CN115961940A - DNA @ SiO 2 Application method of tracer and simulated sample column - Google Patents
DNA @ SiO 2 Application method of tracer and simulated sample column Download PDFInfo
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- CN115961940A CN115961940A CN202210930677.XA CN202210930677A CN115961940A CN 115961940 A CN115961940 A CN 115961940A CN 202210930677 A CN202210930677 A CN 202210930677A CN 115961940 A CN115961940 A CN 115961940A
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Abstract
The application provides a simulation tracing method of a multi-fracture rock stratum and a multi-fracture simulation sample column, which relate to the technical field of oil and gas development, and the method comprises the following steps: providing a multi-fracture rock sample column and a tracer; rock stratum samples are filled in the multi-fracture rock sample column; one end of the multi-crack rock sample column is provided with a first port and a second port; the side surface of the multi-crack rock sample column is provided with at least three tracer injection ports; injecting water into the multi-crack rock sample column from the first port, and infiltrating and washing the rock sample; injecting a tracer into the multi-fracture rock sample column by using the tracer injection port; injecting a displacement fluid into the multi-fracture rock sample column from the second port, and collecting an effluent liquid of the first port to obtain a tracer sample; acquiring the content of a tracer in a tracer sample; wherein each tracer injection port injects a different one of the tracers. The application also provides a multi-crack simulation sample column. The method can solve the technical problem that a single fracture core sample in the prior art is difficult to reflect the seepage condition of the multi-fracture rock formation fluid.
Description
Technical Field
The application relates to the technical field of oil and gas development, in particular toDNA @ SiO 2 Application method of tracer and its analog sample column.
Background
Staged fracturing is a core technology for shale gas development, and the accurate productivity monitoring of the stratified stages of fractures after fracturing construction is the most important content for evaluating the fracturing effect. The tracer technology is one of the most accurate current oil and gas reservoir fracture monitoring methods, has decisive significance for capacity evaluation of shale gas development and overall adjustment of construction schemes, has high actual rock stratum tracing difficulty and high requirement, and is difficult to be suitable for capacity estimation and planning requirements of construction schemes, so that in the oil and gas development process, a rock core sample laboratory physical simulation technology is often adopted to simulate to obtain rock core data, and a basis is provided for oil and gas development. Therefore, the validity of data obtained by physical simulation of a core sample laboratory is very important before and at the beginning of oil and gas development. However, after fracturing construction, a plurality of fractures often exist in a fractured rock stratum, the distribution of the fractures is complex, and conventional rock stratum sample laboratory physical simulation and conventional tracers are difficult to reflect the fluid seepage condition of each layer section in the actual fractured rock stratum, so that the effectiveness of the obtained simulation data is reduced, and the capacity estimation and the construction scheme drawing are not facilitated.
Disclosure of Invention
The purpose of the present application is to provide a DNA @ SiO 2 The application method of the tracer improves the technical problems that the conventional rock stratum sample laboratory physical simulation and the conventional tracer in the prior art are difficult to react with the fluid seepage condition of each layer section in the actual fracture rock stratum.
It is another object of the present application to provide a multi-fracture simulation sample column for a multi-fracture formation.
In order to achieve the purpose, the application provides the following technical scheme:
the embodiment of the application provides a DNA @ SiO 2 An application method of the tracer comprises the following steps:
providing a fissured rock sample column and a plurality of DNA @ SiO 2 A tracer; the fractured rock sample column is provided with at least three tracer injection ports;
using the tracer injection portInjecting DNA @ SiO into the fissured rock sample column 2 A tracer;
regularly obtain the drained tracer sample of the fissure rock sample, measure each DNA @ SiO in the tracer sample 2 The content of the tracer;
according to the DNA @ SiO 2 Acquiring the contribution rate of the fracture fluid production in a unit time period by the content of the tracer and the discharge time;
wherein the unit time period is a time period between two acquisitions of the drained tracer samples of the fractured rock sample.
Further, in some embodiments of the present application, the contribution of the fracture fluid is calculated by the following formula:
wherein M is i Mass (g) of tracer used for time period i in the flowback fluid; n is the number of times of obtaining the discharged tracer sample of the multi-fracture rock sample, and n is a positive integer; i is the serial number of the tracer sample discharged from the multi-crack rock sample obtained at a certain time, and i is a natural number from 1 to n;
wherein M is i ＝∑(C i ·t)·v；
Wherein, C i Concentration of tracer used for the ith time period in flowback fluid (g/m) 3 )；
t is the required calculated fluid production profile time period (h);
v is the drainage rate (m) 3 /h)。
Further, in some embodiments of the present application, the fractured rock sample column is a single fractured rock sample column or a multi fractured rock sample column.
