CN114854387B - Nano flower-nano sheet dual-inorganic nano profile control and flooding system and application thereof - Google Patents
Nano flower-nano sheet dual-inorganic nano profile control and flooding system and application thereof Download PDFInfo
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- CN114854387B CN114854387B CN202210570585.5A CN202210570585A CN114854387B CN 114854387 B CN114854387 B CN 114854387B CN 202210570585 A CN202210570585 A CN 202210570585A CN 114854387 B CN114854387 B CN 114854387B
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Abstract
The invention discloses a nano flower-nano sheet dual-inorganic nano profile control and flooding system and application thereof, and relates to the technical field of oil developmentThe inorganic nano profile control and flooding system comprises modified MoS 2 Nano flower and modified MoS 2 Nanosheets and alkylphenol ethoxylates. The modified MoS 2 Nanosheet and modified MoS 2 The mass ratio of the nanoflower to the alkylphenol ethoxylates is 1. The nano-sheet-nano flower dual-inorganic nano profile control and flooding system has good temperature resistance and salt resistance and is not influenced by impurities in formation water; the concentration required by field injection is small, and a relatively ideal profile control and flooding effect can be achieved by using a small amount of the profile control and flooding agent, so that complicated field injection conditions can be met; as a nanoscale profile control and flooding system, the composite material has small particle size, good compatibility with low-permeability pore throat dimensions and good injectability.
Description
Technical Field
The invention relates to the technical field of petroleum development, in particular to a nanoflower-nanosheet double-inorganic-nano profile control and flooding system and application thereof.
Background
At present, deep profile control and flooding agents for low-permeability oil reservoirs are various in types and can be divided into single-liquid profile control and flooding agents and double-liquid profile control and flooding agents according to injection modes of the profile control and flooding agents. When the profile control is carried out, only one working fluid is used, the working fluid firstly enters a layer with high water saturation, and after the injection pressure is increased, the working fluid sequentially enters a low-permeability layer with high oil saturation to drive out crude oil in the low-permeability layer so as to improve the secondary recovery ratio; the two-fluid method is that two kinds of working fluid must be used during profile control and oil displacement, one is used for profile control and one is used for oil displacement, and during injection, the profile control agent is in front, the oil displacement agent is in back, and the oil displacement agent is injected into stratum to perform deep profile control and oil displacement. The oil displacement agent can be divided into inorganic type, gel type, particle type and the like according to different types of displacement agents, and different displacement agents have different effects on the displacement of the deep part of an oil reservoir and have obvious defects. The common inorganic profile control agent is easy to precipitate, and cannot achieve good effect on profile control and flooding of deeper strata; the gel profile control and flooding agent can keep gel plugging performance for a long time, but is easily influenced by impurities in sewage. Meanwhile, when the concentration of the profile control agent system is low, the injection amount required by field application is large, the cost is high, and complex field injection conditions are difficult to meet; the bulk-expanded particles have the performances of temperature resistance and salt resistance, are convenient to construct and operate, but have overlarge size and overhigh injection pressure, are difficult to transport in the stratum after hydration expansion, and quickly lose efficacy in the stratum along with the increase of the transport distance. In recent years, with the rapid development of nanotechnology, people try to apply nanotechnology to a profile control and drive system, and make great progress. For example, the polymer microsphere modifying and flooding agent with wide prospect is a micro-nano particle which can expand when meeting water and block the pore throat of the stratum step by step, and the injection amount can be adjusted without being influenced by prepared water. However, the polymer microspheres also have the disadvantages of poor rigidity, easy breakage after entering the stratum and being sheared, and the like.
At present, the oil field exploitation enters the middle and later stages, and the low extraction rate and the high water content of the oil field become problems to be solved urgently. Research shows that the reserves of the low-permeability reservoir occupy more than half of the proven reserves, so the method is an important direction for ensuring the safety of oil and gas for the development of the low-permeability reservoir. The pore throats of the low-permeability reservoir are fine, the size difference of the pore throats is obvious, and the pore throats are mainly distributed in a micron-sized (more than 1 mu m) and a nanometer-sized (less than 0.1 mu m) mode, so that the heterogeneity is extremely strong, and the saturation of residual oil in a near-wellbore area is obviously reduced after conventional profile control and flooding; meanwhile, the low-permeability reservoir rock has poor physical properties and high clay content, so that the starting pressure and the injection pressure are high during water injection development, the water content rises quickly, water flow breaks through along a high-permeability layer, and the difference of the water injection profile at the deep part of an oil reservoir is obvious; the pore throat is small, the problems of crude oil blockage, jamin effect and the like are easy to occur, crude oil cannot be effectively displaced, and the water drive recovery rate is low. The deep profile control and flooding technology can selectively block the dominant pore canals, effectively increase the swept volume of a deep reservoir and achieve the effect of improving the recovery ratio, is one of the most effective methods for improving the recovery ratio of the low-permeability heterogeneous oil reservoir at present, and emphasizes that the oil displacement is carried out to the maximum extent in the profile control process by organically combining the deep profile control technology and the oil displacement technology. The profile control agent is a chemical agent with both profile control and oil displacement functions, and the deep profile control technology firstly injects the profile control agent into the deep part of the stratum to block a large pore channel of a high permeable layer, so that the subsequent displacement fluid is redirected into a small pore channel of a low permeable layer, thereby expanding the swept volume of the displacement fluid, improving the oil washing efficiency and further improving the crude oil recovery ratio. Along with the deeper and deeper exploitation oil layer, the temperature of the stratum gradually increases, and the hypersalinity of the stratum water provides higher requirements for the development of the deep profile control agent. When the polymer is developed, the intermolecular chain of the polymer is broken even decomposed at high temperature; the hypersalinity condition will reduce the viscosity of the system and make the polymer flooding less effective. The polymer flooding, binary and ternary combination flooding are not suitable for developing medium and low permeability oil fields and high temperature and high salinity oil fields due to the limitations of the polymer flooding, binary and ternary combination flooding.
