CN107907464B - Device and method for measuring performance of permeable stone cement slurry for fracturing - Google Patents
Device and method for measuring performance of permeable stone cement slurry for fracturing Download PDFInfo
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- CN107907464B CN107907464B CN201711099895.9A CN201711099895A CN107907464B CN 107907464 B CN107907464 B CN 107907464B CN 201711099895 A CN201711099895 A CN 201711099895A CN 107907464 B CN107907464 B CN 107907464B
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- 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
Abstract
The invention discloses a permeable rock cement slurry performance measuring device and method for fracturing, belongs to the technical field of energy, and is characterized in that formation conditions are accurately simulated by a measuring method to measure important parameters of cement slurry such as density, viscosity, fluidity, water loss, free water content, initial setting time, final setting time, compressive strength, permeability, porosity, damage degree to a reservoir and the like, comprehensive data are accurately analyzed, characteristics of the cement slurry in a rock stratum are objectively reflected, the device and method have important significance for formation energy development, convenient experimental operation is provided through a performance measuring device, and more accurate experimental data are collected.
Description
Technical Field
The invention belongs to the technical field of energy, and particularly relates to a research on a method for measuring the performance of permeable stone cement slurry for fracturing reformation of a reservoir of a compact oil and gas field, in particular to a device and a method for measuring the performance of permeable stone cement slurry for fracturing.
Background
The compact oil-gas reservoir belongs to unconventional oil-gas reservoirs, has huge development potential, is mainly reformed by a hydraulic fracturing mode at present, and is developed for the compact oil reservoir, however, the hydraulic fracturing has the defects of large construction scale, high construction pressure, large consumption of manpower, material resources and water resources, great harm to the reservoir, serious environmental pollution of flowback liquid and the like.
The permeable stone is used for replacing conventional fracturing liquid with high-density cement slurry to perform fracturing modification on a reservoir, and has the characteristic of high liquid column pressure, so that the construction pressure is greatly reduced; a large amount of sand carrying liquid is not required to be prepared, and the water consumption is greatly reduced; reverse discharge is not needed after fracturing, and environmental pollution is avoided; high-strength cement-stone supported cracks with high permeability are formed, and the yield increasing effect is obvious.
In order to guarantee the construction effect after fracturing, the real environment of a reservoir needs to be simulated in a laboratory, the permeable rock system is comprehensively and accurately evaluated, and meanwhile, corresponding matched experimental facilities are needed, so that the experimental process is smoother, the experimental efficiency is improved, and the experimental data is more accurate.
Disclosure of Invention
The invention aims to provide a permeable rock cement slurry performance measuring device and method for fracturing.
The technical scheme adopted by the invention for solving the technical problems is as follows: the utility model provides a fracturing is with infiltration stone cement paste capability test device, includes gas cylinder, needle valve, manometer, tee bend, basin, advection pump, force pump, hand wheel, graduated flask, electronic scale, its characterized in that: the gas cylinders are three and respectively comprise a nitrogen cylinder, a methane cylinder and a carbon dioxide cylinder, the gas cylinders are connected in parallel, each gas cylinder is connected with a needle valve and a pressure gauge, the gas cylinders are connected with a middle container through a tee joint, the number of the middle containers is four, the middle containers are arranged in parallel through the tee joint, the two ends of each middle container are provided with the needle valves, the needle valves are arranged between the middle containers which are connected in parallel, the two ends of each advection pump are respectively connected with a water tank and the middle container, the needle valves are arranged between the advection pumps and the middle containers, the two ends of each middle container which are connected in parallel are respectively connected with a steel cup and the tee joint through the needle valves, the steel cups are connected with a rock core holder and a pressure pump through pipelines, the rock core holder is provided with the three pressure gauges, and the rock core holder is connected with the pressure pump through the needle valves, the core holder is also connected with a gas float flowmeter and a measuring cup through pipelines.