Further, in some embodiments of the present application, the fractured rock sample column is filled with a rock sample; one end of the fractured rock sample column is provided with a first port, and the other end of the fractured rock sample column is provided with a second port; the tracer injection port is arranged on the side face of the fractured rock sample column;
using the tracer injection opening to the fractured rock sampleInjection of DNA @ SiO into the column 2 A tracer, comprising:
injecting water into the fractured rock sample column from the first port, and infiltrating and washing the rock sample;
using the DNA @ SiO 2 Injecting the DNA @ SiO into the fractured rock sample column through a tracer injection port 2 A tracer;
injecting a displacement fluid into the fractured rock sample column from the second port, and collecting an effluent liquid of the first port to obtain a tracer sample;
obtaining each DNA @ SiO in the tracer sample 2 The tracer content.
Further, in some embodiments of the present application, each of the tracer injection ports injects the same concentration of the active ingredient for tracing in the tracer.
Further, in some embodiments of the present application, injecting water into the multi-fracture rock sample column from the first port, infiltrating and flushing the rock sample comprises:
and injecting water into the fractured rock sample column from the first port at the flow rate of 3-6 mL/min, and infiltrating and washing the rock stratum sample for 15-60 min.
Further, in some embodiments of the present application, injecting a displacement fluid into the fractured rock sample string from the second port comprises:
and injecting a displacement fluid into the multi-fracture rock sample column from the second port at a flow rate of 2.5-5 mL/min.
Further, in some embodiments of the present application, collecting effluent from the first port comprises:
collecting effluent liquid of the first port regularly and quantitatively; wherein the interval time between two adjacent times of collection is 0.5-2 min.
Further, in some embodiments of the present application, when the fractured rock sample string is a multi-fractured rock sample string, the formation sample is provided with a plurality of primary fractures; the main fracture corresponds to the tracer injection port.
The application also provides a multi-fracture simulation sample column of a multi-fracture rock formation, comprising: the device comprises a shell, a plurality of tracer injection holes and a plurality of tracer injection holes, wherein an accommodating cavity is formed in the shell, and the tracer injection holes are communicated with the accommodating cavity and are used for injecting different tracers; openings are also formed in the two ends of the shell; and a sealed end; the sealing ends comprise a first sealing end and a second sealing end, and the first sealing end and the second sealing end are respectively connected with the openings at the two ends of the shell in a sealing manner; the first sealing end is provided with a first port for injecting/discharging fluid; the second sealed end is provided with a second port for injecting/discharging fluid.
The application provides a DNA @ SiO 2 An application method of a tracer comprises the steps of taking a crack sample as a core sample, and injecting DNA @ SiO with different concentrations into different positions on the core sample 2 The tracer agent is used for simulating the flowback process of the tracer agent, the fracturing fluid output curve can be obtained by intensively collecting flowback liquid of each interval according to the flowback of the tracer agent, the characteristics of the tracer agent output curve are observed, the contribution rate of the fracture in the simulation experiment of the fracture rock stratum is further obtained, and effective data are provided for the prediction of the analysis of the staged fracturing fracture fluid output; the method improves the relationship between flowback of each interval in the existing rock stratum sample laboratory physical simulation and the time which is difficult to react by the conventional tracer, and fully reacts the seepage of the tracer in the fracture sample.
The multi-fracture simulation sample column for the multi-fracture rock stratum is simple in structure and easy to operate, and can overcome the defect that the sample column in the prior art is difficult to react on the fluid seepage condition of the multi-fracture rock stratum.
Drawings
In order to more clearly illustrate the detailed description of the present application or the technical solutions in the prior art, the drawings needed to be used in the detailed description of the present application or the prior art description will be briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present application, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a schematic diagram of a multi-fracture simulation sample column for a multi-fracture formation according to an embodiment of the present disclosure;
FIG. 2 is a schematic diagram of a multi-fracture simulation sample column of a multi-fracture rock formation according to an embodiment of the present disclosure for infiltrating, flushing, and injecting a tracer during multi-fracture sample simulation;
FIG. 3 is a schematic diagram of a multi-fracture simulation sample column of a multi-fracture rock formation flowback during multi-fracture sample simulation provided by an embodiment of the present disclosure;
FIG. 4 is a standard curve of a nano tracer T1 provided in the examples of the present application;
FIG. 5 is a standard curve of a nano tracer T2 provided in the examples of the present application;
FIG. 6 is a standard curve of a nano tracer T3 provided in the examples of the present application;
fig. 7 is a graph showing output curves of the nano tracer T1, the nano tracer T2, and the nano tracer T3 in the multi-fracture core sample according to the embodiment of the present disclosure;
fig. 8 shows the productivity contribution rates of a fracture 1, a fracture 2, and a fracture 3 in a multi-fracture core sample provided in the embodiment of the present application;
wherein 1-shell, 11-first port, 12-second port, 13-tracer injection port, 2-containing cavity.