In summary, the conventional profile control and flooding system has the following problems: (1) poor effect: after the oil is injected into a stratum, the oil is easy to lose efficacy under the influence of factors such as high temperature, hypersalinity and the like, and cannot enter the deep part of the oil reservoir in a low-permeability oil reservoir to adjust a water injection profile and displace oil, so that the oil displacement effect is poor; (2) When the concentration of the profile control agent system is low, the injection amount required by field application is large, and complex field injection conditions are difficult to meet; (3) poor matching: the particle size of the profile control system is not matched with the pore throat size of an oil reservoir, the particle size is too large, profile control cannot be performed in smaller pore depth, the particle size is too small, the effect of adjusting a water drive profile cannot be achieved after injection, and a series of problems such as 'no injection, no blockage, no displacement' and the like are easy to occur; (4) the contradiction of 'adjusting' and 'driving' is prominent: at present, most of the design of a regulating and driving system focuses on profile control, a high-permeability channel is blocked through a bridging effect, the swept volume is increased, however, the utilization degree of a low-permeability layer oil layer with small pore size is poor, and the contradictory contradiction problem of 'regulating' and 'driving' cannot be solved.
In view of the above problems, it is urgently needed to develop a new profile control and flooding system suitable for the characteristics of low-permeability oil reservoirs.
Disclosure of Invention
In view of the above existing technologiesThe invention develops a novel nano flower-nano sheet dual-inorganic nano profile control and flooding system and application thereof. The nano-sheets in the profile control and flooding system are used as oil displacement agents, the nano-flowers are used as profile control and plugging agents, the deep profile control and flooding effect is good, and the method can be used for deep profile control and flooding of low-permeability heterogeneous oil reservoirs. The nano-sheet-nano flower dual-inorganic nano profile control and flooding system has good temperature resistance and salt resistance and is not influenced by impurities in formation water; the concentration required by field injection is small, and a relatively ideal profile control and flooding effect can be achieved by using a small amount of the profile control and flooding agent, so that complicated field injection conditions can be met; as a nano-scale profile control system, the polymer material has small particle size, good compatibility with low-permeability pore throat dimensions and good injectivity. Modified MoS 2 The nanosheet is used as an oil displacement agent, can play the roles of wedge-shaped permeation and oil gathering to form a wall, reduces the adhesion work of crude oil and rock, peels off an oil film on the rock wall of a fine pore throat and further improves the recovery ratio of the low-permeability pore throat; modified MoS 2 The nanoflowers as the plugging agent have self-aggregation capability, and can automatically aggregate to form large-size aggregates along with continuous migration in the stratum to plug deep and large pore throats and promote modified MoS 2 Deep fluid diversion occurs on the nanosheets, crude oil in a low-permeability layer is expelled, the process of migration, plugging and breakthrough is realized, and the effect of deep profile control and flooding is finally achieved. The invention initiates a nano-flower-nano-sheet dual-inorganic material nano profile control and flooding system, is formed by compounding dual inorganic nano materials, does not generate the conditions of shear failure and migration failure in a stratum, further improves the plugging capability and the oil displacement capability of the system, can effectively solve the problems in the deep profile control and flooding development process, improves the development effect of low-permeability oil reservoirs and high-temperature high-mineralization-degree heterogeneous oil reservoirs, and effectively improves the oil displacement efficiency.
In order to achieve the purpose, the invention provides the following scheme:
the invention provides a nano flower-nano sheet dual-inorganic nano profile control and flooding system, which comprises modified MoS 2 Nano flower and modified MoS 2 Nanosheets and alkylphenol ethoxylates.
Further, the modified MoS 2 Nanosheet, modified MoS 2 The mass ratio of the nanoflower to the alkylphenol ethoxylates is 1.
Further, the preparation method of the nano flower-nano sheet dual-inorganic nano profile control and flooding system comprises the following steps:
respectively weighing 0.005g of prepared modified MOS 2 Nanosheet and 0.005g modified MoS 2 Placing nanometer flower in beaker, adding formation water to 100g, and preparing 0.005wt% modified MOS 2 Nanosheets and 0.005wt% modified MoS 2 Dispersion of nanoflower according to modified MoS 2 Nanosheet: modified MoS 2 Nano flower: adding alkylphenol polyoxyethylene ether (OP-10) =1 2 Nanosheet and modified MoS 2 And (3) taking out the nano flowers after the nano flowers are completely dissolved to form a suspension, wherein the process is about 5-10 min, so that a nano flower-nano sheet dual-inorganic nano profile control and flooding system is obtained.
Further, the modified MoS 2 The preparation method of the nanoflower comprises the following steps:
(1) Mixing MoS 2 And NH 4 SCN, adding mineralized water, steaming at 180-220 deg.C under high pressure (10-12 MPa) for 12-36 h, cooling to room temperature, centrifuging, washing, and freeze drying to obtain solid MoS 2 A nanoflower;
(2) Mixing the solid MoS 2 Dispersing the nanoflower in water, and adding alkyl glycoside for primary grafting;
(3) Adding gemini quaternary ammonium salt surfactant into the mixture obtained in the step (2) for secondary grafting;
(4) Adding betaine into the mixture obtained in the step (3), carrying out grafting for three times, cooling to room temperature after grafting, washing, and dialyzing to obtain modified MoS 2 And (4) nano flowers.