A method for measuring the performance of permeable stone cement slurry for fracturing sequentially comprises the following steps:
(1) preparing experimental slurry, preparing STS-1 slurry, adding 45 parts by volume of distilled water and 100 parts by volume of phosphoaluminate cement into a container, and uniformly stirring for later use; preparing STS-1 liquid, adding 50 parts by volume of distilled water into a container for later use;
(2) detecting the basic performance of the STS-1 slurry, measuring the density, viscosity, fluidity, water loss amount, free water content, initial setting time, final setting time and compressive strength of the STS-1 slurry at 25 ℃ and normal pressure, and recording; measuring the density, viscosity, fluidity, water loss, free water content, initial setting time, final setting time and compressive strength of the STS-1 slurry at 50 ℃ and normal pressure, and recording;
(3) measuring the initial water-phase permeability of the rock core,
① packing a tight sandstone core with the diameter of 25 multiplied by 40 ~ 60mm into a core holder;
② ring-pressing the core under 25MPa, back-pressing the end of the core holder under 5MPa, opening the temperature control system, adjusting the heating temperature to 50 deg.C, and heating for 4 hr;
③, pumping distilled water into the core holder, and recording the pressure difference delta p1 before and after the pressure difference before and after the core holder is stable, and the displacement Q1 of the pump at the moment;
(4) measuring the gas-phase permeability of the core CO2, measuring the initial gas-phase permeability of the core by using supercritical CO2, pumping supercritical CO2 into the core holder, and recording the pressure difference delta p2 before and after the pressure difference before and after the holder is stable and the discharge Q2 of the pump at the moment;
(5) measuring the gas-phase permeability of the core CH4, measuring the initial gas-phase permeability of the core by using a supercritical CH4, pumping and injecting supercritical CH4 into the core holder, and recording the pressure difference delta p3 before and after the pressure difference before and after the holder is stable and the discharge capacity Q3 of the pump at the moment;
(6) the manufacture of the permeable stone sample is carried out,
① applying ring pressure to the core holder to 35MPa, injecting STS-1 slurry and liquid into the core holder at a discharge rate of 3:1 (ratio of STS-1 slurry to STS-1 liquid by volume), applying ring pressure to the core holder to make the pressure inside the core holder reach 30MPa, closing the valve, keeping the temperature at 50 ℃ unchanged, and waiting for setting for 72 h;
② opening an outlet valve of the core holder after the initial setting time is reached, injecting high-pressure nitrogen into the core holder for replacement, and closing the outlet valve to continue waiting for setting when the pressure difference between the front and the back of the holder is less than 25 MPa;
③ maintaining the temperature at 50 deg.C and the pressure at 30MPa, and curing the penetrated stone for 72 hr;
(7) measuring gas-phase permeability of permeant rock CO2, measuring the gas-phase permeability of the permeant rock by using supercritical CO2, reducing the ring pressure of the core holder to 25MPa, opening an outlet valve of the core holder, pumping supercritical CO2 into the core holder, and recording the pressure difference delta p4 before and after the pressure difference before and after the holder is stable and the discharge Q4 of the pump at the moment;
(8) measuring gas-phase permeability of permeastone CH4, measuring the gas-phase permeability of the permeastone by using supercritical CH4, pumping CH4 into the core holder, and recording the pressure difference delta p5 before and after the pressure difference before and after the holder is stable and the discharge capacity Q5 of the pump at the moment;
(9) measuring the secondary liquid phase permeability of the rock core, pumping distilled water into the rock core holder, and recording the pressure difference delta p6 before and after the pressure difference before and after the rock core holder is stable, and the discharge capacity Q6 of the pump at the moment;
(10) measuring the gas phase permeability of secondary CO2 of the rock core, pumping supercritical CO2 into the rock core holder, and recording the pressure difference delta p7 before and after the pressure difference before and after the rock core holder is stable and the discharge capacity Q7 of the pump at the moment;
(11) measuring the secondary CH4 gas-phase permeability of the core, pumping supercritical CH4 into the core holder, and recording the pressure difference delta p8 before and after the pressure difference before and after the core holder is stable and the discharge Q8 of the pump at the moment;
(12) slicing, namely taking the permeable stone sample out of the core holder, and measuring the porosity of the permeable stone sample by using a slicing method;
(13) measuring the compressive strength of the permeable stone sample;
(14) all permeabilities involved in the above experiments were calculated, and the core damage rate was calculated.
Preferably, the measuring cup is placed on the surface of the electronic scale, two needle valves and a tee joint are arranged between the rock core holder and the measuring cup, and the tee joint is connected with the gas flowmeter through the needle valves and a pipeline.
Preferably, the structure of the intermediate container is the same as that of the hydraulic cylinder.
As optimization, the core holder is also provided with a temperature control system.