Detailed Description
The technical solutions of the present application will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are some, but not all embodiments of the present application. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
In a first aspect, an embodiment of the present application provides a method for simulating and tracing a multi-fracture rock formation, including:
providing a fissured rock sample column and a plurality of DNA @ SiO 2 A tracer; the fractured rock sample column is provided with at least three tracer injection ports;
injecting DNA @ SiO into the fractured rock sample column by using the tracer injection port 2 A tracer;
regularly obtain the drained tracer sample of the crack rock sample, measure each DNA @ SiO in the tracer sample 2 The content of the tracer;
according to the DNA @ SiO 2 Acquiring the contribution rate of the fracture fluid production in a unit time period by the content of the tracer and the discharge time;
wherein the unit time period is a time period between two acquisitions of the drained tracer samples of the fractured rock sample.
Wherein each of the tracer injection ports injects a different one of the tracers. Each tracer injection port injects the same concentration of the effective component for tracing in the tracer.
In some embodiments, the fractured rock sample column is a single fractured rock sample column or a multi fractured rock sample column. When the fractured rock sample column is a single fractured rock sample column, the application can research DNA @ SiO 2 The influence of the tracer on a single-section output curve under different displacement speeds is researched to research the influence of DNA @ SiO 2 The tracer and the exposed DNA tracer trace the characteristics of a production curve, so that the relation between the flow-back liquid of each layer section and time and displacement speed is researched, and effective reference data is provided for capacity estimation and the planning of a construction scheme; furthermore, DNA @ SiO 2 The tracer utilizes the excellent characteristics of DNA, solves the bottleneck problem of the current tracer technology in the development application of shale gas, expands the traditional oil field tracer from a molecule and ion system with single function to a DNA tracer system, increases the quantity of the tracer, and utilizes the coded DNA to independently mark the number of layers and the number of sections of the layered fracturing, thereby pertinently solving the key technical problem of the development of the shale gas. When the fracture rock sample post is many fracture rock sample post, the application that this application provided can also be based on the peak area of tracer output curve, judges the cracked oil gas output rate of multistage.
It should be noted that after obtaining the tracer content in the tracer sample, the method further includes:
according to the content of the tracer in each tracer sample and the sampling time, adopting normalized C/C 0 And (5) drawing a production curve of the tracer.
In performing the analysis, further comprising establishing a standard curve for the tracer. The standard curve of the tracer was established by the fluorescence qPCR method.
And drawing a production curve of the tracer after measurement according to fluorescence qPCR.
It should be noted that in the present application, the difference of injecting the tracer into each tracer injection port should be understood as: the DNA in the tracer injected by each tracer injection port is different, so that the respective content of various tracers in each tracer sample can be distinguished according to the fluorescence qPCR test, and the influence on the test result caused by the difference of the viscosity, the flow rate and the like of the conventional different tracers can be avoided.
In some embodiments, DNA @ SiO as used herein 2 The tracer can be a tracer whose tracer components are modified nanosilica and the dsDNA solution. Wherein, the modified nano silicon dioxide can be modified nano silicon dioxide obtained by modifying nano silicon dioxide with positive charge modifier solution.
Wherein the positive charge modifier solution can be alcohol containing 1-6 carbon atoms, such as ethanol, isopropanol, methanol; or trimethoxysilylpropyl-N, N, N-trimethylammonium chloride.
In some embodiments, the concentration of the effective component injected into the tracer for tracing is the same through each tracer injection port, so that the variables are reduced, and the accuracy of the simulation result is improved.
In some embodiments, the contribution of the fracture fluid is calculated by the following formula:
wherein M is i Mass (g) of tracer used for time period i in the flowback fluid; n is the number of times of obtaining the discharged tracer sample of the multi-fracture rock sample, and n is a positive integer; i is the serial number of the trace sample discharged from the multi-crack rock sample obtained at a certain time, and i is a natural number from 1 to n;
wherein M is i ＝∑(C i ·t)·v；
Wherein, C i Concentration of tracer used for i time period in flowback fluid (g/m) 3 )；
t is the required calculated fluid production profile time period (h);
v is the drainage rate (m) 3 /h)。
In some embodiments, the fractured rock sample column is filled with a rock formation sample; one end of the fractured rock sample column is provided with a first port, and the other end of the fractured rock sample column is provided with a second port; the tracer injection port is arranged on the side face of the fractured rock sample column;
injecting DNA @ SiO into the fractured rock sample column by using the tracer injection port 2 A tracer, comprising:
injecting water into the fractured rock sample column from the first port, and infiltrating and washing the rock sample;
using the DNA @ SiO 2 Injecting the DNA @ SiO into the fractured rock sample column through a tracer injection port 2 A tracer;
injecting a displacement fluid into the fractured rock sample column from the second port, and collecting an effluent liquid of the first port to obtain a tracer sample;
obtaining each DNA @ SiO in the tracer sample 2 The tracer content.
In some embodiments, the water is selected from any one of formation water, distilled water, deionized water, pure water, ultrapure water; and/or
The displacement fluid is selected from any one of formation water, distilled water, deionized water, pure water and ultrapure water.
The water is preferably ultrapure water and the displacement fluid is preferably the same as the water.
