CN115991982A - Ultra-small-size active nano fluid and preparation method and application thereof - Google Patents
Ultra-small-size active nano fluid and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses an ultra-small-size active nano fluid, which consists of 0.05-0.2 wt% of ultra-small-size active nano silicon dots and water. A method for preparing ultra-small active nano-fluid comprises (1) preparing ultra-small active nano-silicon dot solid powder; (2) Dissolving the ultra-small-size active nano silicon dot solid powder in water to prepare mother solution; (3) Adding water into the mother solution under the stirring condition, and diluting the mother solution to the concentration of 0.05-0.2 wt%. The application of the ultra-small-size active nano fluid in low-permeability reservoir oil displacement agents. The invention has the following beneficial effects: (1) The low permeability oil is high in matching with the Tibetan microporous throat, easy to enter the nano microporous throat and small in damage to the microporous throat; (2) The high interfacial activity can obviously reduce the oil-water interfacial tension and improve the recovery degree of the low-permeability oil reservoir; (3) the oil film stripping efficiency is higher; (4) environmental protection, self-dispersion and easy preparation.
Description
Technical Field
The invention relates to an ultra-small-size active nano fluid and a preparation method and application thereof, and belongs to the technical field of oil and gas field development engineering.
Background
The specific gravity of low-permeability oil reservoirs in petroleum reserves is larger, the geological reserves of petroleum are cumulatively detected nationally, the low-permeability oil reservoirs are about 141 hundred million tons, and the ratio of the low-permeability oil reservoirs reaches 49%. The residual oil resource amount is 799 hundred million tons, wherein the ratio of the low-permeability oil reservoir to the total amount of the residual oil resource is up to 54 percent, and the ratio of the low-permeability oil reservoir to the total amount of the residual oil resource in the crude oil yield is increased year by year.
The reservoir physical properties and crude oil physical properties of the low-permeability oil reservoir are relatively poor, the oil-containing area is controlled by various geological factors, and the oil-gas-water distribution, the oil layer physical properties, the crude oil properties and the crack development degree have great differences in different areas. As the pore throat of the low-permeability reservoir matrix is mostly in micro-nano scale (50-900 nm), the capillary effect is remarkable, the oil/water/solid interface effect in the confined space is remarkable, the fluid flow resistance is high, the matrix energy is difficult to supplement, the phenomenon that the injection is not carried out and the extraction is not carried out is shown, and the use efficiency of the crude oil with the matrix pores is low. And as the proportion of deep low-permeability oil reservoirs increases year by year, the oil reservoir conditions have the rigor characteristics of high temperature and high salt, and the high-efficiency development of the low-permeability oil reservoirs faces a great challenge.
The low-permeability oil reservoir in China has abundant resources, but due to the characteristics of low porosity, small pore throat, poor seepage capability and the like, the conventional chemical flooding is difficult to be applied, for example, the polymer has large molecular size, and the pore throat is easy to be seriously blocked; thermal and chemical degradation at high temperatures causes severe loss of polymer viscosity; the surfactant stratum has large adsorption quantity, is sensitive to high-temperature and high-mineralization reservoirs, is easy to hydrolyze, and has the effect that the effectiveness is difficult to exert. Therefore, there is a need to find new high-performance materials to solve the above problems, so as to be suitable for efficient development of low-permeability reservoirs with high temperature, high mineralization degree and other complex conditions.
The nano material can solve the engineering problem which cannot be solved or is difficult to solve in the traditional petroleum exploitation field due to the special performance, particularly the self nano effect. The nano material has small size effect, surface effect, wetting characteristic and shear thickening characteristic, and unique heat, force, magnetism, chemistry and other properties, and has wide application prospect in the field of improving oil and gas recovery ratio. The main mechanism is to generate structure separation pressure, change rock wettability, reduce oil-water interfacial tension, inhibit particle migration and the like. The nano particles not only have good temperature resistance and salt resistance, but also have the particle size of nano-scale, and can pass through the nano-scale pore throat of the low-permeability oil reservoir, and the unique characteristics of the nano particles can just solve the problems existing in the conventional chemical flooding well, so that the nano particles have great potential in the application of the low-permeability oil reservoir enhanced recovery technology.