The optimized STS-1 slurry is prepared from 45 parts by volume of distilled water, 5 parts by volume of sulfate and 100 parts by volume of phosphoaluminate cement, and the STS-1 liquid is prepared from 50 parts by volume of distilled water and 5 parts by volume of carbonate.
The invention has the beneficial effects that: compared with the prior art, the device and the method for measuring the performance of the permeable stone cement slurry for fracturing are characterized in that different types of air sources are provided by the air cylinders in the measuring device, different intermediate containers are used for injecting different media into an experimental object by matching the intermediate containers with a constant flow pump, so that mutual disturbance does not occur in the experimental process, the media flow path of the device is simply adjusted by opening and closing needle valves at different positions, the ring pressure of the core clamping device is more conveniently and accurately adjusted by adjusting the pressure pump through a hand wheel, and accurate measurement of liquid is realized by matching a measuring cup with an electronic balance; the method has the advantages that the formation conditions are accurately simulated by the measuring method to measure important parameters of the cement paste such as density, viscosity, fluidity, water loss, free water content, initial setting time, final setting time, compressive strength, permeability, porosity, damage degree to a reservoir and the like, the comprehensive data are accurately analyzed, the characteristics of the cement paste in the rock stratum are objectively reflected, and the method has important significance for the development of formation energy.
Drawings
FIG. 1 is a view showing the construction of a performance chart measuring apparatus according to the present invention;
wherein, 1 gas cylinder, 2 middle containers, 3 needle valves, 4 pressure gauges, 5 three-way valves, 6 water tanks, 7 advection pumps, 8 steel cups, 9 gas float flowmeters, 10 core holders, 11 pressure pumps, 12 hand wheels, 13 measuring cups and 14 electronic scales.
Detailed Description
In the process of measuring the performance of the penetrated stone cement paste, the following method is adopted:
(1) preparing experimental slurry, preparing STS-1 slurry, adding 45 parts by volume of distilled water and 100 parts by volume of phosphoaluminate cement into a container, and uniformly stirring for later use; preparing STS-1 liquid, adding 50 parts by volume of distilled water into a container for later use;
(2) detecting the basic performance of the STS-1 slurry, measuring the density, viscosity, fluidity, water loss amount, free water content, initial setting time, final setting time and compressive strength of the STS-1 slurry at 25 ℃ and normal pressure, and recording; the density, viscosity, fluidity, water loss, free water content, initial setting time, final setting time and compressive strength of STS-1 slurry at 50 ℃ and normal pressure are measured and recorded, and the temperature is adjusted to simulate the use environment of the permeable stone cement slurry due to different reservoir environment conditions at different depths, so that the obtained data is more in line with the actual situation and is beneficial to being used as corresponding reference in the construction of reservoir at different depths;
(3) measuring the initial water-phase permeability of the rock core,
① packing a tight sandstone core with the diameter of 25 multiplied by 40 ~ 60mm into a core holder;
② ring pressing 25MPa to the core, adding 5Mpa back pressure to the end of the core holder, opening the temperature control system, adjusting the heating temperature to 50 deg.C, heating for 4 hours, because there is a certain temperature and pressure gradient in the reservoir, the indoor test must be done by pressurizing and heating to simulate the reservoir environment, 50 deg.C simulates 1000m-1500m underground, different geological conditions, different temperature gradients, so the well depths corresponding to the temperatures of different reservoirs are different;
③, pumping distilled water into the core holder, and recording the pressure difference delta p1 before and after the pressure difference before and after the core holder is stable, and the displacement Q1 of the pump at the moment;
(4) measuring the gas-phase permeability of the core CO2, measuring the initial gas-phase permeability of the core by using supercritical CO2, pumping supercritical CO2 into the core holder, and recording the pressure difference delta p2 before and after the pressure difference before and after the holder is stable and the discharge Q2 of the pump at the moment;
(5) measuring the gas-phase permeability of the core CH4, measuring the initial gas-phase permeability of the core by using a supercritical CH4, pumping and injecting supercritical CH4 into the core holder, and recording the pressure difference delta p3 before and after the pressure difference before and after the holder is stable and the discharge capacity Q3 of the pump at the moment;