In some embodiments, injecting water into the multi-fracture rock sample column from the first port, infiltrating and flushing the rock sample comprises:
and injecting water into the fractured rock sample column from the first port at the flow rate of 3-6 mL/min, and infiltrating and washing the rock stratum sample for 15-60 min.
Preferably, water is injected into the multi-fracture rock sample column from the first port at a flow rate of 5mL/min, and the rock sample is infiltrated and washed for 30min.
In some embodiments, injecting a displacement fluid into the fractured rock sample string from the second port comprises:
and injecting a displacement fluid into the multi-fracture rock sample column from the second port at the flow rate of 2.5-5 mL/min.
Preferably, a displacement fluid is injected into the multi-fractured rock sample column from the second port at a flow rate of 4 mL/min.
In some embodiments, collecting effluent from the first port comprises:
collecting effluent liquid of the first port at fixed time and quantity; wherein the interval time between two adjacent times of collection is 0.5-2 min.
In some embodiments, the rock stratum sample is obtained by filling 40-70 meshes of quartz sand in a segmented mode, and effective supporting and sealing of fractures of a fractured interval can be achieved.
In some embodiments, when the fractured rock sample string is a multi-fractured rock sample string, the formation sample is provided with a plurality of primary fractures; the main fracture corresponds to the tracer injection port.
The present application also provides a multi-fracture simulation sample column for a multi-fracture formation, referring to fig. 1, comprising: the device comprises a shell 1, wherein a containing cavity 2 is arranged in the shell 1, and a plurality of tracer injection ports 13 which are communicated with the containing cavity 2 and are used for injecting different tracers are arranged on the shell 1; openings are also formed at two ends of the shell 1; and a sealed end; the sealing ends comprise a first sealing end and a second sealing end, and the first sealing end and the second sealing end are respectively connected with the openings at the two ends of the shell in a sealing manner; the first sealed end is provided with a first port 11 for injecting/discharging fluid; the second sealed end is provided with a second port 12 for the injection/outflow of fluid.
The application also provides a DNA @ SiO 2 Preparation method of tracer, DNA @ SiO adopted in this application 2 The tracer may be introduced into the reaction vessel byThe following method is adopted to obtain:
providing a nano-silica solution, a dsDNA solution, a positive charge modifier solution and a polymer solution;
mixing the positive charge modifier solution and the nano-silica solution, and modifying the surface potential of the nano-silica by using the positive charge modifier to obtain modified nano-silica;
mixing the modified nano-silica and the dsDNA solution to enable the dsDNA to be attached to the modified nano-silica, and separating to obtain binding particles;
mixing the combined particles and the polymer solution to enable the polymer to be attached to the combined particles, and separating to obtain template particles;
by using
And growing silicon dioxide on the template particles, and separating to obtain the nano tracer.
Wherein, the nano-silica solution can be an alcoholic solution of nano-silica, and the solvent of the nano-silica solution is selected from alcohols containing 1 to 6 carbon atoms, such as ethanol, isopropanol and methanol, and is used for dispersing the nano-silica, which is helpful for avoiding the agglomeration of silica particles. The positive charge modifier solution is an alcoholic solution of the positive charge modifier, and the solvent of the positive charge modifier solution is selected from alcohols containing 1-6 carbon atoms, such as ethanol, isopropanol and methanol.
The dsDNA solution may be, among others, an ultra-pure aqueous solution of dsDNA. The polymer solution is an aqueous solution of a polymer, and the solvent water used in the polymer solution can be pure water, ultrapure water, deionized water and the like.
Wherein the particle size range of the nano silicon dioxide is 70-100 nm.
In some embodiments, after mixing the positive charge modifier solution and the nanosilica solution, the volume ratio of alcohol as solvent to positive charge modifier is from 100.
In some embodiments, the modified nanosilica has a surface potential from +25mV to +35mV.
In some embodiments, mixing the positive charge modifier solution and the nanosilica solution comprises:
and mixing the positive charge modifier solution and the nano silicon dioxide solution for 10-16 h at the rotating speed of 500-1500 rad/min.
In some embodiments, the positive charge modifier solution and the nanosilica solution are mixed for 10 to 16 hours, after separation, the precipitate is re-dissolved with isopropanol before separation, and this operation is repeated at least once to obtain the modified nanosilica.
When the precipitate is dissolved again by using isopropanol, ultrasonic treatment is carried out for 2-5 min in ultrasonic equipment to disperse and dissolve the precipitate, and then separation is carried out.
In some embodiments, the modified nanosilica is stored dispersed in isopropanol.
In some embodiments, the concentration of the positive charge modifier in the positive charge modifier solution is 30 to 60wt% in mass fraction; and/or
The mass of the positive charge modifier is 0.01-0.02% of that of the nano silicon dioxide; and/or
The concentration of the nano silicon dioxide in the nano silicon dioxide solution is 30-60 mg/mL.
