CN113480985A - Preparation method and application of micro-nano expanded micelle elastic particle oil displacement emulsion - Google Patents
Preparation method and application of micro-nano expanded micelle elastic particle oil displacement emulsion Download PDFInfo
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Abstract
The invention relates to the field of oil field development, profile control and flooding, in particular to a preparation method and application of a micro-nano expanded micelle elastic particle oil displacement emulsion, wherein the preparation method comprises the following materials: the method adopts a multiple crosslinking technology and a dispersion technology, and the nano-scale, micron-scale and millimeter-scale elastic particles obtained by the method can enter the deep part of a stratum through the particle size of the elastic particles and are aggregated and expanded in the deep part of the stratum, so that the stratum water absorption profile can be effectively adjusted, the mobility control capability is strong, and meanwhile, the elastic particle aqueous solution is further compounded with active saponin for the second time, so that the micro-nano oil displacement emulsion with the expansion plugging capability and the strong oil displacement capability is formed.
Description
Technical Field
The invention relates to the field of oil field development and profile control, in particular to a preparation method and application of a micro-nano expanded micelle elastic particle oil displacement emulsion.
Background
The water content increase and yield decrease of an oil well caused by reservoir heterogeneity are main factors influencing the efficient development of an oil reservoir, and the heterogeneity of a stratum needs to be regulated and controlled firstly to improve the water-flooding development effect of the oil reservoir in the middle and later periods. In various current technological measures, polymer injection, a polymer-based binary/ternary composite oil displacement system, gel, polymer microspheres and the like are important technical means for realizing reservoir regulation and control of an oil reservoir. However, the technical measures expose some problems in the implementation process of an oil reservoir and mine field, and are influenced by factors such as shearing of ground injection equipment, stratum seepage shearing, stratum physicochemical properties (temperature, mineralization degree, pH value and the like) and stratum water dilution, so that the viscosity loss based on polymers is large, the fluidity control capability is weakened, and particularly in the subsequent water flooding stage, the injection pressure is reduced quickly, and a long-term effective regulation and control effect is difficult to obtain; for the jelly glue system based on the polymer, under the influence of the shearing and diluting effects, the effective concentration of the polymer injected into the formation jelly glue solution is diluted, the polymer structure is damaged, the jelly time is uncertain, the jelly strength is reduced, and the regulation and control effect is reduced. For low permeability reservoirs, the polymer is not resistant to high temperature, high salt and injection, has more obvious shearing effect, and is not suitable for polymers; the polymer microsphere is prepared by using A Monomer (AM) raw material, so that the environment friendliness is poor, the preparation process is relatively complex, and the cost is high.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a preparation method and application of a micro-nano expanded micelle elastic particle oil displacement emulsion.
(II) technical scheme
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of micro-nano expanded micelle elastic particle oil displacement emulsion is characterized by comprising the following steps:
s1, selecting 0.29-0.71 part of high-temperature high-molecular modified polyacrylamide, 0.6-0.9 part of high-temperature phenolic resin cross-linking agent, 0.1-0.3 part of tannin, 0.1-0.15 part of hydramine accelerator, 0.1-0.2 part of nano silicon dioxide and 0.2-0.3 part of modified saponin by weight parts, adding water into a stainless steel tank to 90% of volume, adding the modified polyacrylamide in a throwing manner, starting a stirring device, and uniformly stirring;
s2, adding the high-temperature phenolic resin cross-linking agent, and continuously stirring uniformly;
s3, sequentially adding tannin and coagulant alcohol amine and continuously stirring uniformly;
s4, heating to 89-96 ℃ after uniformly stirring;
s5, pumping colloid generated by the chemical reaction into a shearing machine, adjusting the frequency of the shearing machine, and grinding and shearing for multiple times to obtain a nano-micron elastic particle aqueous solution with the required granularity in a mine field;
and S6, extracting the nano-micron elastic particle aqueous solution into a stirring tank again, sequentially adding the modified saponin and the nano-silicon dioxide, heating to 60 ℃, and continuously stirring to form a uniform and semitransparent emulsion system.
Preferably, the high-temperature high-molecular modified polyacrylamide, the coagulant alcohol amine, the nano silicon dioxide and the modified saponin are special high-temperature modified polymers.