(6) the manufacture of the permeable stone sample is carried out,
① applying ring pressure to 35MPa to the core holder, injecting STS-1 slurry and liquid (namely permeable stone cement slurry) into the core holder according to the displacement of 3:1 (the volume proportion of STS-1 slurry to STS-1 liquid), applying ring pressure to the core holder to make the internal pressure of the core holder reach 30MPa, closing the valve, keeping the temperature at 50 ℃ unchanged, and waiting for setting for 72 h;
② opening the outlet valve of the core holder after reaching the initial setting time (30 min-120 min), i.e. opening the needle valve to release the pressure, injecting high-pressure nitrogen into the core holder for replacement, and closing the outlet valve to continue waiting for setting when the pressure difference between the front and the back of the holder is less than 25 MPa;
③ maintaining the temperature at 50 deg.C and the pressure at 30MPa, and curing the penetrated stone for 72 hr;
(7) measuring gas-phase permeability of permeant rock CO2, measuring the gas-phase permeability of the permeant rock by using supercritical CO2, reducing the ring pressure of the core holder to 25MPa, opening an outlet valve of the core holder, pumping supercritical CO2 into the core holder, and recording the pressure difference delta p4 before and after the pressure difference before and after the holder is stable and the discharge Q4 of the pump at the moment;
(8) measuring gas-phase permeability of permeastone CH4, measuring the gas-phase permeability of the permeastone by using supercritical CH4, pumping CH4 into the core holder, and recording the pressure difference delta p5 before and after the pressure difference before and after the holder is stable and the discharge capacity Q5 of the pump at the moment;
(9) measuring the secondary liquid phase permeability of the rock core, pumping distilled water into the rock core holder, and recording the pressure difference delta p6 before and after the pressure difference before and after the rock core holder is stable, and the discharge capacity Q6 of the pump at the moment;
(10) measuring the gas phase permeability of secondary CO2 of the rock core, pumping supercritical CO2 into the rock core holder, and recording the pressure difference delta p7 before and after the pressure difference before and after the rock core holder is stable and the discharge capacity Q7 of the pump at the moment;
(11) measuring the secondary CH4 gas-phase permeability of the core, pumping supercritical CH4 into the core holder, and recording the pressure difference delta p8 before and after the pressure difference before and after the core holder is stable and the discharge Q8 of the pump at the moment;
(12) slicing, taking out the permeable rock sample from the core holder, measuring the porosity of the permeable rock sample by using a slicing method, cutting the core into a standard core which is convenient to calculate and test, wherein the standard core has the specification that the diameter is about 2.5cm, and the axial-diameter ratio is 2 ~ 3;
(13) measuring the compressive strength of the permeable stone sample;
(14) calculating all permeability rates involved in the above experiments, calculating core damage rate by using data collected in the experiments,
wherein K is gas permeability mD, and A is rock sample sectional area cm2L is the length cm, Q of the rock sample0Is flow rate cm at atmospheric pressure3S (gas), P1、P2The pressure Mpa, P is the pressure of the inlet and outlet of the rock core0The atmospheric pressure is 0.1Mpa, and the mu is gas viscosity mPa.s; the calculation formula of the core damage rate is as follows: core damage rate = (initial core permeability-post damage core permeability)/initial core permeability 100%); or using the collected data to calculate the core damage rate,wherein A is the cross-sectional area cm of the rock sample2L is the length cm of the rock sample, Q is the flow rate cm under atmospheric pressure3The method comprises the following steps of (i) per second (liquid), wherein delta P is the pressure difference Mpa between the inlet and the outlet of the rock core, mu is the viscosity of the liquid mPa.s, and the calculation formula of the damage rate of the rock core is as follows: core damage rate = (initial core permeability-post damage core permeability)/initial core permeability 100%).
In another embodiment, STS-1 slurry is prepared by adding 45 parts by volume of distilled water and 5 parts by volume of sulfate into a preparation vessel, dissolving them sufficiently, adding 100 parts of phosphoaluminate cement, stirring uniformly for use, preparing STS-2 liquid, adding 50 parts by volume of distilled water and 5 parts by volume of carbonate into another preparation vessel, and stirring sufficiently for use. The STS-1 slurry is mixed to form a permeable stone cement slurry. The permeability of the adjusted permeable stone cement slurry in a simulation experiment is better, and the permeable stone cement slurry is more suitable for stratum fracturing.