In some embodiments, the positive charge modifier is trimethoxysilylpropyl-N, N-trimethylammonium chloride.
In some embodiments, mixing the modified nanosilica and the dsDNA solution comprises:
providing a first solvent; the first solvent is selected from alcohols containing 1 to 6 carbon atoms;
mixing the first solvent and the modified nano-silica to obtain a modified nano-silica suspension;
and mixing the dsDNA solution and the modified nano-silica suspension for 3-8 min at the rotating speed of 500-1500 rad/min.
In some embodiments, the concentration of said dsDNA in said dsDNA solution is 30 to 60 μ g/mL; and/or
The concentration of the modified nano silicon dioxide in the modified nano silicon dioxide is 30-60 mg/mL; and/or
The mass ratio of the dsDNA to the modified nano-silica is 0.01-0.02: 1.
in some embodiments, the bound particles are washed at least once with ultrapure water and separated by centrifugation.
In some embodiments, mixing the binding particles and the polymer solution comprises:
mixing the binding particles and the polymer solution at a rotation speed of 500-1500 rad/min for 10-30 min;
wherein the concentration of the polymer in the polymer solution is 15 to 30wt% in terms of mass fraction.
In some embodiments, the polymer is poly (diallyldimethylammonium chloride).
In some embodiments, the poly (diallyldimethylammonium chloride) has a weight average molecular weight of 200000 to 350000.
In some embodiments, the present separation can be achieved by centrifugation.
In some embodiments, mixing the binding particles and the polymer solution for 10 to 30min, separating, comprising:
centrifugally mixing the combined particles and the polymer solution for 10-30 min, and carrying out solid-liquid separation to obtain a crude product;
washing the crude product by using ultrapure water, centrifuging, and separating to obtain a second centrifugal product;
dispersing the second centrifugal product by using a surfactant, and mixing for 10-30 min at the rotating speed of 500-1500 rad/min; and washing with ultrapure water and ethanol for at least one time in sequence to obtain the template particles.
In some embodiments, the surfactant is selected from polyvinylpyrrolidone, further selected from polyvinylpyrrolidone with a weight average molecular weight of 8000 to 12000.
In some embodiments, the concentration of the second centrifugation product in a solution of the second centrifugation product and the surfactant is between 0.05mg/mL and 0.2mg/mL.
In some embodiments, use is made of
A method of growing silica on said template particles comprising:
providing a second solvent, tetraethoxysilane and a catalyst;
and mixing the template particles, the second solvent, tetraethoxysilane and the catalyst for 6-16 h at the rotating speed of 500-1500 rad/min, and separating to obtain the nano tracer.
In some embodiments, the second solvent is a mixed solution of ethanol and water, wherein the volume ratio of ethanol to water is 4.0 to 4.5:1; further 4.3:1.
in some embodiments, the catalyst is an acid, such as acetic acid.
In some embodiments, the volume fraction of tetraethoxysilane in a solution formed from acetic acid, a second solvent and tetraethoxysilane is between 5% and 10%.
In some embodiments, the volume fraction of acetic acid in the solution formed by acetic acid, the second solvent, and tetraethoxysilane is between 1% and 3%.
In some embodiments, the nano tracer is obtained by centrifugal separation after being washed at least once by ethanol, ultrapure water and isopropanol in sequence.
In some embodiments, the nanotracer is stored dispersed in isopropanol.
The application also provides a nano tracer which is prepared by adopting the tracing method of the nano tracer provided by the application.
It is noted that the nano tracer is spherical or spheroidal.
It should be noted that the simulation tracing method for multi-fracture rock formation provided by the present application may also be applied with other commercially available dna @ sio 2 The tracer is used as a tracer, and the tracer used does not need to depend on the DNA @ SiO prepared by the application 2 The tracer can play a role in comparisonImproved results over the prior art, but the DNA @ SiO provided in the present application 2 The technical effect of the tracer is improved more significantly because:
DNA @ SiO prepared by the preparation method provided by the application 2 The tracer utilizes the positive charge modifier to modify the potential of the nano-silica, then dsDNA molecules and polymers are attached to the modified nano-silica to obtain template particles serving as templates, and the template particles are obtained by
Growing silicon dioxide on the template particles to obtain the DNA nano tracer agent coated by the silicon dioxide, so that the product has controllable appearance, controllable particle size and better uniformity; meanwhile, because the DNA molecules and the silicon dioxide nano particles can generate electrostatic repulsion, the DNA molecules are difficult to load on the surfaces of the silicon dioxide nano particles, the silicon dioxide surfaces are modified into positive charges by using a surface modifier, the DNA is easy to load on the surfaces of the silicon dioxide nano particles, and a strong cationic surfactant (TMAPS) is easy to react with hydroxyl on the surfaces of the silicon dioxide nano particles to generate amido bonds after being hydrolyzed in water, so that the DNA molecules and the silicon dioxide nano particles are bonded on the surfaces of the silicon dioxide nano particles; in addition, one end quaternary amine group of the TMAPS molecule is positively charged and can be used as a charge layer for adsorbing DNA molecules; the positively charged polymer PDADMAC and neutral PVP are thus attached on top of the particles in a layer-by-layer manner, to lighten the negatively charged DNA and promote the growth of the silica; while the stratified polymer deposition allows the solvent to pass from water to ethanol, thus avoiding the agglomeration of silica and finally passing through->
The hydrolysis acid is catalyzed, the silicon dioxide grows on the PVP uniformly to form nano particles with uniform particle size distribution, so that the DNA @ SiO is obtained 2 The tracer is relatively excellent in appearance and particle size, is non-toxic and environment-friendly, has no background value and no biological heredity in the environment, and is more favorable for improving the effectiveness of data.