Preferably, the gel micelle emulsion obtained by the above preparation method is evaluated from the aspects of color, dispersion uniformity, flow viscosity, and the like of the gel micelle emulsion by a visual observation method.
Preferably, the micro-morphology of the liquid-dispersed gel micelle emulsion is observed by a Scanning Electron Microscope (SEM) and an optical microscope.
Preferably, the effective content, particle size, viscosity and pH of the gel micelle emulsion obtained by the above preparation method are checked.
Preferably, the gel micelle emulsion obtained by the preparation method can be tested by testing the dispersibility, the Zeta potential, the expansion coalescence capability, the temperature resistance and salt tolerance, the injection performance and the plugging performance of the gel micelle emulsion.
Preferably, the emulsion obtained by the preparation method of the micro-nano expanded micelle elastic particle oil displacement emulsion is applied to oil reservoir development.
(III) advantageous effects
Compared with the prior art, the invention provides a preparation method of a micro-nano expanded micelle elastic particle oil displacement emulsion, which has the following beneficial effects:
1. the method adopts a multiple crosslinking technology and a dispersion technology, and prepares nano-micron elastic particle aqueous phase dispersion solution after mechanical shearing and grinding of body gel synthesized by special high-temperature modified polymer, tannin and high-temperature crosslinking agent. The nano-micron elastic particles have good viscoelasticity, can move to the deep part along with the deformation of the size and the shape of pores in a stratum, and can avoid the influence of ground shearing, underground seepage shearing and physicochemical properties of a polymer regulation system.
2. The nano-scale, micron-scale and millimeter-scale elastic particles obtained by the method can enter the deep part of the stratum through the particle size of the elastic particles, are gathered and expanded in the deep part of the stratum, can effectively adjust the water absorption profile of the stratum, have strong fluidity control capability, and simultaneously carry out secondary compounding on the aqueous solution of the elastic particles and active saponin to form the micro-nano oil displacement emulsion with expansion plugging capability and strong oil displacement capability.
Drawings
FIG. 1 is a flow chart of the detection experiment of the present invention.
Detailed Description
In order to better understand the purpose, structure and function of the present invention, the preparation method and application of the micro-nano expanded micelle elastic particle oil-displacing emulsion of the present invention will be further described in detail.
A preparation method of micro-nano expanded micelle elastic particle oil displacement emulsion comprises the following steps:
s1, selecting 0.29-0.71 part of high-temperature high-molecular modified polyacrylamide, 0.6-0.9 part of high-temperature phenolic resin cross-linking agent, 0.1-0.3 part of tannin, 0.1-0.15 part of hydramine accelerator, 0.1-0.2 part of nano silicon dioxide and 0.2-0.3 part of modified saponin by weight parts, adding water into a stainless steel tank to 90% of volume, adding the modified polyacrylamide in a throwing manner, starting a stirring device, and uniformly stirring;
s2, adding the high-temperature phenolic resin cross-linking agent, and continuously stirring uniformly;
s3, sequentially adding tannin and coagulant alcohol amine and continuously stirring uniformly;
s4, heating to 89-96 ℃ after uniformly stirring;
s5, pumping colloid generated by the chemical reaction into a shearing machine, adjusting the frequency of the shearing machine, and grinding and shearing for multiple times to obtain a nano-micron elastic particle aqueous solution with the required granularity in a mine field;
and S6, extracting the nano-micron elastic particle aqueous solution into a stirring tank again, sequentially adding the modified saponin and the nano-silicon dioxide, heating to 60 ℃, and continuously stirring to form a uniform and semitransparent emulsion system.
Specifically, in the gradual heating process, the following chemical reactions sequentially occur to materials in the stainless steel tank, firstly, the modified high-molecular polyacrylamide (with the molecular weight of 600-.
The function of adding the nano silicon dioxide in the sixth step is to further enhance the shearing resistance of the molecular functional group, reduce the shearing resistance of the molecular functional group during migration in the pore throat of the stratum, slow down the attenuation speed of the molecular functional group after expansion, delay the expansion residence time of the molecular functional group, increase the plugging time of the molecular functional group for plugging a high water consumption zone in an oil layer and improve the plugging and expansion efficiency.