Disclosure of Invention
Aiming at the defects of the prior art, the invention discloses an ultra-small-size active nano fluid and a preparation method and application thereof. The invention plays the oil displacement role of the nano fluid and provides a new solution for improving the recovery ratio of the low-permeability oil reservoir.
The ultra-small-size active nano silicon dots are compared with the conventional nano SiO 2 The fluid has smaller size (particle size is 3-5 nm), has higher matching property with low permeability oil deposit, high interfacial activity and good water dispersibility, is little affected by the oil deposit environment, can provide a new method for improving the recovery ratio of the low permeability oil deposit,
the technical scheme is as follows: an ultra-small size active nanofluid, consisting of:
the content of the ultra-small-size active nano silicon dots is 0.05 to 0.2 weight percent;
the balance being water.
Further, the water contains K + 、Na + 、Mg 2+ 、Ca 2+ And Cl - Wherein K is + 、Na + The total concentration is 1000-30000 mg/L, ca 2+ And Mg (magnesium) 2+ The total concentration is 100-2000 mg/L, and the total mineralization degree is 2000-60000 mg/L.
Further, the content of the ultra-small-sized active nano silicon dots is 0.1wt% and the content of water is 99.9wt%.
Further, the particle size of the ultra-small-size active nano silicon dots is 3-5 nm.
A method for preparing an ultra-small-sized active nano fluid, which comprises the following steps:
(1) Preparing ultra-small-size active nano silicon dot solid powder;
(2) Dissolving the ultra-small-size active nano silicon dot solid powder in water to prepare ultra-small-size active nano silicon dot mother liquor for later use;
(3) Adding water into the ultra-small-size active nano silicon dot mother solution under the stirring condition, and diluting to the concentration of 0.05-0.2 wt%.
Further, the step (1) includes, in parts by mass:
(11) Dissolving 0.3-0.5 part of trisodium citrate in 7-9 parts of ultrapure water, introducing nitrogen for protection, then adding 1.5-2.5 parts of 3-aminopropyl trimethoxy silane, and stirring uniformly at room temperature to obtain a mixed solution; adding the mixed solution into a high-pressure reaction kettle, heating to 100-240 ℃, and reacting for 1.5-48 hours to obtain an ultra-small-size nano silicon dot solution;
(12) Adding 8-12 parts of glutaraldehyde aqueous solution with the concentration of 20-30 wt% and 2-4 parts of p-phenylenediamine into 35-45 parts of ultrapure water, stirring for 5-10 hours at room temperature, adding the ultra-small-size nano silicon dot solution obtained in the step (11), and continuing stirring for 5-10 hours at room temperature to obtain a mixed solution;
(13) Adding 4-6 parts of sodium sulfanilate and 8-12 parts of glutaraldehyde into the mixed solution obtained in the step (12), continuously stirring for 5-10 hours at room temperature, and freeze-drying to obtain the ultra-small-size active nano silicon dot solid powder.
The application of the ultra-small-size active nano fluid in low-permeability reservoir oil displacement agents.
Further, the reservoir temperature of the low permeability reservoir is 60-120 ℃.
The ultra-small-size active nano fluid suitable for low-permeability reservoir oil displacement provided by the invention has the following characteristics: the particle size is 3-5nm, the matching property of the ultra-small size and the nano-micro pore throat of the low-permeability oil reservoir is high, the interfacial activity is high, the oil-water interfacial tension can be reduced, and the viscoelasticity modulus of the interfacial film is enhanced; the oil film stripping efficiency is improved by 40% compared with that of water, and the extraction degree of the low-permeability oil reservoir can be improved by more than 15%.
The beneficial effects are that: the beneficial effects of the invention are as follows:
(1) The active nano fluid oil displacement agent suitable for low-permeability reservoir oil displacement provided by the invention has the characteristics of ultra-small size (particle size is 3-5 nm), high matching property with low-permeability oil Tibetan micropore throat, easiness in entering the nano micropore throat and small damage to the pore throat.