In order to make the details and operation of the above-mentioned implementation of the present application clearly understood by those skilled in the art, and to make the advanced performance of the nano tracer and the tracing method of the nano tracer provided in the embodiments of the present application significantly manifest, the above-mentioned technical solution is exemplified by the following embodiments.
Examples
Preparing a tracer:
s11 mixing 18mL of ethanol, 0.8mL (25 wt.%) of ammonia solution and 0.5mL of Maldili-QH in a 50mL conical tube 2 O, and 0.8mL TEOS is added. The mixture was shaken at 900rpm/min and kept at room temperature (25 ℃) for 6h;
s12, centrifuging the mixture at room temperature for 20min and discarding the supernatant;
s13, the precipitate is suspended with 20mL of isopropanol (the tube is vortexed for a few seconds and sonicated in a water bath for 5 min);
s14, repeating the steps S12 and S13, centrifuging the tube for 20min at room temperature at 9,000g;
s15, suspending the precipitate in 4mL of isopropanol to obtain nano-silica particles (50 mg/mL).
S21, adding 40-80 mu L of TMAPS (50 wt.% methanol solution) solution into 4mL (50 mg/mL) of nano silicon dioxide obtained in the step 1;
s22, stirring the mixture at the room temperature of 900rpm/min for 12 hours;
s23, centrifuging the tube for 4min at room temperature and removing a supernatant;
s24-suspend the pellet in 4mL isopropanol (vortex tube for a few seconds and sonicate in bath for 3 min);
s25, repeating the steps S23 and S24, suspending the precipitate in 4mL of isopropanol and storing at room temperature. The surface potential of the modified nano silicon dioxide is about +25mV to +35mV.
S31 in Milli-Q H 2 Preparing dsDNA solution with the concentration of 50 mu g/mL in O;
s32. In order to bind the first dsDNA fragment formed by SEQ ID No. 1 and the corresponding SEQ ID No. 2 to the particle surface, 55. Mu.L of the modified particle suspension (50 mg/mL) was mixed with 0.5mL of a 50. Mu.g/mL solution of the first dsDNA fragment in a centrifuge tube and shaken for 5min;
s33, using Milli-Q H 2 The DNA bound particles were washed once, centrifuged for 4min and the supernatant discarded.
S41 addition of 1mL of 1mg/mL Poly (diallyldimethylammonium chloride) solution (PDADMAC, 20wt.% in H) to silica DNA binding particles 2 MW200,000-350,000g/mol, sigma-Aldrich) to deposit a first layer, the polymer being attached to the particles. After shaking at 900rpm for 20min at room temperature, the mixture was shaken with Milli-Q H 2 Washing the particles twice;
s42 redisperse the particles in 2mL of 0.1mg/mL poly (vinylpyrrolidone) solution (PVP, MW 10,000g/mol, sigma-Aldrich). Shaking at 900rpm for 20min at room temperature, and sequentially adding Milli-Q H 2 Washing with ethanol once;
s43 in acid catalysis
Reaction (0.25mL EtOH, 58. Mu.L H 2 O,22 μ L Tetraethoxysilane (TEOS), 5 μ L10M acetic acid). The reaction mixture was shaken (900 rpm) for 10h. The particles were then washed once with ethanol, milli-QH 2 And washing once by using O, washing once by using isopropanol, and finally dispersing in 1mL of isopropanol to obtain the nano tracer T1.
Replacing the first dsDNA fragment with a second dsDNA fragment formed from SEQ ID No. 3 and corresponding SEQ ID No. 4 using the steps S11 to S43 above; obtaining the nano tracer T2.
Replacing the first dsDNA fragment with a third dsDNA fragment formed from SEQ ID No. 5 and SEQ ID No. 6 corresponding thereto, using the steps of S11 to S43 above; obtaining the nano tracer T3.
Preparing a multi-fracture core sample:
taking a multi-crack column with the total length of 25.0cm, the inner diameter of 3.0cm and the length of a small crack end of 3.0cm, filling dry 40-70-mesh quartz sand by a segmented sand filling method to obtain a multi-crack core sample, wherein the parameters of the multi-crack core sample obtained by filling are shown in table 1.
