CN111548465B - CO prevention device for tight oil reservoir2Gas channeling responsive interpenetrating network gel particles and preparation method thereof - Google Patents
CO prevention device for tight oil reservoir2Gas channeling responsive interpenetrating network gel particles and preparation method thereof Download PDFInfo
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Abstract
The invention discloses CO2Responsive interpenetrating network gel particles, the gel particles being prepared from the following materials in mass ratio: 15-25% of acrylamide monomer and 0-5% of temperature-resistant and salt-resistant monomer; 3 to 6 percent of CO2A responsive monomer; and a crosslinking agent, an initiator I, an initiator II and water. Preparing gel particles from acrylamide and a temperature-resistant and salt-resistant monomer, and mixing the prepared gel particles with CO2And (3) dissolving the response monomer and the gel particles in water and reacting for a period of time. In the present invention, the interpenetrating network structure increases the crosslinking density in the unit volume of the particles, thereby increasing the strength of the particles; CO of the invention2Responsive interpenetrating network gel particles with CO2After contact, the particles increase in size, indicating CO2Responsiveness to increase CO2Regulating strength during displacement while not reacting with CO2When contacted, the particles become smaller in size, and good reversibility is exhibited.
Description
Technical Field
The invention relates to the technical field of drilling and production, in particular to a method for preventing CO in a compact oil reservoir2CO of gas channeling2Responsive interpenetrating network gel particles and a preparation method thereof.
Background
The tight oil reservoir has the characteristics of low permeability, complex pore structure and high starting pressure, the main development mode is horizontal well volume fracturing, but after fracturing, failure type exploitation has the advantages of fast time zone pressure reduction, low unit pressure drop yield and high residual oil content in the reservoir, so the recovery ratio needs to be further improved. Conventional reservoir depletion development is usually followed by water injection to increase recovery, but tight reservoirs are more water sensitive and injection of water into the matrix is difficult. And CO2Flooding gradually becomes a research hotspot of tight oil reservoir development due to lower miscible phase pressure and higher recovery ratio after miscible phase. However, the reservoir after volume fracturing has a complex network structure, and injected media can generate channeling or ineffective circulation when the recovery ratio is further increased, so that the ultimate recovery ratio is low, and therefore, the fracture needs to be regulated and controlled.
The method aims to achieve effective regulation and control of the crack by taking the original purpose of not violating the fracturing as a core and expanding the swept volume of the injected medium as much as possible, namely achieving 'blocking but not death' of the crack. On one hand, the regulation system can selectively enter the crack to regulate and control the crack so as to start the matrix; on the other hand the cracks maintain the ability to seep, acting as oil/water flow channels. In the process of regulating and controlling the cracks, the final regulating and controlling effect is greatly influenced by the entering depth of the regulating and controlling system, and when the entering depth of the regulating and controlling system is insufficient, the injected medium quickly bypasses the position regulated and controlled by the regulating and controlling system in the near-wellbore area and returns to the cracks, so that the final regulating and controlling effect is poor. In the material meeting the requirements of 'blocking but not blocking' of cracks and deep regulation, the pre-crosslinked gel particles have certain application potential due to good water absorption expansibility and higher strength and toughness.
However, when the compact oil reservoir is regulated, the cracks are regulated and controlled by the conventional pre-crosslinked gel particles in the modes of bridging, trapping, accumulating and elastic plugging, the difference of the permeability between the regulated cracks and the matrix is still overlarge, and CO is generated2Matrix initiation upon displacement remains difficult.
Disclosure of Invention
Aiming at the defects of the current pre-crosslinked gel particles, the invention provides a method for preventing CO in a compact oil reservoir2CO of gas channeling2Responsive interpenetrating network gel particles having good strength and better CO2The response is suitable for deep displacement of the oil reservoir.
In order to achieve the purpose, the technical scheme of the invention is as follows:
CO (carbon monoxide)2Responsive interpenetrating network gel particles made from, by mass:
the balance of water.
The temperature-resistant salt-resistant monomer is one or a mixture of any two of N, N-dimethyl octadecyl allyl ammonium chloride, N-dimethyl hexadecyl allyl ammonium chloride, methyl acryloyl chloride modified alkylphenol polyoxyethylene ether or methyl acryloyl chloride modified alkyl alcohol polyoxyethylene ether.
The polymerization degree of the methacryloyl chloride modified alkylphenol polyoxyethylene ether or the methacryloyl chloride modified alkyl alcohol polyoxyethylene ether is 7-30.