Furthermore, the high-temperature high-molecular modified polyacrylamide, the coagulant alcohol amine, the nano silicon dioxide and the modified saponin are special high-temperature modified polymers.
Further, after the synthesis of the gel micelle emulsion in the steps, visual observation can be adopted to evaluate the color, the dispersion uniformity, the flowing viscosity and the like of the gel micelle emulsion, the color of the gel micelle emulsion is required to be uniform, no obvious layering phenomenon exists, the fluidity is good, the sample is qualified, the color of the gel micelle emulsion is from faint yellow to brown, if the color is light white or milky white, the complete reaction of the body gel is indicated, and if the bottom of a specific sample is partially precipitated, the sample is stirred for 5 min. If the pellet was easily resuspended again and no further significant pellet formed within 24 hours, the sample was acceptable.
Furthermore, the microscopic morphology of the liquid-state dispersed gel micelle emulsion can be observed by a Scanning Electron Microscope (SEM) and an optical microscope.
The specific test steps for observing the gel micelle emulsion by adopting a scanning electron microscope comprise:
sampling: randomly extracting 500ml of a sample to be detected of the gel micelle emulsion for later use;
preparing a solution: dispersing 10g of the to-be-detected sample of the gel micelle emulsion in 90g of deionized water, stirring for 5 minutes at room temperature, and performing ultrasonic treatment for 5 minutes to form uniformly dispersed gel micelle emulsion;
③ drying the sample: 2-3 drops of the dispersed gel micelle emulsion solution prepared in the second step are taken by a dropper, dropped to a copper mesh, vacuumized and dried for 10 hours, and then is to be detected;
fourthly, spraying gold on the sample: spraying gold on the dried sample to be detected in the step three, placing the sample on an SEM detection table, and observing the sample;
observing a sample: and (3) selecting a proper magnification factor (2 k-8 k) to observe according to needs, and analyzing and determining the shape, size, dispersity and the like of the gel micelle emulsion according to the observed micro-morphology.
The specific test steps for observing the gel micelle emulsion by adopting an optical microscope comprise:
sampling: randomly extracting 500ml of a sample to be detected of the gel micelle emulsion for later use;
preparing a solution: dispersing 10g of the to-be-detected sample of the gel micelle emulsion in 90g of deionized water, stirring for 5 minutes at room temperature, and performing ultrasonic treatment for 5 minutes to form uniformly dispersed gel micelle emulsion;
observation of the sample: and (3) selecting a proper magnification factor (2 k-8 k) to observe according to needs, and analyzing and determining the shape, size, dispersity and the like of the gel micelle emulsion according to the observed micro-morphology.
Furthermore, the effective content, particle size, viscosity and pH value of the gel micelle emulsion are used as tests.
Specifically, the effective content is an important detection index of the gel micelle emulsion, the application effect of the product is directly determined, the effective content of the gel micelle emulsion is determined by adopting a starch-cadmium iodide method in the test, the detection equipment is a Shanghai Ennikov UV-4802 double-beam ultraviolet visible spectrophotometer, and the effective content of the gel micelle emulsion industrialized product is qualified if the effective content is more than 85%.
The test steps are as follows
(1) Principle of detection
The starch-cadmium iodide colorimetric method is a first-step reaction by utilizing Hofmann rearrangement, which is the prior art and is not described too much, amide groups in a body jelly or a polymer which does not participate in the reaction react with bromine water to generate N-bromoamide, the excessive bromine water in the reaction is removed by using a reducing agent sodium formate, the N-bromoamide is further hydrolyzed to generate hypobromous acid, the hypobromous acid can quantitatively oxidize iodide ions into blue triiodide-starch complexes, and the reaction degree is determined by measuring the absorbance of the hypobromous acid. The reaction can still be carried out when the concentration content of the amide group is low, so that the preparation efficiency can be rapidly measured. The reaction mechanism is as follows:
HBrO+2I-+H+→I2+Br-+H2O
I2+I-+ starch → I3 --starch (blue compound)
(2) Preparation of detection reagent
The preparation method of the buffer solution comprises the following steps: 12.50g of sodium acetate trihydrate (CH3 COONa.3H2O) is accurately weighed and dissolved in 400mL of distilled water, 0.25g of hydrated aluminum sulfate (Al2(SO4) 3.18H 2O) is added, the pH value is adjusted to 4.0 by acetic acid, and finally the mixture is diluted to 500mL for standby.