TABLE 1
Drawing a standard curve:
the preparation concentrations are 3.66mg/L and 3.66 x 10 respectively -1 mg/L、3.66×10 -2 mg/L、3.66×10 -3 mg/L、3.66×10 -4 mg/L；4.00×10 -1 mg/L、4.00×10 -2 mg/L、4.00×10 -3 mg/L、4.00×10 -4 mg/L、4.00×10 -5 mg/L；4.30×10 -1 mg/L、4.30×10 -2 mg/L、4.30×10 -3 mg/L、4.30×10 -4 mg/L、4.00×10 - 5 measuring the concentration of DNA of mg/L nano tracer T1, nano tracer T2 and nano tracer T3 by a fluorescence qPCR method, and adopting normalized C/C 0 And drawing standard curves of the nano tracer T1, the nano tracer T2 and the nano tracer T3, as shown in FIGS. 4 to 6, wherein the amplification efficiencies of the obtained T1, T2 and T3 tracers are respectively 0.9406, 1.0425 and 1.1013.
Simulation:
referring to FIGS. 2 and 3, the two ends of the multi-split column were connected to a pump, and ultrapure water was injected from the first port to the second port of the column at 5mL/min to wet and rinse the single-split column for 30min;
and (3) injection process: stopping the pump, and respectively adding 30.6mg of the T1, T2 and T3 tracers into the first tracer injection port, the second tracer injection port and the third tracer injection port;
the direction of ultrapure water injection is switched, and the pump is connected with the second port of the slit. And (4) displacing at the speed of 4mL/min, and injecting ultrapure water from the second port to the first port so as to simulate the flowback condition of the tracer in the flowback stage. Collecting effluent from the first port. Every 0.5mL of the effluent was used as a sample to determine the DNA content. Since the fluorescence spectrophotometer cannot distinguish the concentrations of three DNAs, fluorescence qPCR was used to monitor DNA @ SiO in flowback fluid 2 The content of tracer. Experimental results DNA @ SiO adopting normalized C/C0 2 A production curve of the tracer; as shown in fig. 7; and the obtained tracer characterization results are shown in table 2.
TABLE 2
As can be seen from FIGS. 4-6, the concentrations of the T1, T2 and T3 tracers were 3.66X 10 -4 -3.66mg/L、4.00×10 -4 -4.00×10 -1 mg/L and 4.30X 10 -4 -4.30×10 -1 In mg/L, R 2 0.9972, 0.9952 and 0.9966 respectively, and the linear correlation is good.
As can be seen from tables 1 and 2: the breakthrough sequence of the cracks in the multi-crack core sample is from T1 to T2 to T3, and the breakthrough time is 0.8min, 2.0min and 3.5min respectively. The outflow sequence of the three tracers is consistent with the positions of the tracer placement fractures (the positions are 6.0cm, 12.0cm and 18.0cm respectively) of the experimental design. The output curves of the tracer T1, the tracer T2 and the tracer T3 respectively reflect the information of the fracture 1, the fracture 2 and the fracture 3. The peak heights of T1, T2 and T3 were 5.8X 10 -2 min -1 、5.3×10 -2 min -1 、2.7×10 -2 min -1 The T1 tracer diffuses and perturbs less in the fracture, and the T3 tracer diffuses and perturbs more in the fracture resulting in a lower peak value. The peak heights/peak widths of T1, T2 and T3 were respectively 2.6X 10 -2 min、3.5×10 -2 min、0.4×10 -2 min, it can be assumed that the main flow channel of the T2 is narrowest and the main flow channel of the T1 tracer is widest.
Further, according to the above results, the inventors also utilized the above formula of the flow-back contribution ratio:
the productivity contribution rates of the three fractures per 0.5min were calculated, and the calculation results are shown in table 3 and fig. 8.
TABLE 3
As can be seen from Table 3 and FIG. 8: because the injection directions of the three tracers are different, the contribution of each fracture is different, and the total contribution rate content of the fracture 1, the fracture 2 and the fracture 3 is 44.2%, 36.6% and 19.1% respectively; within 0-1.5min, the produced liquid mainly comes from No. 1 crack, and the contribution rates are 91.2%, 91.5% and 84.9% respectively; the contribution rate of crack No. 2 gradually increases with time; fracture No. 3 contributes less in a multi-stage fracture column. Within 2.0-3.5min, the main liquid production part is No. 2 crack, the contribution rate is 67.5%, 70.9% and 41.2%, the contribution rate of the No. 2 crack is gradually reduced along with the time, and the contribution rate of the No. 3 crack is gradually increased along with the time. Until 3.5-5.0min, the main production fluid comes from the No. 3 fracture, the contribution rates are 64.7%, 86.5%, 85.0% and 80.2%, and the contribution rates of the No. 2 fracture and the No. 3 fracture are gradually reduced. In a multi-stage fracturing experiment, the tracing contribution of each time period is evaluated by the tracing curves of T1, T2 and T3, and the DNA @ SiO is proved 2 The tracer has the potential in analyzing the fluid contribution of the staged fracturing fracture. Therefore, the multi-fracture tracing method provided by the application can be used for more clearly and more according with the actual contribution rate of each fracture in the multi-fracture, and more effective reference data can be provided for the development of the fractured shale gas rock stratum.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solutions of the present application, and not to limit the same; although the present application has been described in detail with reference to the foregoing embodiments, it should be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present application.