(2) The active nano fluid oil displacement agent suitable for low-permeability oil reservoir oil displacement has high interfacial activity, can obviously reduce oil-water interfacial tension and improves the extraction degree of low-permeability oil reservoirs.
(3) The active nano fluid oil displacement agent suitable for low-permeability reservoir oil displacement provided by the invention has the advantages that the oil film stripping efficiency is improved by more than 60% compared with pure water, and is improved by more than 20% compared with a surfactant.
(4) The ultra-small-size active nano fluid suitable for low-permeability reservoir oil displacement is environment-friendly, self-dispersible and easy to prepare.
Drawings
FIG. 1 is an XPS energy spectrum of an ultra-small size active nano-silicon spot.
Fig. 2 is an infrared spectrogram of an ultra-small-sized active nano-silicon dot.
Fig. 3 is a High Resolution Transmission Electron Microscope (HRTEM) image of ultra-small size active nano-silicon dots.
Fig. 4 is a dynamic light scattering nano-particle size analysis (DLS) of ultra-small size active nano-silicon dots.
Fig. 5 is a schematic diagram of oil film peel test results for ultra-small size active nanofluids.
Fig. 6 is a graph of interfacial tension versus concentration for ultra-small size active nanofluids and simulated oil.
FIG. 7 is a graph of the viscoelastic modulus of ultra-small size reactive nanofluids and simulated oil versus the concentration of ultra-small size reactive nanofluids.
Fig. 8a is a schematic diagram of a core displacement process for ultra-small size active nanofluids.
Fig. 8b is a schematic diagram of experimental results of core displacement of ultra-small size active nanofluids.
FIG. 9 is a schematic diagram of the low field nuclear magnetic test results of an ultra-small size reactive nanofluid flooding process.
The specific embodiment is as follows:
the following detailed description of specific embodiments of the invention.
The experimental methods used in the examples below are conventional methods unless otherwise specified. Materials, reagents and the like used in the examples below are commercially available unless otherwise specified.
Example 1
An ultra-small size active nanofluid, consisting of: the content of the ultra-small-size active nano silicon dots is 0.1wt%;
the balance being water.
The water contains K + 、Na + 、Mg 2+ 、Ca 2+ And Cl - Wherein K is + 、Na + The total concentration is 20000mg/L, ca 2+ And Mg (magnesium) 2+ The total concentration is 1000mg/L and the total degree of mineralization is 30000mg/L.
Example 2
An ultra-small size active nanofluid, consisting of: the content of the ultra-small-size active nano silicon dots is 0.05wt%;
the balance being water.
The water contains K + 、Na + 、Mg 2+ 、Ca 2+ And Cl - Wherein K is + 、Na + The total concentration is 1000mg/L, ca 2+ And Mg (magnesium) 2+ The total concentration is 100mg/L and the total mineralization degree is 2000mg/L.
Example 3
An ultra-small size active nanofluid, consisting of: the content of the ultra-small-size active nano silicon dots is 0.2wt%;
the balance being water.
The water contains K + 、Na + 、Mg 2+ 、Ca 2+ And Cl - Wherein K is + 、Na + The total concentration is 30000mg/L, ca 2+ And Mg (magnesium) 2+ The total concentration is 2000mg/L and the total mineralization degree is 60000mg/L.
Example 4: ultra-small-size active nano silicon point characterization for low-permeability reservoir oil displacement
Characterizing the ultra-small-size active nano-silicon dot solid powder by XPS and infrared spectroscopy, and analyzing the element composition of the ultra-small-size active nano-silicon dot and the surface group composition of the ultra-small-size active nano-silicon dot, as shown in figures 1 and 2;
the 0.1wt% of the ultra-small-sized active nano fluid prepared in example 1 was used for testing HRTEM and DLS, and the micro morphology and the particle size distribution of the ultra-small-sized active nano silicon dots were analyzed, as shown in FIGS. 3 and 4, wherein the particle size of the HRTEM is 2-4 nm, the HRTEM is in a spherical structure, and the hydration particle size is 3-5 nm.