Further, the MoS in the step (1) 2 And NH 4 The molar ratio of SCN is 1:4.
further, the alkyl glycoside in the step (2) has a polymerization degree of 1,R of 12 and is added in an amount of 3mmol/L, wherein R is a hydrocarbon chain length, the number of R represents a carbon number, and 3mmol/L is a unit of measurement, meaning that the alkyl glycoside is added in an amount based on the total amount of the dispersion liquid;
the reaction temperature is 150-180 ℃, and the reaction time is 12h.
Further, the addition amount of the gemini quaternary ammonium salt surfactant in the step (3) is 2mmol/L, and the gemini quaternary ammonium salt surfactant is added based on the total amount of the dispersion liquid;
the reaction temperature was raised to 200 ℃ and the reaction time was 24h.
Further, the betaine was added in an amount of 1mmol/L (based on the total amount of the dispersion) in step (4), the reaction temperature was raised to 300 ℃ and the reaction time was 24 hours.
Further, modified MoS 2 The preparation method of the nano sheet comprises the following steps:
(1) Dispersing molybdenum disulfide in water to obtain a molybdenum disulfide dispersion, dissolving hexaammonium heptamolybdate ((NH 4) in the molybdenum disulfide dispersion 6 ·Mo 7 O 24 ·4H 2 O) and thiourea, steaming and pressing for 18-25 h at the temperature of 180-220 ℃ under high pressure (10-12 MPa), cooling the solution, and freeze-drying to obtain a solid molybdenum disulfide nano flaky material;
(2) Dispersing the solid molybdenum disulfide nano flaky material in water, and adding alkyl glycoside for primary grafting;
(3) Adding a gemini quaternary ammonium salt surfactant into the mixture obtained in the step (2) for secondary grafting;
(4) Adding betaine into the mixture obtained in the step (3), carrying out grafting for three times, cooling to room temperature after grafting, washing, and dialyzing to obtain modified MoS 2 Nanosheets.
Further, in the step (1), the mass concentration of the hexaammonium heptamolybdate in the molybdenum disulfide dispersion liquid is 0.2wt% -0.6 wt%, and the mass concentration of the thiourea in the molybdenum disulfide dispersion liquid is 0.2wt% -3 wt%, wherein the mass ratio of the hexaammonium heptamolybdate to the thiourea is (1:1) - (1:5).
Further, the polymerization degree of the alkyl glycoside in the step (2) is 1,R of 12, the adding amount is 3mmol/L (based on the total amount of the dispersion liquid), the reaction temperature is 150 ℃, and the reaction time is 12h;
the addition amount of the gemini quaternary ammonium salt surfactant in the step (3) is 2mmol/L (based on the total amount of the dispersion liquid), the reaction temperature is increased to 200 ℃, and the reaction time is 24 hours;
in the step (4), the addition amount of the betaine is 1mmol/L (based on the total amount of the dispersion liquid), the reaction temperature is increased to 300 ℃, and the reaction time is 24 hours.
The invention also provides application of the profile control system in the development of low-permeability reservoirs and high-temperature and high-salinity heterogeneous reservoirs.
Aiming at the defects of the existing profile control and flooding technology, the novel nano flower-nano sheet dual-inorganic nano profile control and flooding system is provided by combining the characteristics of good dispersibility, uniform particle size, large specific surface area, strong adsorption capacity and the like of a nano material, the defect that the traditional inorganic profile control and flooding agent cannot realize deep profile control and flooding is overcome, oil can be gathered to form a wall, the adhesion work of crude oil and rock is reduced, plugging and displacement are performed alternately, the effects of enlarging microscopic wave and volume and improving oil washing efficiency are achieved, and the macro recovery rate of the crude oil is further improved. The nano flower-nano sheet dual-inorganic nano profile control and flooding system has good compatibility, can be uniformly dispersed in formation water, has good temperature resistance and salt tolerance, and can be suitable for various severe oil field environments; the concentration required by the nano flower-nano sheet dual-inorganic nano profile control and flooding system to exert the profile control and flooding functions is extremely low, the field usage amount is small, large-scale popularization and production can be carried out, and the production cost is reduced; realize "side is transferred and is driven": the nanoflowers block the high-permeability channels through self-aggregation, promote the flow regulation and steering of the nanosheets and enlarge the swept volume; meanwhile, the nano sheets can play a role in wedge-shaped penetration, an oil film is continuously stripped to form an oil slug, the follow-up liquid is driven to intelligently turn to a secondary channel, the regulation and the drive are integrated, and the oil reservoir recovery rate is greatly improved; "the entering of notes, block up": the nanometer material size ensures that the profile control and flooding system has good injection performance, and the nanoflowers form aggregates with large particle size under the self-aggregation action after being injected into a stratum to plug a high-permeability channel, thereby realizing the goal of deep profile control and flooding integration.