The CO is2The responsive monomer is one or a mixture of two of dimethylaminoethyl methacrylate and dimethylaminopropyl methacrylamide.
The cross-linking agent is N, N-methylene bisacrylamide.
The initiator I is one of persulfate and azobisisobutylamidine hydrochloride, and the initiator II is 4,4' -azobis (4-cyanovaleric acid).
In the invention, the synthesis process of the methacrylic chloride modified alkyl alcohol polyoxyethylene ether and the methacrylic chloride modified alkylphenol polyoxyethylene ether is the same, and taking the methacrylic chloride modified alkyl alcohol polyoxyethylene ether as an example, the synthesis steps are as follows:
dissolving a certain amount of alkyl alcohol polyoxyethylene ether in dichloromethane, slowly adding methacryloyl chloride with the molar weight 1.2 times that of the alkyl alcohol polyoxyethylene ether into the alkyl alcohol polyoxyethylene ether at the temperature of-5-0 ℃ under the condition of stirring, and controlling the dropping time to be 1 h; then reacting for 24 hours at 25 ℃; and after the reaction is finished, removing unreacted methacryloyl chloride and dichloromethane by using rotary distillation to obtain the methacryloyl chloride modified alkyl alcohol polyoxyethylene ether.
The invention also discloses CO2The preparation method of the responsive interpenetrating network gel particles comprises the following steps:
(1) completely dissolving acrylamide, a temperature-resistant and salt-resistant monomer and a cross-linking agent into distilled water, wherein the addition amount of the cross-linking agent is 50% of the total amount of the cross-linking agent, and the content of the monomer in the system is controlled to be 20% -28%;
(2) slowly adding an initiator 1 into the system, introducing N for 230 minutes to remove oxygen in the system, raising the temperature to 45-60 ℃, and reacting for 2-4 hours;
(3) granulating, drying and crushing the product in the step (2) to obtain pre-crosslinked gel particles;
(4) introducing CO2Dissolving the responsive monomer, the initiator 2 and the rest of the cross-linking agent in water, controlling the mass of the added monomer to be 7-15% of the mass of the solution, adding the pre-crosslinked gel particles into the solution under the stirring condition, allowing the mixture to absorb water and expand for 24 hours, raising the temperature to 60-70 ℃, and reacting for 4 hours;
(5) granulating, drying and crushing the product obtained in the step (4) to obtain CO2Responsiveness ofInterpenetrating network gel particles.
The invention has the following beneficial effects:
1. the temperature-resistant and salt-resistant monomer is introduced to weaken the compression effect of metal ions in water on the polymer chain, so that the polymer chain keeps a larger size under high-temperature and high-salt conditions, and the temperature-resistant and salt-resistant performance of the invention is stronger.
2. CO of the invention2The responsive interpenetrating network gel particles have higher strength. The interpenetrating network structure increases the crosslink density per unit volume of the particle, thereby increasing the strength of the particle.
3. CO of the invention2Responsive interpenetrating network gel particles with CO2After contact, the particle size increases, indicating CO2Responsiveness to increase CO2The regulation and control strength of the cracks in the displacement process is stronger in the plugging effect of the cracks, so that CO is generated2The driving effect is better; while discharging CO2Then, the particle size becomes small, and good response reversibility is exhibited.
In conclusion, the invention has good strength and CO2And the response property can be applied to a tight oil reservoir, so that the recovery rate of the tight oil reservoir is improved.
Drawings
FIG. 1 shows CO2Responsive interpenetrating network gel particle CO2Responsiveness;
FIG. 2 shows CO2Introducing CO into responsive interpenetrating network gel particles2The strength of the front;
FIG. 3 is CO2Introducing CO into responsive interpenetrating network gel particles2The latter strength;
FIG. 4 is a graph of the magnitude of enhanced recovery of conventional gel particles;
FIG. 5 shows CO2The responsive interpenetrating network gel particles increase the recovery rate.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
(1) completely dissolving 48g of acrylamide, 6g of methacryloyl chloride modified alkylphenol polyoxyethylene ether and 0.2g N, N-methylene bisacrylamide into 150mL of distilled water by utilizing ultrasound;
(2) slowly adding 0.01g of ammonium persulfate into the system, introducing N230 minutes to remove oxygen in the system, raising the temperature to 50 ℃, and reacting for 4 hours to obtain the pre-crosslinked gel.
(3) Granulating the obtained gel, drying at 70 deg.C, and pulverizing to obtain pre-crosslinked gel particles (ASSAP).