Example 5: ultra-small-size active nano fluid oil film stripping evaluation for low-permeability reservoir oil displacement
The method comprises the steps of respectively preparing ultrapure water, petroleum sodium sulfonate with the concentration of 0.1wt%, AES with the concentration of 0.1wt%, sodium dodecyl benzene sulfonate with the concentration of 0.1wt% and ultra-small-size active nano fluid with the concentration of 0.1wt% into five oil displacement agents, recording oil film stripping experimental phenomena at different moments by using a high-definition camera at 50 ℃, and calculating oil film stripping efficiency by using image J. The oil film peeling results are shown in table 1 and fig. 5.
TABLE 1
As can be seen from table 1 and fig. 5: the oil film stripping efficiency of the ultra-small-size active nano fluid is higher than that of the surfactant with the same concentration, and the final oil film stripping rate is higher than that of the surfactant with the same concentration by more than 25%, so that the potential of improving the crude oil recovery ratio is higher.
Example 6: interfacial activity of ultra-small size active nanofluids
Ultra-small size active nanofluids with concentrations of 0wt%, 0.01wt%, 0.05wt%, 0.1wt%, 0.2wt%, and 0.5wt% were prepared, and interface tensions of simulated oil, n-hexane and the ultra-small size active nanofluids with different concentrations were tested at 60 ℃, as shown in table 3 and fig. 6.
The interfacial elastic modulus of the simulated oil with various concentrations (0, 0.01wt%,0.1wt%,0.5 wt%) of ultra-small size active nanofluids was tested at 60 ℃ and the results are shown in fig. 7.
TABLE 3 Table 3
| Concentration/ |
0 | 0.01 | 0.05 | 0.1 | 0.2 | 0.5 | 1.0 |
| Simulated oil interfacial tension/(mN/m) | 34.38 | 27.63 | 19.74 | 13.596 | 10.54 | 9.73 | 9.213 |
| N-hexane interfacial tension/(mN/m) | 40.30 | 30.43 | 21.03 | 14.14 | 12.02 | 10.35 | 9.66 |
From table 3, fig. 6 and fig. 7, it is clear that the ultra-small-sized active nano-fluid can reduce the interfacial tension of oil and water, can improve the viscoelastic modulus of oil and water interface, and has better interfacial activity.
Example 7: ultra-small-size active nano fluid core displacement experiment
The spontaneous imbibition method in the literature is used for evaluating imbibition and oil discharge capacity,
the experimental steps are as follows:
(1) the outcrop hypotonic core is respectively called dry mass, and the permeability and the porosity of the air measurement core are respectively measured;
(2) vacuumizing saturated simulated oil of a saturated stratum;
(3) the outcrop core is respectively called wet mass;
(4) at 60 ℃, water is firstly injected for displacement, and after the water displacement is finished;
(5) 0.1wt% of an ultra-small size active nanofluid is injected for displacement. The displacement flow diagram is shown in fig. 8 a;
(6) and reading the volume of the oil displacement at different times, and calculating the recovery ratio. Experimental results fig. 8b.
The result shows that the recovery ratio of the core is improved by 15.8% compared with water, the core has better oil displacement capability, and the recovery ratio of the low-permeability oil reservoir can be obviously improved.
Example 8: low field nuclear magnetic experiment of ultra-small size active nano fluid
As example 7 saturated core method is consistent, 0.1wt% of ultra-small size active nanofluid is prepared by heavy water, and the change of T2 spectrum at different displacement moments is tested by on-line low-field nuclear magnetism; the experimental results are shown in FIG. 9. The experimental results show that: the ultra-small-size active nano fluid can effectively use crude oil in small and medium pores, thereby effectively improving the recovery ratio of the hypotonic oil reservoir.
Example 9
A method for preparing an ultra-small-sized active nano fluid, which comprises the following steps:
(1) Preparing ultra-small-size active nano silicon dot solid powder;
(2) Dissolving the ultra-small-size active nano silicon dot solid powder in water to prepare ultra-small-size active nano silicon dot mother liquor for later use;
(3) Adding water into the ultra-small-size active nano silicon dot mother solution under the stirring condition, and diluting to the concentration of 0.05 wt%.