The invention discloses the following technical effects:
(1) The nano flower-nano sheet dual inorganic material profile control and flooding system can be widely applied to low-permeability heterogeneous oil reservoirs, has good temperature resistance and salt resistance, and can meet complex field injection conditions;
(2) The production cost is obviously reduced, the concentration of the prior art is generally more than 1000ppm, the concentration of the nano flower-nano sheet dual-inorganic material profile control and flooding system is 50ppm, the concentration required by field injection of the nano flower-nano sheet dual-inorganic material profile control and flooding system is small, and the ideal profile control and flooding effect can be achieved by using a small amount of the profile control and flooding system;
(3) The nano flower-nano sheet dual inorganic nano profile control and flooding system has smaller grain diameter, good compatibility with the pore throat size of a low-permeability oil reservoir, good injectivity, migration in a stratum, and plugging of the pore throat with large size through self-aggregation, thereby achieving the effect of 'injection-migration-plugging';
(4) The invention realizes the aim of integration of 'adjustment' and 'drive': nano-sheets in nano-flower-nano-sheet dual-inorganic nano-material profile control and flooding system are used as oil displacement agent to modify MoS 2 The nanosheet is used as an oil displacement agent, can play the roles of wedge-shaped penetration and oil gathering wall formation, reduces the adhesion work of crude oil and rock, peels off an oil film on the rock wall of a fine pore throat, and further improves the recovery ratio of the low-permeability pore throat; modified MoS 2 The nanoflowers as the plugging agent have self-aggregation capability, and can automatically aggregate to form large-size aggregates along with continuous migration in the stratum to plug deep large pore throats and promote modified MoS 2 The nano sheets generate deep liquid flow diversion to drive out crude oil in a low-permeability layer, and the nano materials continuously break through and enter a deeper stratum to plug along with the continuous increase of the injection amount, so that the effect of deep profile control and flooding is finally achieved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 shows MoS in example 1 2 FEI-SEM micrograph of nanoplatelets;
FIG. 2 shows MoS in example 1 2 Atomic force microscopy images of the nanoplatelets;
FIG. 3 shows MoS in example 1 2 The result of the wedge-shaped infiltration of the nano-sheets;
FIG. 4 shows the modified MoS of example 2 2 FEI-SEM micrograph of nanoflower material (500 μm);
FIG. 5 shows the modified MoS of example 2 2 FEI-SEM micrograph of nanoflower material (500 nm);
FIG. 6 shows the modified MoS of example 2 2 A graph of the self-aggregation rate of the nanoflower and time;
fig. 7 is the appearance change of the nano flower-nano sheet dual inorganic nano profile control and flooding system, which is the initial condition, aging for 3 days, aging for one week and aging for two weeks from left to right;
fig. 8 is a variation curve of injection pressure and recovery ratio in the displacement process of the nano flower-nano sheet dual-inorganic nano profile control and flooding system prepared in example 3.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but rather as a more detailed description of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. Further, for numerical ranges in this disclosure, it is understood that each intervening value, between the upper and lower limit of that range, is also specifically disclosed. Every intervening value, to the extent any stated value or intervening value in a stated range, and any other stated or intervening value in a stated range, is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference herein for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. The description and examples are intended to be illustrative only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including, but not limited to.
The polymerization degree of the alkyl glycoside in the embodiment of the invention is 1,R of 12.
Example 1 oil displacing agent-modified MoS 2 Nanosheet preparation
2g of molybdenum disulfide was dispersed in 98g of deionized water to obtain a molybdenum disulfide dispersion. In 100g of the molybdenum disulfide dispersion, hexaammonium heptamolybdate ((NH 4) 6 ·Mo 7 O 24 ·4H 2 O) and thiourea, (NH 4) 6 ·Mo 7 O 24 ·4H 2 The mass concentration of O in the dispersion was 0.4% by weight, and the mass concentration of thiourea in the dispersion was 0.2% by weight, wherein hexaammonium heptamolybdate (NH 4) 6 ·Mo 7 O 24 ·4H 2 The mass ratio of O to thiourea is 1:3. putting the reactant into a three-neck flask, setting the rotation speed at 200rpm, steaming and pressing for 20 hours at the temperature of 200 ℃ and 10MPa, cooling the solution, and freeze-drying to obtain solid MoS 2 A nano-platelet material. Solid state MoS 2 Distributing a plurality of active grafting sites on the surface of the nano flaky material, dispersing 4g of solid molybdenum disulfide nano flaky material into 96g of deionized water, adding 3mmol/L (based on the total liquid amount of the dispersion liquid, the same below) of alkyl glycoside for primary grafting, keeping the rotating speed at 150rpm, and reacting at 150 ℃ under normal pressure for 12 hours; then, 2mmol/L gemini quaternary ammonium salt surfactant is added into the reaction mixture, the rotating speed is kept at 200rpm, the temperature is increased to 200 ℃, and the reaction is carried out for 24 hours at high temperature and high pressureCarrying out secondary grafting of unsaturated sites; finally, 1mmol/L betaine is added into the mixture for three times of grafting, the rotation speed is kept at 300rpm, and the pressure reaction is carried out for 24 hours at 300 ℃. After cooling the solution to room temperature, the modified MoS was washed several times with water and ethanol 2 The nanosheet material is dialyzed with ultrapure water to remove unreacted reagents and other impurities to obtain a modified MoS 2 Nanosheets.
Modified MoS 2 And (3) microscopic characterization of the nanosheets:
MoS was observed by FEI-SEM microscopy 2 The FEI-SEM micrograph of the nanosheets is shown in FIG. 1, and it can be seen from FIG. 1 that the area is about 50nm × 60nm, and the nanosheets are small in size. In addition, moS is known from the atomic force microscope and the corresponding height distribution of the nanosheets (fig. 2) 2 The thickness of the nanosheets is on average about 1.2nm, i.e., moS 2 The size of the nanosheets is about 50nm by 60nm by 1.2nm.