(4) And (3) adding the pre-crosslinked gel particles obtained in the step (3) into 100ml of deionized water solution in which 10g of dimethylaminoethyl methacrylate, 0.03g of 4,4' -azobis (4-cyanovaleric acid) and 0.2g N, N-methylenebisacrylamide are dissolved under the stirring condition, allowing the mixture to absorb water and expand for 24 hours, raising the temperature to 70 ℃ again, and reacting for 4 hours to obtain the hydrogel.
(5) Granulating the obtained gel, drying at 70 ℃, and crushing to finally obtain CO2Responsive interpenetrating network gel particles, code IPN-ASSAP.
The synthesis method of the methacryloyl chloride modified alkylphenol polyoxyethylene ether comprises the following steps:
dissolving 0.05mol of octyl phenol polyoxyethylene ether-10 in 200ml of dichloromethane, adjusting the temperature to-5-0 ℃ in an ice bath, starting stirring, then taking 0.06mol of methacrylic chloride, dropwise adding the methacrylic chloride into the solution of the octyl phenol polyoxyethylene ether-10 for 1h, reacting for 24h at 25 ℃ after dropwise adding, taking the product, and then carrying out rotary distillation to remove unreacted octyl phenol polyoxyethylene ether-10 and methacrylic chloride, thus obtaining the methacrylic chloride modified alkylphenol polyoxyethylene ether.
Example 2:
production of CO2Method for preparing responsive interpenetrating network gel particlesThe procedure is as in example 1, with the only modification that in step (2), 0.1g of ammonium persulfate was changed to 0.08g of azobisisobutylamidine hydrochloride.
Example 3:
production of CO2The procedure for the responsive interpenetrating network gel particles was the same as in example 1, except that in step (4), dimethylaminoethyl methacrylate was replaced with dimethylaminopropyl methacrylamide.
(II) performance test:
1、CO2response Performance testing
In order to test the CO of the present invention2Responsive interpenetrating network gel particles to CO2Taking CO in example 1 as the responsiveness of2Responsive interpenetrating network gel particles, introducing CO by measuring gel particles with a laser particle size analyzer2The size distribution before and after the measurement is carried out, and the specific test result is shown in figure 1.
As can be seen from FIG. 1, CO was introduced2The size distribution of the gel particles is 0.6-55 mu m, and the median particle diameter is 18.24 mu m; CO was introduced at a rate of 10ml/min2After 30min, the size distribution of the gel particles became 2.1 μm to 77 μm, and the median particle diameter became 25.86 μm. In order to verify the response reversibility of the gel particles, N was then introduced into the system again for 230min at the same rate, and the size distribution of the particles became 1 μm to 63 μm, and the median diameter became 19.2. mu.m. The experimental results show that CO2Responsive interpenetrating network gel particles with CO2Particle size increases significantly after contact, CO2The responsiveness is obvious, and CO is discharged2After then, CO2The size of the responsive interpenetrating network gel particles is smaller than the initial size, and good response reversibility is shown.
2. Gel Strength test
Taking the CO in example 12Responsive interpenetrating network gel particles, by measuring the introduced CO with a TGU experimental device of a pressure-diversion method2The strength change before and after the test, further study of CO2For CO of the present invention2The final measurement results are shown in fig. 2, based on the influence of the responsive interpenetrating network gel particles.
As can be seen from FIGS. 2 and 3, CO was introduced2The gel particles had a strength of 106.1kPa, and were charged with CO2After that, CO in the gel particles2The responsive group undergoes protonation reaction, the hydrophilicity of the particle is enhanced, more water molecules enter the interior of the gel particle, the size of the particle becomes larger, the pressure required for passing through the screen is increased, and accordingly the strength of the particle is increased to 127.2 kPa.
3. Tight reservoir flooding test
To verify the CO of the present invention2Responsive interpenetrating network gel particles in compact reservoir CO2Effect in flooding, flooding experiments were performed, with the purpose of illustrating the CO of the present invention2The superiority of responsive interpenetrating network gel particles over conventional gel particles in low permeability reservoir displacement was compared using the pre-crosslinked gel particles ASSAP comparative experiment in example 1. The core parameters used for the experiment were: length 8cm, diameter 3.8cm, crack width 0.2mm, matrix permeability 0.5mD, and water flooding-CO2flooding-gel-injection-CO2The final measurement results of the driving steps are shown in fig. 4 and 5.