The preparation method of the starch-cadmium iodide reagent comprises the following steps: accurately weighing 1.25g of starch in 200mL of distilled water, heating and boiling for 10min, cooling, diluting to about 400mL, adding 5.50g of cadmium iodide, dissolving, filtering, and finally diluting to 500mL for later use.
The specific experimental steps are as follows: adding 5mL of buffer solution into a 50mL volumetric flask, wherein the polymer content is within the range of 15-300 mu g, the solution in the volumetric flask is not more than 30mL, and then diluting the solution to 35mL by using distilled water; after being mixed uniformly, 1mL of saturated bromine water is added, after shaking uniformly, reaction is carried out for 10min, and then 3mL of sodium formate solution with the mass fraction of 1% is added; after the reaction lasts for 5min, 5mL of starch-cadmium iodide reagent is immediately added, then the mixture is diluted to the scale with distilled water and shaken up, and the reaction lasts for 10 min. And measuring the absorbance of the sample by using a spectrophotometer, measuring each sample in parallel twice, and taking the average value as an experimental result.
(3) Detection step
Firstly, measuring a standard curve: taking a raw material polymer for preparing the gel micelle emulsion, and preparing a 100mg/L polymer standard solution by using deionized water. Adding 5mL of buffer solution into 9 50mL colorimetric tubes respectively, adding 0, 0.3mL, 0.5mL, 0.8mL, 1.0mL, 1.5mL, 2.0mL, 2.5mL and 3.0mL of standard solution respectively, diluting the solution to 35mL by deionized water, adding 1mL of saturated bromine water respectively, reacting for 15min, adding 5mL of 1% sodium formate solution, adding 5mL of starch-cadmium iodide solution after reacting for 5min, diluting the solution to a scale by deionized water, developing the solution for 15min, carrying out color comparison at a wavelength of 590nm by using a 1cm cuvette, and drawing a standard curve by using the solution concentration as an abscissa and the absorbance as an ordinate.
Preparing a solution: and (3) dispersing 10g of the to-be-detected sample of the gel micelle emulsion in 90g of deionized water, stirring for 5 minutes at room temperature, and performing ultrasonic treatment for 5 minutes to form the uniformly dispersed gel micelle emulsion.
③ 5mL of buffer solution is added into the volumetric flask, 0.5mL of gel micelle emulsion is dripped into the volumetric flask, and then the solution is diluted to 35mL by distilled water and mixed evenly.
And fourthly, adding 1mL of saturated bromine water, shaking up and reacting for 10 min.
Fifthly, adding 3mL of sodium formate solution with the mass fraction of 1 percent, and reacting for 5 min.
Sixthly, adding 5mL of starch-cadmium iodide reagent, diluting to 50mL by using distilled water, shaking up, and reacting for 10 min.
And measuring absorbance, measuring each sample twice in parallel, and taking an average value as a test result.
More specifically, the particle size determines the stability of the industrial product of the gel micelle emulsion, and ensures that the injected product can meet the use requirement.
The test steps are as follows
(1) Principle of testing
The test uses a laser particle size analyzer to measure the particle size of the expanded particles, the model of the laser particle size analyzer is Bettersize2000, and the test principle is as follows: in the propagation of light, the wave front is limited by the gap holes or particles which are equivalent to the wavelength scale, the emission which takes each elementary wave at the limited wave front as a source is interfered in space to generate diffraction and scattering, and the spatial (angle) distribution of the diffracted and scattered light energy is related to the wavelength of the light wave and the scale of the gap holes or particles. When laser is used as a light source and the light is monochromatic light with a certain wavelength, the spatial (angular) distribution of diffracted and scattered light energy is only related to the particle size. For the diffraction of the particle group, the size of each particle grade determines the light energy obtained at each specific angle, and the proportion of the light energy at each specific angle in the total light energy reflects the distribution abundance of each particle grade. And establishing a mathematical physical model for representing the abundance of the particle size fraction and the light energy obtained at each specific angle, measuring the light energy, and comparing the light energy measured at the specific angle with the total light energy to deduce the abundance ratio of the corresponding particle size fraction of the particle group.