Modified MoS 2 Wedge-shaped infiltration of the nanosheets:
the prepared modified MoS 2 Mixing the nanosheet with formation water in a ratio of 0.005wt%, 1:2, adding alkylphenol polyoxyethylene (OP-10), placing the mixture into an ultrasonic stirrer for oscillation, and ensuring that the aqueous solution and the modified MoS are mixed 2 The nanoplatelets and OP-10 were completely dissolved to form a suspension, which was about 8min. MoS 2 The result of the wedge-shaped permeation of the nanosheets is shown in FIG. 3, and from FIG. 3, the modified MoS 2 The fluid has obvious microscopic osmotic pressure, and wedge-shaped permeation is formed under the action of the microscopic osmotic pressure to generate stripping force, so that oil drops are shoveled off from the surface of the rock (no oil film is left).
EXAMPLE 2 plugging agent-modified MoS 2 Preparation of nanometer flower
0.005mol of MoS 2 And 0.020mmol NH 4 SCN was placed in a 100mL teflon lined hydrothermal reaction kettle. Preparing ultrapure water, adding inorganic salt into the ultrapure water according to different ion proportions, and preparing the ionized water with different degrees of mineralization (1000ppm, 5000ppm,10000ppm and 30000ppm). Adding mineralized water into the hydrothermal reaction kettle to 60% of the total volume, stirring for 0.5h, sealing, setting the rotation speed to be 200rpm, and autoclaving at 200 ℃ for 24h. Cooling to the chamberAfter warming, centrifugal separation, repeated washing with ultrapure water and absolute ethyl alcohol to remove unreacted reagents and other impurities, and freeze-drying to obtain solid MoS 2 And (4) nano flowers. 4g of solid MoS 2 Dispersing the nanoflower material in 96g of deionized water, adding 3mmol/L alkyl glycoside for primary grafting, keeping the rotating speed at 150 revolutions, and reacting at 150 ℃ under normal pressure for 12 hours; then, adding 2mmol/L gemini quaternary ammonium salt surfactant into the reaction mixture, keeping the rotating speed at 200rpm, raising the temperature to 200 ℃, and carrying out high-temperature high-pressure reaction for 24 hours to carry out secondary grafting of unsaturated sites; finally, 1mmol/L betaine is added into the mixture for three times of grafting, the rotation speed is kept at 300rpm, and the pressure reaction is carried out for 24 hours at 300 ℃. Cooling the solution to room temperature, washing the modified molybdenum disulfide nanosheet-shaped material with water and ethanol for multiple times, and dialyzing the material with ultrapure water to remove unreacted reagents and other impurities to obtain modified MoS 2 And (4) nano flowers.
Modified MoS 2 Microscopic characterization of the nanoflower:
the modified MoS is obtained under the hydrothermal condition with the reaction temperature of 200 ℃ and the reaction time of 24h 2 FEI-SEM micrographs of the nanoflower material are shown in FIG. 4 (500 μm) and FIG. 5 (500 nm). It can be obviously seen that the modified molybdenum disulfide chips are not simply combined but are mutually interpenetrated and mutually wrapped, and a plurality of modified molybdenum disulfide chips form nanoflowers in the reaction process. As can be seen from FIGS. 4 and 5, moS 2 The diameter of the nanoflower structure is about 500-600 nm, the thickness of the lamellar structure is about 3-4nm 2 The nano-flower structure is formed by orderly stacking a plurality of flaky petals from one center to all directions in a radioactive mode, each nano-flower is not aggregated under the dry condition, the form is stable, and the modified MoS is shown 2 The nanometer flower has better dispersibility under the dry condition.
Modified MoS 2 The self-aggregation performance of the nanoflower is as follows:
modified MoS 2 The particle size of the nanoflower is far smaller than the pore throat diameter of the oil reservoir, and the nanoflower can be transported to the deep part of the oil reservoir. Modified MoS 2 The nanoflower has a self-aggregation effect, and the graph of the self-aggregation rate and the time is shown in FIG. 6. By modifying MoS 2 Self-aggregation of nanoflowerThe oil-water-retention agent can be transported to a deep zone of a high-permeability layer of a low-permeability reservoir within a specified time, and an aggregate (cluster structure) with a larger size is formed to block pore throats and block water channeling channels of the high-permeability layer.
Example 3 nanoflower-nanosheet dual inorganic nano profile control and flooding system preparation
Respectively weighing 0.0025g of prepared modified MOS 2 Nanosheet and 0.0025g modified MoS 2 Placing nanometer flower in beaker, adding formation water to 100g, and preparing 0.0025wt% (25 ppm) modified MOS 2 Nanosheets and 0.0025wt% (i.e., 25 ppm) modified MoS 2 Nanoflower, nanodispersion at a total concentration of 0.005wt% (50 ppm) and as nanoplatelets: and (3) nano flowers: alkylphenol ethoxylates (OP-10) =1:1:2, adding alkylphenol polyoxyethylene ether, placing into an ultrasonic stirrer for oscillation to ensure that the modified MOS is 2 Nanosheet and modified MoS 2 And (3) taking out the nano flowers after the nano flowers are completely dissolved to form a suspension, wherein the process is about 8min, so that a nano flower-nano sheet dual-inorganic nano profile control and flooding system is obtained.
The nano flower-nano sheet double inorganic nano profile control and flooding system has the following performance characteristics:
1. degree of mineralization water compatibility:
the nanoflower-nanosheet dual-inorganic profile control and flooding system prepared in example 3 is compounded with formation water with different degrees of mineralization, the pH values of the systems are all stabilized at about 7, and the viscosity of the profile control and flooding agent is 3mPa & s. The nano flower-nano sheet dual-inorganic nano profile control and flooding system has no phenomena of precipitation, flocculation, discoloration and the like, and can be used for low-permeability oil reservoirs with high mineralization degree. The test data are shown in table 1.