As can be seen from fig. 5, the recovery rate in the water flooding phase is 8.9%, and mainly the crude oil in the fractures is displaced and then water channeling occurs; CO injection2During displacement, residual oil in the cracks and part of crude oil in the matrix near the edges of the cracks are extracted, and gas channeling occurs after the recovery rate is improved by 8.2%. CO injection2After the responsive interpenetrating network gel particles are adopted, the injection pressure is obviously increased, which indicates that the cracks are effectively regulated and controlled. Reinjection of CO2At this time, the injection pressure is first increased to account for the particles and CO2After contact, the size is increased, and the plugging strength of the crack is increased. The recovery ratio is improved by 23.1 percent after the crack is regulated and controlled. While FIG. 4 shows the pressure increase after injecting the gel particles and re-injecting CO2When the pressure is slightly increased and then rapidly reduced, the recovery ratio is improved by 8.9 percent after the gel particles are injected. The experimental results show that CO is relatively high compared with the conventional gel particles2The responsive interpenetrating network gel particles can effectively block cracks and improve the recovery ratio.
Although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (4)
1. CO (carbon monoxide)2Responsive interpenetrating network gel particles, characterized in that said gel particles are prepared from the following, in mass ratio:
15 to 25 percent of acrylamide monomer;
1-5% of a temperature-resistant salt-resistant monomer;
CO23% -6% of responsive monomer;
0.3 to 0.8 percent of cross-linking agent based on the total amount of the monomers;
initiating agent one: 0.01 to 0.05 percent of the total amount of the monomers;
and (2) initiator II: 0.01 to 0.05 percent of the total amount of the monomers;
the balance of water;
the preparation method comprises the following steps:
(1) completely dissolving acrylamide, a temperature-resistant and salt-resistant monomer and a cross-linking agent into distilled water, wherein the addition amount of the cross-linking agent is 50% of the total amount of the cross-linking agent, and the content of the monomer in the system is controlled to be 20% -28%;
(2) adding initiator into the system slowly, and introducing N2Removing oxygen in the system within 30 minutes, raising the temperature to 45-60 ℃, and reacting for 2-4 hours;
(3) granulating, drying and crushing the product in the step (2) to obtain pre-crosslinked gel particles;
(4) introducing CO2The responsive monomer, the initiator II and the rest of the cross-linking agent are dissolved inIn water, controlling the mass of the added monomer to be 7-15% of the mass of the solution, adding pre-crosslinked gel particles into the solution under the stirring condition, allowing the mixture to absorb water and expand for 24 hours, raising the temperature to 60-70 ℃, and reacting for 4 hours;
(5) granulating, drying and crushing the product obtained in the step (4) to obtain CO2Responsive interpenetrating network gel particles;
the temperature-resistant salt-resistant monomer is one or a mixture of any two of N, N-dimethyl octadecyl allyl ammonium chloride, N-dimethyl hexadecyl allyl ammonium chloride, methyl acryloyl chloride modified alkylphenol polyoxyethylene ether or methyl acryloyl chloride modified alkyl alcohol polyoxyethylene ether;
the CO is2The responsive monomer is one or a mixture of two of dimethylaminoethyl methacrylate and dimethylaminopropyl methacrylamide.
2. The gel particles according to claim 1, wherein the polymerization degree of the methacryloyl chloride-modified alkylphenol polyoxyethylene ether or the methacryloyl chloride-modified alkylol polyoxyethylene ether is 7 to 30.
3. The gel particles of claim 1, wherein the cross-linking agent is N, N-methylene bis acrylamide.
4. The gelled particles of claim 1, wherein the first initiator is one of a persulfate and azobisisobutylamidine hydrochloride and the second initiator is 4,4' -azobis (4-cyanovaleric acid).
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| CN113831482B (en) * | 2021-10-20 | 2023-03-14 | 四川大学 | CO based on tertiary amine group 2 Responsive tackifying polymer and preparation method and application thereof |
| CN116023917B (en) * | 2021-10-26 | 2024-03-26 | 中国石油化工股份有限公司 | CO (carbon monoxide) 2 Responsive gel system, preparation method thereof and oil reservoir CO prevention 2 Leakage method |
| CN113969157B (en) * | 2021-11-05 | 2022-05-24 | 西南石油大学 | Compact reservoir CO2Flooding multi-scale channeling control system and preparation method thereof |
| CN115850569A (en) * | 2022-12-08 | 2023-03-28 | 西南石油大学 | For micro-crack of cement stoneRepaired CO 2 Preparation method of responsive gel material |
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