherein the viscosity of the liquid sulfur is calculated by the following formula when the simulated formation temperature is less than 160.5 ℃:
μs＝-481.222728445625+19.8512164855695×T+(-0.314248940080241)×T2+0.00245792988973678×T3+(-0.00000955032579659511)×T4+0.0000000147751020559072×T5 (1)
in the formula: mu.ssViscosity of liquid sulfur, mPa · s; t is the formation simulation temperature, DEG C.
4. The method for testing high temperature and high pressure water-liquid sulfur two-phase cementation according to claim 2, wherein when the simulated formation temperature is equal to or higher than 160.5 ℃ and equal to or lower than 187.575 ℃, the viscosity of the liquid sulfur is calculated by the following formula:
in the formula: mu.ssViscosity of liquid sulfur, mPa · s; t is the formation simulation temperature, DEG C.
5. The method for testing high temperature and high pressure water-liquid sulfur two-phase infiltration according to claim 2, wherein when the simulated formation temperature is greater than 187.575 ℃ and less than 314 ℃, the viscosity of the liquid sulfur is calculated by the following formula:
in the formula: mu.ssViscosity of liquid sulfur, mPa · s; t is the formation simulation temperature, DEG C.
6. The method for testing high temperature and high pressure water-liquid sulfur two-phase permeability according to claim 1, wherein in step S4, when the effective permeability of the liquid sulfur phase and the aqueous phase is determined by a steady state method, the effective permeability of the liquid sulfur phase and the aqueous phase at different water saturation levels is determined.
7. The method for testing the two-phase permeability of high temperature and high pressure water-liquid sulfur according to claim 1, wherein in step S4, when the relative permeability of water and liquid sulfur is determined by the unsteady state method, the core is saturated with liquid sulfur, and then water flooding is performed to determine the relative permeability of water and liquid sulfur.
8. The high-temperature high-pressure water-liquid sulfur two-phase infiltration testing method according to any one of claims 1 to 7, characterized in that in step S1, the phase infiltration testing device comprises an injection system, a core holder, a back pressure system, a metering system and a formation simulation system;
the injection system is connected with the input end of the core holder, and a first valve and a first pressure gauge are sequentially arranged on a pipeline connected with the injection system; the injection system comprises a gas phase injection pipeline, a liquid sulfur phase injection pipeline and a water phase injection pipeline which are arranged in parallel, wherein the gas phase injection pipeline comprises a nitrogen cylinder and a valve II which are connected in sequence; the liquid sulfur phase injection pipeline comprises a first input pump, a third valve, a liquid sulfur intermediate container and a fourth valve which are connected in sequence; the water phase injection pipeline comprises an input pump II, a valve V, a water phase intermediate container and a valve VI which are connected in sequence;
two ends of the rock core holder are connected with two detection ends of the resistivity tester;
the back pressure system comprises a second pressure gauge, a back pressure pump and a back pressure valve which are sequentially connected, the input end of the back pressure valve is connected with the output end of the core holder, and a seventh valve and a third pressure gauge are sequentially arranged on a pipeline connected with the back pressure valve;
the metering system comprises a liquid-liquid separator, a liquid-sulfur meter and a water meter, wherein one output end of the liquid-liquid separator is connected with the liquid-sulfur meter, a valve eighth is arranged on a connected pipeline, the other output end of the liquid-liquid separator is connected with the water meter, and a valve ninth is arranged on the connected pipeline;
the stratum simulation system comprises a constant temperature box and a confining pressure pump, the confining pressure pump is connected with a pressure gauge IV, and the output end of the confining pressure pump is connected with the confining pressure input end of the core holder; the liquid sulfur intermediate container, the water phase intermediate container, the first pressure gauge, the rock core holder, the third pressure gauge, the liquid-liquid separator, the liquid sulfur meter and the water meter are all arranged in the thermostat.
9. The high-temperature high-pressure water-liquid sulfur two-phase infiltration test method according to claim 8, characterized in that two ends of the core holder are respectively connected with two detection ends of a pressure difference meter.
10. The method for testing the two-phase infiltration of high temperature and high pressure water-liquid sulfur according to claim 8, wherein the first input pump and the second input pump both use constant-speed and constant-pressure pumps.
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