Further, the step (1) includes, in parts by mass:
(11) Dissolving 0.3 part of trisodium citrate in 7 parts of ultrapure water, introducing nitrogen for protection, then adding 1.5 parts of 3-aminopropyl trimethoxysilane, and stirring uniformly at room temperature to obtain a mixed solution; adding the mixed solution into a high-pressure reaction kettle, heating to 100 ℃, and reacting for 48 hours to obtain an ultra-small-size nano silicon dot solution;
(12) Adding 8 parts of glutaraldehyde water solution with the concentration of 20wt% and 2 parts of p-phenylenediamine into 35 parts of ultrapure water, stirring for 5 hours at room temperature, adding the ultra-small-size nano silicon dot solution obtained in the step (11), and continuing stirring for 5 hours at room temperature to obtain a mixed solution;
(13) Adding 4 parts of sodium sulfanilate and 8 parts of glutaraldehyde into the mixed solution obtained in the step (12), continuously stirring for 5 hours at room temperature, and freeze-drying to obtain the ultra-small-size active nano silicon dot solid powder.
The application of the ultra-small-size active nano fluid in low-permeability reservoir oil displacement agents.
Still further, the reservoir temperature of the low permeability reservoir is 60 ℃.
Example 10
A method for preparing an ultra-small-sized active nano fluid, which comprises the following steps:
(1) Preparing ultra-small-size active nano silicon dot solid powder;
(2) Dissolving the ultra-small-size active nano silicon dot solid powder in water to prepare ultra-small-size active nano silicon dot mother liquor for later use;
(3) Adding water into the ultra-small-size active nano silicon dot mother solution under the stirring condition, and diluting to the concentration of 0.2 wt%.
Further, the step (1) includes, in parts by mass:
(11) Dissolving 0.5 part of trisodium citrate in 9 parts of ultrapure water, introducing nitrogen for protection, then adding 2.5 parts of 3-aminopropyl trimethoxysilane, and stirring uniformly at room temperature to obtain a mixed solution; adding the mixed solution into a high-pressure reaction kettle, heating to 240 ℃, and reacting for 48 hours to obtain an ultra-small-size nano silicon dot solution;
(12) Adding 12 parts of glutaraldehyde water solution with the concentration of 30wt% and 4 parts of p-phenylenediamine into 45 parts of ultrapure water, stirring for 10 hours at room temperature, adding the ultra-small-size nano silicon dot solution obtained in the step (11), and continuing stirring for 10 hours at room temperature to obtain a mixed solution;
(13) Adding 6 parts of sodium sulfanilate and 12 parts of glutaraldehyde into the mixed solution obtained in the step (12), continuously stirring at room temperature for 10 hours, and freeze-drying to obtain the ultra-small-size active nano silicon dot solid powder.
The application of the ultra-small-size active nano fluid in low-permeability reservoir oil displacement agents.
Still further, the reservoir temperature of the low permeability reservoir is 120 ℃.
Example 11
A method for preparing an ultra-small-sized active nano fluid, which comprises the following steps:
(1) Preparing ultra-small-size active nano silicon dot solid powder;
(2) Dissolving the ultra-small-size active nano silicon dot solid powder in water to prepare ultra-small-size active nano silicon dot mother liquor for later use;
(3) Adding water into the ultra-small-size active nano silicon dot mother solution under the stirring condition, and diluting to the concentration of 0.1 wt%.
Further, the step (1) includes, in parts by mass:
(11) Dissolving 0.4 part of trisodium citrate in 8 parts of ultrapure water, introducing nitrogen for protection, then adding 2 parts of 3-aminopropyl trimethoxysilane, and stirring at room temperature to obtain a mixed solution; adding the mixed solution into a high-pressure reaction kettle, heating to 160 ℃, and reacting for 24 hours to obtain an ultra-small-size nano silicon dot solution;
(12) Adding 10 parts of glutaraldehyde aqueous solution with the concentration of 25wt% and 3 parts of p-phenylenediamine into 40 parts of ultrapure water, stirring at room temperature for 8 hours, adding the ultra-small-size nano silicon dot solution obtained in the step (11), and continuing stirring at room temperature for 8 hours to obtain a mixed solution;
(13) Adding 5 parts of sodium sulfanilate and 10 parts of glutaraldehyde into the mixed solution obtained in the step (12), continuously stirring at room temperature for 7 hours, and freeze-drying to obtain the ultra-small-size active nano silicon dot solid powder.