(2) Measurement procedure
Sampling: randomly extracting 500ml of a sample to be detected of the gel micelle emulsion for later use;
preparing a solution: dispersing 10g of the to-be-detected sample of the gel micelle emulsion in 90g of deionized water, stirring for 5 minutes at room temperature, and performing ultrasonic treatment for 5 minutes to form uniformly dispersed gel micelle emulsion;
starting the instrument: and pouring deionized water into the sample cell of the laser particle size analyzer, enabling the liquid level of the deionized water to be over the upper side edge of the water inlet, opening the drain valve, closing the drain valve (discharging bubbles of the circulating system) when the drain pipe is seen to have liquid flowing out, starting the circulating pump to enable the circulating system to be full of the liquid, and then turning off the circulating pump.
Calibrating an instrument: opening a circulating pump, performing ultrasonic treatment, performing circulating stirring, clicking a 'test' button, and then clicking a pop-up box to ensure that the test software enters a reference measurement state; a background calibration is performed.
Testing the particle size: and (3) placing a proper amount of sample (the amount of the sample added is controlled according to the shading ratio) into a sample cell, and measuring, wherein the ultrasonic treatment and the stirring are carried out all the time in the measuring process until the sample detection is finished.
Each sample was subjected to the above measurement procedure in triplicate, and the average was taken as the measurement result.
It is noted that the expansion and coalescence ability of the gel micelle emulsion was observed by the particle size, the micro-morphology (scanning electron microscopy and optical microscopy) and the direct measurement method, and this was taken as a test.
The test steps are as follows
(1) Particle size analysis method
The particle size of the gel micelle emulsion before and after aging is measured by a laser particle size analyzer, and the measuring device is the same as the particle size measuring method.
The specific determination steps are as follows:
sampling: randomly extracting 500ml of a sample to be detected of the gel micelle emulsion for later use;
preparing a solution: and (3) dispersing 10g of the to-be-detected sample of the gel micelle emulsion in 40g of the prepared liquid water, stirring for 5 minutes at room temperature, and performing ultrasonic treatment for 5 minutes to form the uniformly dispersed gel micelle emulsion.
And thirdly, aging the solution prepared in the second step for 3 days, 5 days, 10 days, 20 days, 30 days and the like under the oil reservoir temperature condition, and testing.
And fourthly, sample determination: and (3) taking the solution of the gel micelle emulsion with different aging days, and determining according to a determination method of a laser particle size analyzer, wherein ultrasound is not required to be started in the determination process, and the circulation speed of the apparatus is set to be 600 rpm/min. Each sample was assayed in triplicate and the average was taken as the test result.
(3) Micro-topography method
Adopting SEM to represent the state of the gel micelle emulsion before and after aging, the testing device and the method are the same as the micro-morphology testing steps, and the specific testing steps are as follows:
sampling: randomly extracting 500ml of a sample to be detected of the gel micelle emulsion for later use;
preparing a solution: dispersing 10g of the to-be-detected sample of the gel micelle emulsion in 40g of the solution removing water, stirring for 5 minutes at room temperature, and performing ultrasonic treatment for 5 minutes to form uniformly dispersed gel micelle emulsion;
and thirdly, aging the solution prepared in the second step for 3 days, 5 days, 10 days, 20 days, 30 days and the like under the oil reservoir temperature condition, and testing.
And fourthly, sample determination: and (3) taking the solution of the gel micelle emulsion with different aging days, and determining according to a determination method of a scanning electron microscope.
(4) Direct observation method
The coalescence-expansion performance of the gel micelle emulsion is determined by adopting a direct observation or direct measurement method, if samples with different test days have sediment at the bottom, the gel micelle emulsion has certain coalescence performance, and the specific steps are as follows:
sampling: randomly extracting 500ml of a sample to be detected of the gel micelle emulsion for later use;
preparing a solution: dispersing 10g of the to-be-detected sample of the gel micelle emulsion in 40g of the solution removing water, stirring for 5 minutes at room temperature, and performing ultrasonic treatment for 5 minutes to form uniformly dispersed gel micelle emulsion;
and thirdly, aging the solution prepared in the second step for 3 days, 5 days, 10 days, 20 days, 30 days and the like under the oil reservoir temperature condition, and testing.