TABLE 1 basic Properties of the nanoflower-nanosheet Dual inorganic Profile control and flooding System
2. Temperature resistance:
the nano flower-nano sheet dual-inorganic nano profile control and flooding system just prepared in the embodiment 3 is placed in four test tubes, a port is sealed, 20mL of profile control and flooding agent is placed in each test tube, the test tubes are placed in a 120 ℃ oven, after aging for two weeks, whether the reagents have the phenomena of precipitation, flocculation, discoloration and the like is observed, and the appearance change of the nano flower-nano sheet dual-inorganic nano profile control and flooding system is shown in a figure 7 (from left to right, the initial conditions, aging for 3 days, aging for one week and aging for two weeks are sequentially adopted). The experimental result shows that the appearance of the nano flower-nano sheet dual inorganic nano profile control and flooding system is not changed, which shows that the nano flower-nano sheet dual inorganic nano profile control and flooding system has stronger high-temperature stability and can be used for low-permeability oil reservoirs with higher temperature.
Dynamic profile control and flooding characteristics of nanoflower-nanosheet double-inorganic-nanometer profile control and flooding system
1. Single tube profile control experiment
A core model of a single sand-filled pipe is manufactured, and the plugging performance and the recovery efficiency improving effect of a nano flower-nano sheet dual-inorganic nano profile control system (taking the example prepared in example 3) are inspected through the dynamic change of the injection pressure and the characteristics of oil production and water production of the core in the deep profile control process.
The experimental steps are as follows:
(1) And (3) manufacturing a sand-filled pipe core model with the permeability of 30mD according to requirements, wherein the porosity is 23.94%. Vacuumizing, saturating formation water, measuring the permeability of a rock core by water, and aging saturated formation crude oil in a 65 ℃ oven for 24 hours;
(2) Performing primary water drive at the injection rate of 0.2mL/min until the water content at the outlet end reaches 95%, and recording the injection pressure, the oil production and the water production;
(3) Injecting the nano flower-nano sheet dual-inorganic nano profile control and flooding system at an injection rate of 0.2mL/min until the water content at the outlet end reaches 95%;
(4) And performing subsequent water flooding at the injection rate of 0.2mL/min until the water content at the outlet end reaches 98%, and recording the injection pressure, the oil production and the water production.
The prepared nanoflower-nanosheet inorganic nano profile control and flooding system has good injectability in the experimental process, mainly reflects that no advection pump pressure building phenomenon occurs in the injection process, and no accumulation phenomenon occurs on the injection end face of the sand filling pipe after the experiment is finished, so that the nanoflower-nanosheet inorganic nano profile control and flooding system can smoothly enter the core of the sand filling pipe. FIG. 8 is a variation curve of injection pressure and recovery ratio during displacement, from which it can be seen that in the primary water flooding stage, the injection pressure reaches a stable value at a relatively fast speed, and the stable pressure value is about 0.5MPa; after the profile control agent is injected, the injection pressure is rapidly increased to the maximum value of 4.5MPa, which is about 9 times of that of primary water flooding. The results show that the nanoflower-nanosheet inorganic nano profile control and flooding system can effectively block pore throats and increase seepage resistance. The recovery ratio curve shows that when the primary water drive is finished, the recovery ratio is only 27 percent, which indicates that the water drive has serious channeling and forms a main flow channel of the water drive, so that most of crude oil cannot be driven out; after the nano flower-nano sheet inorganic nano profile control and flooding system is injected for profile control and flooding, the recovery ratio gradually rises, and finally is kept at 50%, and the rising amplitude reaches 20%. The improvement of the recovery ratio shows that the nano flower-nano sheet inorganic nano profile control and flooding system has obvious profile control and flooding effects, on one hand, the profile control effect of the nano flowers blocks a main flow channel, the swept volume of an injected fluid is increased, and on the other hand, the wedge-shaped permeability and the high surface activity of the nano sheets improve the oil displacement efficiency of a low-permeability layer.
2. Double-pipe driving and regulating experiment
The core model of the parallel sand-filled pipe is manufactured, the heterogeneous condition of an oil reservoir is simulated, and the selective plugging and shunting performance of the nanoflower-nanosheet profile control and flooding system in the heterogeneous reservoir and the scouring resistance after plugging are inspected by adopting a co-injection and separate mining mode.
The experimental steps are as follows:
(1) The permeability of the upper layer is 30mD, and the permeability grade difference is 1:2. 1:3. 1:5. 1:7, respectively vacuumizing the parallel sand filling pipe core model, and starting a displacement process after the initial permeability of saturated formation water and saturated formation crude oil is measured by water;
(2) After the water content of the outlet end reaches 95% through primary water flooding, a nanoflower-nanosheet inorganic nano profile control and flooding system is injected until the water content of the outlet end reaches 95%;
(3) And (5) performing subsequent water drive until the water content at the outlet end reaches 98%. In the experimental process, the liquid production amount, the flow rate and the recovery ratio of the high-permeability pipe and the low-permeability pipe are respectively recorded and calculated.
The experimental results are as follows:
the core parameters and the shunt experiment results of the sand-filled pipe with different permeability grade differences are shown in table 2, and it can be seen that: for a difference in permeability level of 1:2. 1:3. 1:5. 1:7, the total recovery ratio of the primary water flooding is 47.25%, 39.53%, 37.69% and 36.42% in sequence, the total recovery ratio is increased to 63.19%, 62.57%, 61.09% and 58.40% in sequence after the nanoparticle system is injected, and the recovery ratio of the low-permeability pipe is higher than that of Gao Shenguan, which shows that the nano flower-nano sheet profile control system can preferentially block the high-permeability layer, effectively improve the swept volume and the oil washing efficiency of the low-permeability layer, thereby greatly improving the total recovery ratio of the heterogeneous reservoir, and the improved recovery ratio is mainly from the low-permeability layer; in addition, along with the increase of the permeability grade difference, the improvement amplitude of the whole recovery ratio is increased firstly and then reduced, which shows that the nano flower-nano sheet profile control and flooding system has certain selectivity on the permeability grade difference, and the proper permeability grade difference can better play the profile control and flooding role of the nano flower-nano sheet profile control and flooding system.