Claims (10)
1. DNA @ SiO 2 The application method of the tracer is characterized by comprising the following steps:
providing a fissured rock sample column and a plurality of DNA @ SiO 2 A tracer; the fractured rock sample column is provided with at least three tracer injection ports;
injecting DNA @ SiO into the multi-crack rock sample column by utilizing the tracer injection port 2 TracingAn agent;
regularly obtain the drained tracer sample of the fissure rock sample, measure each DNA @ SiO in the tracer sample 2 The content of the tracer;
according to the DNA @ SiO 2 Acquiring the contribution rate of the fracture fluid production in a unit time period by the content of the tracer and the discharge time;
wherein the unit time period is a time period between two acquisitions of the drained tracer samples of the fractured rock sample.
2. DNA @ SiO according to claim 1 2 The application method of the tracer is characterized in that the contribution rate of the fracture fluid is calculated by the following formula:
wherein M is i Mass (g) of tracer used for the ith time period in the flowback fluid; n is the number of times of obtaining the discharged tracer sample of the multi-fracture rock sample, and n is a positive integer; i is the serial number of the tracer sample discharged from the multi-crack rock sample obtained at a certain time, and i is a natural number from 1 to n;
wherein, M i ＝∑(C i ·t)·v；
Wherein, C i Concentration of tracer used for i time period in flowback fluid (g/m) 3 )；
t is the required calculated fluid production profile time period (h);
v is the drainage rate (m) 3 /h)。
3. DNA @ SiO according to claim 1 2 The application method of the tracer is characterized in that the fractured rock sample column is a single-fractured rock sample column or a multi-fractured rock sample column.
4. DNA @ SiO according to claim 1 2 The application method of the tracer is characterized in that a rock stratum sample is filled in the fractured rock sample column; the cracksOne end of the rock sample column is provided with a first port, and the other end of the rock sample column is provided with a second port; the tracer injection port is arranged on the side face of the fractured rock sample column;
injecting DNA @ SiO into the fractured rock sample column by utilizing the tracer injection port 2 A tracer, comprising:
injecting water into the fractured rock sample column from the first port, and infiltrating and washing the rock sample;
using the DNA @ SiO 2 Injecting the DNA @ SiO into the fractured rock sample column through a tracer injection port 2 A tracer;
injecting a displacement fluid into the fractured rock sample column from the second port, and collecting an effluent liquid of the first port to obtain a tracer sample;
obtaining each DNA @ SiO in the tracer sample 2 The tracer content.
5. The DNA @ SiO of claim 4 2 The application method of the tracer is characterized in that the concentration of the effective component for tracing injected into the tracer by each tracer injection port is the same.
6. DNA @ SiO according to claim 4 2 The application method of the tracer is characterized in that water is injected into the multi-fracture rock sample column from the first port, and the rock sample is infiltrated and washed, and comprises the following steps:
and injecting water into the multi-fracture rock sample column from the first port at the flow rate of 3-6 mL/min, and infiltrating and washing the rock sample for 15-60 min.
7. DNA @ SiO according to claim 4 2 The application method of the tracer is characterized in that a displacement fluid is injected into the multi-fracture rock sample column from the second port, and comprises the following steps:
and injecting a displacement fluid into the multi-fracture rock sample column from the second port at a flow rate of 2.5-5 mL/min.
8. According to the claimsObtaining the DNA @ SiO of claim 4 2 A method of tracer application, wherein collecting effluent from the first port comprises:
collecting effluent liquid of the first port at fixed time and quantity; wherein the interval time between two adjacent times of collection is 0.5-2 min.
9. DNA @ SiO according to claim 3 2 The application method of the tracer is characterized in that when the fractured rock sample column is a multi-fractured rock sample column, the rock stratum sample is provided with a plurality of main fractures; the main fracture corresponds to the tracer injection port.
10. A multi-fracture simulation sample column for a multi-fracture formation, comprising:
the tracer injection device comprises a shell, wherein a containing cavity is arranged in the shell, and a plurality of tracer injection ports which are communicated with the containing cavity and are used for injecting different tracers are arranged on the shell; openings are also formed in the two ends of the shell; and
sealing the end; the sealing ends comprise a first sealing end and a second sealing end, and the first sealing end and the second sealing end are respectively connected with the openings at the two ends of the shell in a sealing manner; the first sealing end is provided with a first port for injecting/discharging fluid; the second sealed end is provided with a second port for injecting/discharging fluid.
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