And fourthly, sample determination: the solutions of the gel micelle emulsions with different aging days were measured according to the measurement method of an optical microscope.
Similarly, the temperature resistance and salt tolerance of the gel micelle emulsion are observed by particle size, micro morphology (scanning electron microscopy and optical microscopy) and direct measurement method, and the test steps are the same as the measurement method.
Specifically, the temperature resistance and salt tolerance of the gel micelle emulsion are determined by adopting a direct observation or direct measurement method, and if samples with different aging days have sediment at the bottom and have no obvious flocculent or degradation phenomenon, the gel micelle emulsion has certain temperature resistance and salt tolerance.
Specifically, the SEM is adopted to represent the states of the gel micelle emulsion before and after aging, if the particles have obvious adhesion and coalescence phenomena, good temperature resistance and salt tolerance are shown, and if no obvious particles or substances exist, the temperature resistance and salt tolerance of the test sample are poor.
Specifically, a laser particle size analyzer is used for measuring the particle size of the gel micelle emulsion before and after aging, the temperature resistance and salt tolerance of the gel micelle emulsion are represented by the change of the particle size, if the measured particle size is obviously increased, the gel micelle emulsion has better temperature resistance and salt tolerance, and if the particle size is reduced, the temperature resistance and salt tolerance is poorer.
Further, viscosity is an important index for reflecting dispersibility and injectability of the gel micelle emulsion, if the viscosity is too high, the injectability is poor for low-permeability or ultra-low-permeability oil reservoirs, and meanwhile, the burden in the liquid preparation process can be caused, so that the gel micelle emulsion cannot be dispersed.
The test steps are as follows
(1) Principle of testing
The principle of the rotational viscometer is to rotate an object entering a fluid to be measured or to keep the object stationary, so that when the fluid around the object is rotated and flows, the object in the fluid will be subjected to a viscous moment due to a shear stress. If the same conditions such as rotation are ensured, the magnitude of the viscous torque changes along with the change of the viscosity of the fluid, and the viscosity of the fluid can be obtained according to a viscosity formula by measuring the magnitude of the viscous torque.
(2) Test procedure
Sampling: randomly extracting 500ml of a sample to be detected of the gel micelle emulsion for later use;
preparing a solution: taking 100g of the gel micelle emulsion to be detected, stirring at room temperature for 5 minutes, and carrying out ultrasonic treatment for 5 minutes to be detected;
starting the instrument: starting a Brookfield II viscometer, starting an ultrasonic circulating water bath, and selecting a 0# rotor to measure at 30 ℃.
And fourthly, after the measurement is finished, closing the system, taking down the rotor, cleaning, wiping and putting the rotor back into the box.
The test determines the sample three times, and the average value of the three times is taken as the test result.
Further, the pH of the gel micelle emulsion affects the storage and application of the product, and also affects the safety of the product.
The test steps are as follows
(1) Principle of testing
The pH meter operates on the principle of a galvanic cell, the electromotive force between two electrodes of which is related, according to nernst's law, both to the properties of the electrodes themselves and to the concentration of hydrogen ions in the solution. There is a corresponding relationship between the electromotive force of the primary cell and the hydrogen ion concentration, and the negative logarithm of the hydrogen ion concentration is the pH value.
(2) Test method
Calibrating an instrument: randomly extracting 500ml of a sample to be detected of the gel micelle emulsion for later use;
preparing a solution: taking 100g of the gel micelle emulsion to be detected, stirring at room temperature for 5 minutes, and carrying out ultrasonic treatment for 5 minutes to be detected;
testing the sample: the pH viscometer was started and the pH was measured at 30 ℃.
The product is measured three times, and the average value of the three times is taken as the test result.
Furthermore, the product dispersibility comprises two parts of the dispersibility of the stock solution of the gel micelle emulsion product and the dispersibility of the prepared solution, and the good dispersibility is a good basis for the application of the gel micelle emulsion industrial product.