In the embodiment shown in fig. 1, a device for measuring the performance of permeable stone cement slurry for fracturing comprises an air bottle 1, a needle valve 3, a pressure gauge 4, a tee joint 5, a water tank 6, a constant flow pump 7, a pressure pump 11, a hand wheel 12, a measuring cup 13 and an electronic scale 14, and is characterized in that: the gas cylinder 1 is provided with three nitrogen cylinders, a methane cylinder and a carbon dioxide cylinder, the gas cylinders 1 are connected in parallel, each gas cylinder 1 is connected with a needle valve 3 and a pressure gauge 4, the gas cylinders 1 are connected with an intermediate container 2 through a tee joint 5, the number of the intermediate containers 2 is four, the intermediate containers 2 are arranged in parallel through the tee joint 5, the two ends of the intermediate container 2 are provided with the needle valves 3, the needle valves 3 are arranged between the intermediate containers 2 which are connected in parallel, the two ends of the advective pump 7 are respectively connected with a water tank 6 and the intermediate container 2, the needle valves 3 are arranged between the advective pump 7 and the intermediate container 2, the two ends of the intermediate container 2 which are connected in parallel are respectively connected with a steel cup 8 and a tee joint 5 through the needle valves 3, the steel cup 8 is connected with a rock core holder 10 and a pressure pump 11 through pipelines, the core holder 10 is provided with three pressure gauges 4, the core holder 10 is connected with a pressure pump 11 through a needle valve 3, the core holder 10 is further connected with a gas float flowmeter 9 and a measuring cup 13 through pipelines, the structure of the middle container 2 is the same as that of a hydraulic cylinder, the core holder 10 is further provided with a temperature control system, all patterns with the same structure in the drawing are the same, and the reason that no mark is given is that the drawing is clearer.
The structure of the intermediate container 2 is the same as that of a traditional hydraulic cylinder, in the using process of the intermediate container 2, it needs to be noted that the intermediate container 2 uses water as a power supply medium, a single gas is used as a compressed medium, for example, when nitrogen needs to be injected into the core holder 10, a nitrogen cylinder (gas cylinder 1) is fixedly injected into one of the intermediate containers 2 through opening and closing of different needle valves 3, the other intermediate containers 2 are closed by valves to avoid polluting the other intermediate containers 2, the needle valves of the nitrogen cylinder are closed after the gas is injected, the needle valves 3 at the bottom of the intermediate container 2 are opened, water is injected into the intermediate container 2 through a advection pump 7, the needle valves 3 at the top of the intermediate container 2 and the needle valves 3 at other relevant parts are opened, and the nitrogen is pressed into the core holder 10 by utilizing the pressure of water to match with the structure of the intermediate container 2. Other gases are injected by a similar method, and the gases enter the core holder 10 in a high-pressure mode through the opening and closing of the needle valve 3, and meanwhile, the experimental data are not accurate due to the fact that the gases are mixed. It should be noted that the intermediate container 2 used when the core holder 10 needs to be filled with water is of a conventional barreled construction, since the hydraulic medium and the test medium are identical.
The use of a layer energy measuring device is introduced by combining a permeable stone cement slurry performance measuring method,
measuring the initial water phase permeability of the rock core in the step (3),
① packing a tight sandstone core with the diameter of 25 multiplied by 40 ~ 60mm into a core holder;
② ring-pressing the core at 25MPa, back-pressing the end of the core holder at 5MPa, driving the pressure pump 11 by hand wheel 12, applying ring-pressing to the core holder to 25MPa by using the water absorbed from the steel cup as pressure medium, applying 5MPa pressure to the outlet, opening the temperature control system, adjusting the heating temperature to 50 deg.C, heating for 4 hours;
③ pumping distilled water into the core holder, the distilled water passing through the water tank 6, the advection pump 7, the middle container 2, the core holder 10, after the pressure difference between the front and the back of the core holder is stable, observing the pressure situation through two pressure gauges 4 at the front and the back of the core holder 10, recording the pressure difference delta p1 between the front and the back, and the displacement Q1 of the pump, the displacement being measured by the measuring cup 13, the distilled water flowing through the core holder 10 being a dynamic process, in a simple point, when the system is in a stable state, the distilled water continuously flows out, the outlet pressure and the outlet pressure of the holder will not change at this time, the pressure difference between the front and the back = the inlet pressure-the outlet pressure being a fixed value, the volume of the distilled water flowing out of the holder in a certain time is also basically constant, that is, the displacement;