Table 2 different permeability level differences of parallel sand-packed pipe core parameters and diversion experiment results
Example 4
Oil displacing agent-modified MoS 2 The preparation method of the nano-sheet comprises the following steps:
1g of molybdenum disulfide was dispersed in 99g of deionized water to obtain a molybdenum disulfide dispersion. In 100g of the molybdenum disulfide dispersion, hexaammonium heptamolybdate ((NH 4) 6 ·Mo 7 O 24 ·4H 2 O) and thiourea, (NH 4) 6 ·Mo 7 O 24 ·4H 2 The mass concentration of O in the dispersion was 0.2wt%, and the mass concentration of thiourea in the dispersion was 0.2wt%, wherein hexaammonium heptamolybdate (NH 4) 6 ·Mo 7 O 24 ·4H 2 The mass ratio of O to thiourea is 1:1. putting the reactant into a three-neck flask, setting the rotating speed at 200rpm, steaming and pressing for 25 hours at the temperature of 220 ℃ and 10MPa, cooling the solution, and freeze-drying to obtain solid MoS 2 A nano-platelet material. Solid state MoS 2 Distributing a plurality of active grafting sites on the surface of the nano flaky material, dispersing 5g of solid molybdenum disulfide nano flaky material in 95g of deionized water, adding 3mmol/L alkyl glycoside for primary grafting, keeping the rotation speed at 150rpm, and reacting at 150 ℃ under normal pressure for 12h; then, adding 2mmol/L gemini quaternary ammonium salt surfactant into the reaction mixture, keeping the rotating speed at 200rpm, raising the temperature to 200 ℃, and carrying out high-temperature high-pressure reaction for 24 hours to carry out secondary grafting of unsaturated sites; finally, 1mmol/L betaine is added into the mixture for three times of grafting, the rotation speed is kept at 300rpm, and the pressure reaction is carried out for 24 hours at 300 ℃. After cooling the solution to room temperature, the modified MoS was washed several times with water and ethanol 2 The nano flaky material is dialyzed by ultrapure water to remove unreacted reagents and other impurities, thus obtaining the modified MoS 2 Nanosheets.
The modified MoS prepared in this example was tested in the same manner as in example 1 2 Wedge-shaped penetration of the nanoplates, similar to example 1, results modified MoS 2 The fluid has obvious microscopic osmotic pressure, and wedge-shaped permeation is formed under the action of the microscopic osmotic pressure to generate stripping force, so that oil drops are shoveled off from the surface of the rock (no oil film is left).
Plugging agent-modified MoS 2 The preparation method of the nanoflower is the same as that of example 2.
The preparation method of the nano flower-nano sheet double inorganic nano profile control and flooding system is the same as that in example 3.
Example 5
Oil displacing agent-modified MoS 2 The preparation method of the nano-sheet comprises the following steps:
3g of molybdenum disulfide was dispersed in 97g of deionized water to obtain a molybdenum disulfide dispersion. In 100g of the molybdenum disulfide dispersion, hexaammonium heptamolybdate ((NH 4) 6 ·Mo 7 O 24 ·4H 2 O) and thiourea, (NH 4) 6 ·Mo 7 O 24 ·4H 2 The mass concentration of O in the dispersion liquid was 0.6wt%, and the mass of thiourea in the dispersion liquidAt a concentration of 3% by weight, hexaammonium heptamolybdate (NH 4) 6 ·Mo 7 O 24 ·4H 2 The mass ratio of O to thiourea is 1:5. putting the reactant into a three-neck flask, setting the rotation speed at 200rpm, steaming and pressing for 18 hours at the temperature of 180 ℃ under 12MPa, cooling the solution, and freeze-drying to obtain solid MoS 2 A nano-platelet material. Solid state MoS 2 Distributing a plurality of active grafting sites on the surface of the nano flaky material, dispersing 3g of solid molybdenum disulfide nano flaky material in 97g of deionized water, adding 3mmol/L alkyl glycoside for primary grafting, keeping the rotation speed at 150rpm, and reacting at 150 ℃ under normal pressure for 12h; then, adding 2mmol/L gemini quaternary ammonium salt surfactant into the reaction mixture, keeping the rotating speed at 200rpm, raising the temperature to 200 ℃, and carrying out high-temperature high-pressure reaction for 24 hours to carry out secondary grafting of unsaturated sites; finally, 1mmol/L betaine is added into the mixture for three times of grafting, the rotation speed is kept at 300rpm, and the pressure reaction is carried out for 24 hours at 300 ℃. After cooling the solution to room temperature, the modified MoS was washed several times with water and ethanol 2 The nanosheet material is dialyzed with ultrapure water to remove unreacted reagents and other impurities to obtain a modified MoS 2 Nanosheets.
The modified MoS prepared in this example was tested in the same manner as in example 1 2 Wedge-shaped penetration of the nanoplates, similar to example 1, results modified MoS 2 The fluid has obvious microscopic osmotic pressure, and wedge-shaped permeation is formed under the action of the microscopic osmotic pressure to generate stripping force, so that oil drops are shoveled off from the surface of the rock (no oil film is left).