The test steps are as follows
(1) Test method
The dispersibility of the gel micelle emulsion is measured by adopting an intuitive observation method, the stability of the industrial product of the gel micelle emulsion or the prepared solution is mainly observed, and whether the system has irreversible floating or precipitation is observed.
(2) Measurement procedure
Stability of the gel micelle emulsion industrial product:
sampling: and randomly drawing 500ml of the sample to be detected of the gel micelle emulsion for later use.
Observation: and (3) taking 100g of the gel micelle emulsion to be detected, stirring at room temperature for 5 minutes, carrying out ultrasonic treatment for 5 minutes, and observing whether a precipitation or delamination phenomenon exists within 10 days.
Stability of the gel micelle emulsion industrial product preparation solution:
sampling: randomly extracting 500ml of a sample to be detected of the gel micelle emulsion for later use;
preparing a solution: dissolving 10g of the gel micelle emulsion in formation water, stirring for 5 minutes at room temperature, and carrying out ultrasonic treatment for 5 minutes to be detected;
observation: and (3) placing the prepared solution at room temperature to observe whether precipitation or delamination occurs within 10 days.
Further, the Zeta potential is an important parameter for characterizing the stability of the product of the gel micelle emulsion. When the Zeta potential absolute value of the particles is higher than 30mV, the particles are relatively stable; when the absolute value of the Zeta potential of the particles is lower than 30mV, the particles are easy to generate coagulation phenomenon. The potential of the gel micelle emulsion product is measured by a Brookhein Omni multi-angle particle size and high-sensitivity Zeta potential analyzer. The Zeta potential of the product is-22 to-30 mV.
The Zeta potential of the gel micelle emulsion product is measured by the following specific steps:
sampling: randomly extracting 500ml of a sample to be detected of the gel micelle emulsion for later use;
preparing a solution: dispersing 10g of the to-be-detected sample of the gel micelle emulsion in 90g of deionized water, stirring for 5 minutes at room temperature, and performing ultrasonic treatment for 5 minutes to form uniformly dispersed gel micelle emulsion;
starting the instrument: starting the Bruk Highun Omni multi-angle granularity and high-sensitivity Zeta potential analyzer, and after 15min, placing a sample to be measured in the analyzer for measurement at the measurement temperature of 30 ℃.
And fourthly, sample determination: each sample was assayed in triplicate and the average was taken as the test result.
Furthermore, the experiment characterizes the injection capability, namely the injection performance, of the gel micelle emulsion by the resistance coefficient, and the test steps are as follows:
(1) detection method
The injection capability of the gel micelle emulsion is evaluated by adopting a core flow device, and the experimental flow is shown in figure 1.
(2) Experimental procedure
Firstly, extracting a natural rock core, drying and measuring the dry weight;
secondly, saturating the core with water, measuring the wet weight, and calculating the pore volume and the core permeability;
③ taking the industrial product of the gel micelle emulsion, adding 20g of the stock solution into 20g of the prepared solution water, and stirring for 5 minutes to form a uniformly dispersed solution.
Fourthly, injecting the 5PV gel micelle emulsion at a pump speed of 0.5ml/min, and recording the pressure change;
changing the permeability or injection concentration of the rock core and repeating the steps;
sixthly, calculating the resistance coefficient according to a formula (in the effective content detection step).
Furthermore, the test shows the plugging capability and the plugging performance of the gel micelle emulsion by the plugging rate and the residual resistance coefficient, and the test steps are as follows:
(1) detection indexes are as follows: and (4) plugging rate.
(2) The experimental steps are as follows:
firstly, extracting a natural rock core, drying and measuring the dry weight;
secondly, saturating the core with water, measuring the wet weight, and calculating the pore volume and the core permeability;
③ taking the industrial product of the gel micelle emulsion, adding 20g of the stock solution into 20g of the prepared solution water, and stirring for 5 minutes to form a uniformly dispersed solution.
Fourthly, injecting 1PV gel micelle emulsion at the pump speed of 0.5ml/min, and recording the pressure change;
fifthly, placing the core in the oil reservoir for aging for 7 days, then performing water drive, and recording the pressure change
Sixthly, repeating the steps by changing the permeability or injection concentration of the rock core.
And (c) calculating residual resistance coefficients and blocking rates of the core parameters according to the (5-2) and the (5-3).