step (4), measuring the gas-phase permeability of the rock core CO2, measuring the initial gas-phase permeability of the rock core by using supercritical CO2, pumping supercritical CO2 into the rock core holder, injecting high-pressure water into the middle container 2 by using carbon dioxide through a gas cylinder 1 (a carbon dioxide gas cylinder) -a tee joint 5-the middle container 2, closing a related needle valve 3 and injecting the high-pressure water into the middle container 2 through a constant flow pump 7, so that the carbon dioxide is injected from the middle container 2-the rock core holder 10, observing the pressure condition through two pressure meters 4 in front of and behind the rock core holder 10 after the front-back pressure difference of the holder is stable, recording the front-back pressure difference delta p2, and measuring the discharge capacity Q2 of the pump at the moment;
step (5), measuring the gas-phase permeability of the rock core CH4, measuring the initial gas-phase permeability of the rock core by using a supercritical CH4, pumping supercritical CH4, a methane gas cylinder 1 (methane gas cylinder) -three-way valve 5-another intermediate container 2 into the rock core holder, closing a related needle valve 3, injecting high-pressure water into the intermediate container 2 by using a constant flow pump 7, observing the pressure condition by using two pressure gauges 4 in front of and behind the rock core holder 10 after the front-back pressure difference of the holder is stabilized, recording the front-back pressure difference delta p3, and measuring the discharge capacity of the pump Q3 at the moment, and finishing the discharge capacity measurement by using gas through the rock core holder 10-a gas float flowmeter 9;
step (6) manufacturing a permeating stone sample,
①, applying ring pressure to the core holder to 35MPa, driving a pressure pump 11 through a hand wheel 12, applying ring pressure to the core holder to 35MPa by taking water sucked from a steel cup as a pressure medium, injecting STS-1 slurry and liquid into the core holder at a discharge capacity of 3:1 (ratio of STS-1 slurry to STS-1 liquid by volume), applying ring pressure to the core holder to make the internal pressure of the core holder reach 30MPa, closing a valve, keeping the temperature at 50 ℃ unchanged, waiting for setting for 72h, wherein the internal pressure refers to pump grouting liquid to make the internal pressure of the core holder reach 30MPa, and waiting for setting for 72 h;
②, after the initial setting time is reached, opening an outlet valve (needle valve 3) of the core holder, injecting high-pressure nitrogen into the core holder for replacement, closing the relevant needle valve 3, injecting high-pressure water into the middle container 2 through an air bottle 1 (nitrogen bottle) -tee joint 5-another middle container 2 through a constant-current pump 7 to enable the nitrogen to flow from the middle container 2 to the core holder 10, observing the pressure condition through two pressure gauges 4 at the front and the back of the core holder 10 until the pressure difference at the front and the back of the holder is less than 25MPa, and closing the outlet valve to continue to wait for setting;
③ maintaining the temperature at 50 deg.C and the pressure at 30MPa, and curing the penetrated stone for 72 hr;
step (7), determining gas phase permeability of permeable rock CO2, determining the gas phase permeability of the permeable rock by using supercritical CO2, reducing the ring pressure of the core holder to 25MPa, opening an outlet valve of the core holder, pumping supercritical CO2 into the core holder, injecting high-pressure water into the middle container 2 through a gas cylinder 1 (a carbon dioxide gas cylinder) -tee joint 5-another middle container 2 by closing a related needle valve 3 through a advection pump 7 to inject the carbon dioxide into the middle container 2 through the middle container 2-the core holder 10, observing the pressure condition through two pressure meters 4 at the front and the back of the core holder 10 after the front and the back of the holder are stable, recording the front and the back pressure difference delta p4, and measuring the discharge capacity Q4 of the pump at the moment through a measuring cup 13;
step (8), determining gas phase permeability of the permeance stone CH4, determining the gas phase permeability of the permeance stone by using supercritical CH4, pumping methane from the middle container 2 to the core holder 10 through the gas cylinder 1 (methane gas cylinder) -tee joint 5-middle container 2, closing the related needle valve 3, and injecting high-pressure water into the middle container 2 through the advection pump 7, pumping CH4 into the core holder, observing the pressure condition through two pressure gauges 4 at the front and the back of the core holder 10, and recording the pressure difference delta p5 at the front and the back of the core holder after the pressure difference at the front and the back of the holder is stable, and the discharge Q5 of the pump at the moment;