The application of the ultra-small-size active nano fluid in low-permeability reservoir oil displacement agents.
Still further, the reservoir temperature of the low permeability reservoir is 90 ℃.
The embodiments of the present invention have been described in detail. However, the present invention is not limited to the above-described embodiments, and various modifications may be made within the knowledge of those skilled in the art without departing from the spirit of the present invention.
Claims (8)
1. An ultra-small size active nanofluid characterized by being composed of:
the content of the ultra-small-size active nano silicon dots is 0.05 to 0.2 weight percent;
the balance being water.
2. The ultra-small size reactive nanofluid of claim 1, wherein said water comprisesK + 、Na + 、Mg 2+ 、Ca 2+ And Cl - Wherein K is + 、Na + The total concentration is 1000-30000 mg/L, ca 2+ And Mg (magnesium) 2+ The total concentration is 100-2000 mg/L, and the total mineralization degree is 2000-60000 mg/L.
3. The ultra-small size reactive nanofluid of claim 1, wherein the ultra-small size reactive nanofluid comprises 0.1wt% and 99.9wt% water.
4. The ultra-small size reactive nanofluid of claim 1, wherein the ultra-small size reactive nanofluid has a particle size of 3-5 nm.
5. The preparation method of the ultra-small-size active nano fluid is characterized by comprising the following steps of:
(1) Preparing ultra-small-size active nano silicon dot solid powder;
(2) Dissolving the ultra-small-size active nano silicon dot solid powder in water to prepare ultra-small-size active nano silicon dot mother liquor for later use;
(3) Adding water into the ultra-small-size active nano silicon dot mother solution under the stirring condition, and diluting to the concentration of 0.05-0.2 wt%.
6. The method of preparing an ultra-small-sized active nanofluid according to claim 5, wherein the step (1) comprises, in parts by mass:
(11) Dissolving 0.3-0.5 part of trisodium citrate in 7-9 parts of ultrapure water, introducing nitrogen for protection, then adding 1.5-2.5 parts of 3-aminopropyl trimethoxy silane, and stirring uniformly at room temperature to obtain a mixed solution; adding the mixed solution into a high-pressure reaction kettle, heating to 100-240 ℃, and reacting for 1.5-48 hours to obtain an ultra-small-size nano silicon dot solution;
(12) Adding 8-12 parts of glutaraldehyde aqueous solution with the concentration of 20-30 wt% and 2-4 parts of p-phenylenediamine into 35-45 parts of ultrapure water, stirring for 5-10 hours at room temperature, adding the ultra-small-size nano silicon dot solution obtained in the step (11), and continuing stirring for 5-10 hours at room temperature to obtain a mixed solution;
(13) Adding 4-6 parts of sodium sulfanilate and 8-12 parts of glutaraldehyde into the mixed solution obtained in the step (12), continuously stirring for 5-10 hours at room temperature, and freeze-drying to obtain the ultra-small-size active nano silicon dot solid powder.
7. Use of the ultra-small size active nanofluid of any one of claims 1-4 for low permeability reservoir oil displacement agents.
8. The use of claim 7, wherein the low permeability reservoir has a reservoir temperature of 60 to 120 ℃.
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| CN113136193A (en) * | 2021-04-23 | 2021-07-20 | 西南石油大学 | High-activity nano oil displacement agent and preparation method thereof |
| CN113201321A (en) * | 2021-03-30 | 2021-08-03 | 中国地质大学（北京） | Temperature-resistant salt-tolerant nano active fluid for oil seepage and drainage of tight oil reservoir |
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| CN106833586A (en) * | 2016-12-28 | 2017-06-13 | 浙江海洋大学 | One kind receives micron polymer particle and surfactant combination flooding method |
| CN110484229A (en) * | 2019-08-05 | 2019-11-22 | 中国石油天然气股份有限公司 | A kind of composite oil-displacing system and its methods for making and using same for low-permeability oil deposit |
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