In conclusion, the indexes of the static evaluation of the gel micelle emulsion mainly comprise:
the effective content: 85% -90%;
the macroscopic appearance is as follows: light yellow to light yellow;
③ microcosmic appearance: spherical particles;
particle size: 600-10000 nm, and determining the product specification according to the reservoir condition;
viscosity: the viscosity of the stock solution is less than or equal to 100 mPas, and the viscosity of the injected working solution is less than or equal to 5 mPas;
⑥pH：6.5～8.0；
seventh, dispersibility: the dispersion time in the prepared liquid water is less than or equal to 5 minutes;
[ Zeta potential ]: -24 to-32 mV;
ninthly, expansion and coalescence capacity: aging at 60 deg.C for 30 days.
It is to be understood that the present invention has been described with reference to certain embodiments, and that various changes in the features and embodiments, or equivalent substitutions may be made therein by those skilled in the art without departing from the spirit and scope of the invention. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the invention without departing from the essential scope thereof. Therefore, it is intended that the invention not be limited to the particular embodiment disclosed, but that the invention will include all embodiments falling within the scope of the appended claims.
Claims (7)
1. A preparation method of micro-nano expanded micelle elastic particle oil displacement emulsion is characterized by comprising the following steps:
s1, selecting 0.29-0.71 part of high-temperature high-molecular modified polyacrylamide, 0.6-0.9 part of high-temperature phenolic resin cross-linking agent, 0.1-0.3 part of tannin, 0.1-0.15 part of hydramine accelerator, 0.1-0.2 part of nano silicon dioxide and 0.2-0.3 part of modified saponin by weight parts, adding water into a stainless steel tank to 90% of volume, adding the modified polyacrylamide in a throwing manner, starting a stirring device, and uniformly stirring;
s2, adding the high-temperature phenolic resin cross-linking agent, and continuously stirring uniformly;
s3, sequentially adding tannin and coagulant alcohol amine and continuously stirring uniformly;
s4, heating to 89-96 ℃ after uniformly stirring;
s5, pumping colloid generated by the chemical reaction into a shearing machine, adjusting the frequency of the shearing machine, and grinding and shearing for multiple times to obtain a nano-micron elastic particle aqueous solution with the required granularity in a mine field;
and S6, extracting the nano-micron elastic particle aqueous solution into a stirring tank again, sequentially adding the modified saponin and the nano-silicon dioxide, heating to 60 ℃, and continuously stirring to form a uniform and semitransparent emulsion system.
2. The preparation method of the micro-nano expanded micelle elastic particle oil-displacing emulsion according to claim 1, wherein the high-temperature polymer modified polyacrylamide, the coagulant alcohol amine, the nano silicon dioxide and the modified saponin are special high-temperature modified polymers.
3. The preparation method of the micro-nano expanded micelle elastic particle oil-displacing emulsion according to claim 1, wherein the gel micelle emulsion obtained by the preparation method is evaluated from the aspects of color, dispersion uniformity, flow viscosity and the like of the gel micelle emulsion by adopting an intuitive observation method.
4. The preparation method of the oil displacement emulsion of micro-nano expanded micelle elastic particles according to claim 1, wherein the micro-morphology of the liquid dispersed gel micelle emulsion is observed by a Scanning Electron Microscope (SEM) and an optical microscope.
5. The preparation method of the micro-nano expanded micelle elastic particle flooding emulsion according to claim 1, wherein the effective content, particle size, viscosity and pH value of the gel micelle emulsion obtained by the preparation method are used for detection.
6. The preparation method of the micro-nano expanded micelle elastic particle oil-displacing emulsion according to claim 1, wherein the gel micelle emulsion obtained by the preparation method can be tested by testing the dispersibility, the Zeta potential, the expansion coalescence capability, the temperature resistance and salt tolerance, the injection performance and the plugging performance of the gel micelle emulsion.
7. The emulsion obtained by the preparation method of the micro-nano expanded micelle elastic particle oil displacement emulsion is applied to oil reservoir development.
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| CN115011321A (en) * | 2022-06-01 | 2022-09-06 | 大庆亿莱检验检测技术服务有限公司 | Preparation device and method of shale oil reservoir imbibition nano oil displacement emulsion |
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