measuring the secondary liquid phase permeability of the rock core, pumping distilled water into the rock core holder, wherein the distilled water passes through a water tank 6, a constant-current pump 7, an intermediate container 2 and the rock core holder 10, observing the pressure condition through two pressure gauges 4 in front of and behind the rock core holder 10 after the front-back pressure difference of the rock core holder is stable, and recording the front-back pressure difference delta p6 and the discharge capacity Q6 of the pump;
step (10) measuring the gas-phase permeability of secondary CO2 of the rock core, and injecting high-pressure water into the middle container 2 through a gas cylinder 1 (a carbon dioxide gas cylinder) -tee joint 5-another middle container 2 through a pipeline, closing a related needle valve 3, and injecting high-pressure water into the middle container 2 through a constant-flow pump 7, so that the oxidation tower pumps supercritical CO2 into the rock core holder from the middle container 2 to the rock core holder 10, observing the pressure condition through two pressure meters 4 in front of and behind the rock core holder 10, and recording the front-back pressure difference delta p7 and the discharge Q7 of the pump when the front-back pressure difference of the rock core holder is stable;
step (11) measuring the secondary CH4 gas-phase permeability of the rock core, and injecting high-pressure water into the middle container 2 through a gas cylinder 1 (a methane gas cylinder) -tee joint 5-middle container 2, closing a related needle valve 3, and injecting the high-pressure water into the middle container 2 through a constant-flow pump 7 to pump methane from the middle container 2-a rock core holder 10 to the rock core holder 10, and injecting supercritical CH4 into the rock core holder, observing the pressure condition through two pressure gauges 4 in front of and behind the rock core holder 10 after the front-back pressure difference of the rock core holder is stable, and recording the front-back pressure difference delta p8 and the discharge Q8 of the pump at the moment;
the above embodiments are only specific cases of the present invention, and the protection scope of the present invention includes but is not limited to the product form and style of the above embodiments, and any suitable changes or modifications of the apparatus and method for measuring the properties of the permeable rock cement slurry for fracturing according to the claims of the present invention should fall within the protection scope of the present invention.
Claims (5)
1. The use method of the permeable stone cement slurry performance measuring device for fracturing is characterized in that: the permeable stone cement slurry performance testing device for fracturing comprises gas cylinders, needle valves, pressure gauges, three-way valves, a water tank, a constant-flow pump, a pressure pump, a hand wheel, a measuring cup and an electronic scale, wherein the three gas cylinders are respectively a nitrogen cylinder, a methane cylinder and a carbon dioxide cylinder, the gas cylinders are connected in parallel, each gas cylinder is connected with the needle valve and the pressure gauge, the gas cylinders are connected with an intermediate container through three-way pipes, the number of the intermediate containers is four, the intermediate containers are arranged in parallel through the three-way pipes, the needle valves are arranged at two ends of the intermediate container, the needle valves are arranged between the intermediate containers in parallel, the two ends of the constant-flow pump are respectively connected with the water tank and the intermediate container, the needle valves are arranged between the constant-flow pump and the intermediate container, the two ends of the intermediate container in parallel connection are respectively connected with the steel cup and the three-way pipes, the steel cup is connected with the core holder and the pressure pump through pipelines, three pressure gauges are arranged on the core holder, the core holder is connected with the pressure pump through a needle valve, and the core holder is also connected with a gas float flowmeter and a measuring cup through pipelines;
the use method of the permeable stone cement slurry performance measuring device for fracturing comprises the following steps:
(1) preparing experimental slurry, preparing STS-1 slurry, adding 45 parts by volume of distilled water and 100 parts by volume of phosphoaluminate cement into a container, and uniformly stirring for later use; preparing STS-1 liquid, and adding 50 parts by volume of distilled water into a container for later use;
(2) detecting the basic performance of the STS-1 slurry, measuring the density, viscosity, fluidity, water loss amount, free water content, initial setting time, final setting time and compressive strength of the STS-1 slurry at 25 ℃ and normal pressure, and recording; measuring the density, viscosity, fluidity, water loss, free water content, initial setting time, final setting time and compressive strength of the STS-1 slurry at 50 ℃ and normal pressure, and recording;
(3) measuring the initial water-phase permeability of the rock core,
① packing a tight sandstone core with the diameter of 25 multiplied by 40 ~ 60mm into a core holder;
② ring-pressing the core under 25MPa, back-pressing the end of the core holder under 5MPa, opening the temperature control system, adjusting the heating temperature to 50 deg.C, and heating for 4 hr;