Plugging agent-modified MoS 2 The preparation method of the nanoflower is the same as that of example 2.
The preparation method of the nano flower-nano sheet double inorganic nano profile control and flooding system is the same as that in example 3.
The different permeability level differences of the nano flower-nano sheet dual inorganic nano profile control and flooding system in the embodiment 4 and the embodiment 5 are tested, the core parameters of the sand-packed pipe and the diversion results are connected in parallel, the testing method is the same as that in the embodiment 3, the results in the embodiment 4 are shown in table 3, and the results in the embodiment 5 are shown in table 4.
TABLE 3 core parameters of parallel sand-packed pipes with different permeability grade differences and flow distribution experiment results
Table 4 different permeability level differences of parallel sand-packed pipe core parameters and diversion experiment results
The above-described embodiments are only intended to illustrate the preferred embodiments of the present invention, and not to limit the scope of the present invention, and various modifications and improvements made to the technical solution of the present invention by those skilled in the art without departing from the spirit of the present invention should fall within the protection scope defined by the claims of the present invention.
Claims (8)
1. A nano flower-nano sheet dual inorganic nano profile control and flooding system is characterized by comprising modified MoS 2 Nano flower and modified MoS 2 Nanosheets and alkylphenol ethoxylates;
the modified MoS 2 Nanosheet and modified MoS 2 The mass ratio of the nanoflower to the alkylphenol ethoxylates is 1;
the modified MoS 2 The preparation method of the nanoflower comprises the following steps:
(1) Will MoS 2 And NH 4 SCN, adding mineralized water, autoclaving at 180-220 ℃ for 12-36 h, cooling to room temperature, centrifuging, washing, and freeze-drying to obtain solid MoS 2 A nanoflower;
(2) Mixing the solid MoS 2 Dispersing the nanoflower in water, and adding alkyl glycoside for primary grafting;
(3) Adding gemini quaternary ammonium salt surfactant into the mixture obtained in the step (2) for secondary grafting;
(4) Adding betaine into the mixture obtained in the step (3), carrying out grafting for three times, cooling to room temperature after grafting, washing, and dialyzing to obtain modified MoS 2 Nano flower;
the modified MoS 2 The preparation method of the nano sheet comprises the following steps:
(1) Dispersing molybdenum disulfide in water to obtain a molybdenum disulfide dispersion liquid, dissolving hexaammonium heptamolybdate and thiourea in the molybdenum disulfide dispersion liquid, carrying out high-pressure autoclaved treatment at the temperature of 180-220 ℃ for 18-25 h, cooling the solution, and freeze-drying to obtain a solid molybdenum disulfide nano flaky material;
(2) Dispersing the solid molybdenum disulfide nano flaky material in water, and adding alkyl glycoside for primary grafting;
(3) Adding gemini quaternary ammonium salt surfactant into the mixture obtained in the step (2) for secondary grafting;
(4) Adding betaine into the mixture obtained in the step (3), carrying out grafting for three times, cooling to room temperature after grafting, washing, and dialyzing to obtain modified MoS 2 A nanosheet.
2. The profile control and flooding system according to claim 1, characterized in that in modified MoS 2 In the preparation method of the nanoflower, the MoS is prepared in the step (1) 2 And NH 4 The molar ratio of SCN is 1:4; the high pressure is 10-12 MPa.
3. The profile control and flooding system according to claim 1, characterized in that the modified MoS 2 In the preparation method of the nanoflower, the polymerization degree of the alkyl glycoside in the step (2) is 1, the length of a hydrocarbon chain is 12, and the adding amount is 3mmol/L;
the reaction temperature is 150-180 ℃, and the reaction time is 12h.
4. The profile control and flooding system according to claim 1, characterized in that in modified MoS 2 In the preparation method of the nanoflower, the addition amount of the gemini quaternary ammonium salt surfactant in the step (3) is 2mmol/L;
the reaction temperature is 200 ℃, and the reaction time is 24h.
5. The profile control and flooding system according to claim 1, characterized in that in modified MoS 2 In the preparation method of the nanoflower, the addition amount of the betaine in the step (4) is 1mmol/L, the reaction temperature is raised to 300 ℃, and the reaction time is 24 hours.
6. The profile control and flooding system according to claim 1, characterized in that in modified MoS 2 In the preparation method of the nanosheet, in the step (1), the mass concentration of the hexaammonium heptamolybdate in the molybdenum disulfide dispersion liquid is 0.2-0.6 wt%, and the mass concentration of the thiourea in the molybdenum disulfide dispersion liquid is 0.2-3 wt%, wherein the mass ratio of the hexaammonium heptamolybdate to the thiourea is (1:1) - (1:5); the high pressure is 10-12 MPa.
7. The profile control and flooding system according to claim 1, characterized in that in modified MoS 2 In the preparation method of the nanosheet, the polymerization degree of the alkyl glycoside in the step (2) is 1, the length of the hydrocarbon chain is 12, the adding amount is 3mmol/L, the reaction temperature is 150-180 ℃, and the reaction time is 12h;
in the step (3), the addition amount of the gemini quaternary ammonium salt surfactant is 2mmol/L, the reaction temperature is raised to 200 ℃, and the reaction time is 24 hours;
in the step (4), the addition amount of the betaine is 1mmol/L, the reaction temperature is increased to 300 ℃, and the reaction time is 24 hours.
8. The profile control and flooding system according to any one of claims 1 to 7 is applied to the development of low-permeability reservoirs and high-temperature and high-salinity heterogeneous reservoirs.
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