③, pumping distilled water into the core holder, and recording the pressure difference delta p1 before and after the pressure difference before and after the core holder is stable, and the displacement Q1 of the pump at the moment;
(4) measuring the gas-phase permeability of the core CO2, measuring the initial gas-phase permeability of the core by using supercritical CO2, pumping supercritical CO2 into the core holder, and recording the pressure difference delta p2 before and after the pressure difference before and after the holder is stable and the discharge Q2 of the pump at the moment;
(5) measuring the gas-phase permeability of the core CH4, measuring the initial gas-phase permeability of the core by using a supercritical CH4, pumping and injecting supercritical CH4 into the core holder, and recording the pressure difference delta p3 before and after the pressure difference before and after the holder is stable and the discharge capacity Q3 of the pump at the moment;
(6) the manufacture of the permeable stone sample is carried out,
①, applying ring pressure to the core holder to 35MPa, injecting STS-1 slurry and liquid into the core holder according to the volume ratio of 3:1 of STS-1 slurry to STS-1 liquid, applying ring pressure to the core holder to make the internal pressure of the core holder reach 30MPa, closing a valve, keeping the temperature at 50 ℃ unchanged, and waiting for setting for 72 hours;
② opening an outlet valve of the core holder after the initial setting time is reached, injecting high-pressure nitrogen into the core holder for replacement, and closing the outlet valve to continue waiting for setting when the pressure difference between the front and the back of the holder is less than 25 MPa;
③ maintaining the temperature at 50 deg.C and the pressure at 30MPa, and curing the penetrated stone for 72 hr;
(7) measuring gas-phase permeability of permeant rock CO2, measuring the gas-phase permeability of the permeant rock by using supercritical CO2, reducing the ring pressure of the core holder to 25MPa, opening an outlet valve of the core holder, pumping supercritical CO2 into the core holder, and recording the pressure difference delta p4 before and after the pressure difference before and after the holder is stable and the discharge Q4 of the pump at the moment;
(8) measuring gas-phase permeability of permeastone CH4, measuring the gas-phase permeability of the permeastone by using supercritical CH4, pumping CH4 into the core holder, and recording the pressure difference delta p5 before and after the pressure difference before and after the holder is stable and the discharge capacity Q5 of the pump at the moment;
(9) measuring the secondary liquid phase permeability of the rock core, pumping distilled water into the rock core holder, and recording the pressure difference delta p6 before and after the pressure difference before and after the rock core holder is stable, and the discharge capacity Q6 of the pump at the moment;
(10) measuring the gas phase permeability of secondary CO2 of the rock core, pumping supercritical CO2 into the rock core holder, and recording the pressure difference delta p7 before and after the pressure difference before and after the rock core holder is stable and the discharge capacity Q7 of the pump at the moment;
(11) measuring the secondary CH4 gas-phase permeability of the core, pumping supercritical CH4 into the core holder, and recording the pressure difference delta p8 before and after the pressure difference before and after the core holder is stable and the discharge Q8 of the pump at the moment;
(12) slicing, namely taking the permeable stone sample out of the core holder, and measuring the porosity of the permeable stone sample by using a slicing method;
(13) measuring the compressive strength of the permeable stone sample;
(14) all permeabilities involved in the above experiments were calculated, and the core damage rate was calculated.
2. The use method of the apparatus for measuring the properties of the permeable stone cement slurry for fracturing as claimed in claim 1, wherein: the measuring cup is placed on the surface of the electronic scale, two needle valves and a tee joint are arranged between the rock core holder and the measuring cup, and the tee joint is connected with the gas flowmeter through the needle valves and a pipeline.
3. The use method of the apparatus for measuring the properties of the permeable stone cement slurry for fracturing as claimed in claim 1, wherein: the structure of the middle container is the same as that of the hydraulic cylinder.
4. The use method of the apparatus for measuring the properties of the permeable stone cement slurry for fracturing as claimed in claim 1, wherein: the core holder is also provided with a temperature control system.
5. The use method of the apparatus for measuring the properties of the permeable stone cement slurry for fracturing as claimed in claim 1, wherein: the STS-1 slurry comprises, by volume, 45 parts of distilled water, 5 parts of sulfate and 100 parts of phosphoaluminate cement, and the STS-1 liquid comprises, by volume, 50 parts of distilled water and 5 parts of carbonate.
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| CN111693429A (en) * | 2020-02-20 | 2020-09-22 | 南通华兴石油仪器有限公司 | Fluid positive and negative displacement device and using method thereof |
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