CN114621739A - Temperature-resistant salt-resistant super-hydrophobic particle plugging agent and preparation method thereof - Google Patents
Temperature-resistant salt-resistant super-hydrophobic particle plugging agent and preparation method thereof Download PDFInfo
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- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/42—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
- C09K8/46—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement
- C09K8/467—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement containing additives for specific purposes
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Abstract
The invention provides a temperature-resistant salt-resistant super-hydrophobic particle plugging agent and a preparation method thereof, relating to the technical field of oilfield plugging agents, and the method comprises the following steps: (1) adding tetraethoxysilane into an alcohol solution, adding an acid solution, adjusting the pH, and stirring and refluxing at constant temperature; (2) adding a mixed solution of an alkali solution and alcohol into the solution obtained in the step (1), heating and stirring for reaction; (3) adding normal hexane into the solution obtained in the step (2), stirring, standing and centrifuging to obtain a solid substance; (4) and (4) adding the solid substance obtained in the step (3) into the silane coupling agent after hydrolysis, heating and stirring for reaction to obtain the particle plugging agent. The particle plugging agent comprises nano silicon dioxide particles and a hydrophobic material grafted on the nano silicon dioxide particles, and can realize a good plugging effect.
Description
Technical Field
The invention relates to the technical field of oilfield plugging agents, in particular to a temperature-resistant salt-resistant super-hydrophobic particle plugging agent and a preparation method thereof.
Background
Due to poor formation homogeneity of the tower river clastic rock reservoir, the water plugging of the horizontal well has low success rate and poor oil increasing effect, the reservoir layer of the reservoir has strong heterogeneity, the water outlet mechanism of the horizontal well is relatively complex, and the general oil recovery rate is very low. The horizontal well is the type of an oil well mainly developed by a tower river clastic rock oil reservoir at present, but the high water content of the oil well seriously influences the development effect of the clastic rock horizontal well and is the main contradiction of efficient development of the tower river clastic rock horizontal well. The water shutoff and profile control process is a main means for controlling water of a high-water-content horizontal well of a clastic rock oil reservoir of a tower river, and the water shutoff effect of the clastic rock horizontal well is considerable from development of an oil field to the end of 2013. However, as the exploitation time increases, the potential of the oil well becomes smaller, the effect of the existing water plugging technology becomes worse, the oil increase of a single water plugging well gradually decreases, and the water plugging effective rate is in a descending trend along with the water plugging turns. The existing single water plugging profile control of the horizontal well cannot meet the profile control requirement of the clastic rock oil reservoir horizontal well in the tower river oil field.
Patent CN110387222A reports a porous gel plugging agent, a preparation method and application thereof, relating to the technical field of gel plugging. The porous gel plugging agent is obtained by the polymerization reaction of raw materials comprising a monomer, a cross-linking agent, an initiator, an inorganic reinforcing material, a gas generating agent and water, and the gel plugging agent is in a porous structure. The raw materials of the preparation method of the porous gel plugging agent adopt the raw materials, have the advantages of rapid gelling and high colloid strength at a medium-low temperature oil reservoir (75-110 ℃), have good permeability, are a temporary plugging system easy to break and degrade, and are suitable for application in oil and gas well completion, well workover, leak protection and plugging, and temporary plugging fracturing and acidizing. The document (the application of the nano material in water shutoff profile control of oil fields is advanced, the oil field chemistry [ J ], Pengbaoliang and the like, 2016,33 (3): 552-556) reports that the nano material can improve the performance of the water shutoff profile control agent, plays more and more important roles in the water shutoff profile control of oil fields, introduces the structure and performance characteristics of the nano material, outlines the research and application progress of the nano material in the aspect of water shutoff profile control of oil fields, discusses the performance of the nano material in the aspects of regulating and controlling gel gelling time, improving the stability and mechanical property of the water shutoff profile control agent and improving the stability of emulsion and foam, and shows the application prospect of the nano composite material in the aspects of water shutoff profile control of high-temperature oil reservoirs, ultrahigh-permeability oil reservoir channels and low-permeability oil reservoirs.
The heterogeneity of the clastic rock oil reservoir horizontal well causes low-water-level drilling or channeling, the high water content of the oil well is serious, and the early-stage ultrafine calcium carbonate water plugging has 3 problems, namely poor controllability and larger particle size, and shallow depth (less than 50cm) of the entering stratum; secondly, the plugging strength is low (less than 60 percent); and thirdly, the oil-water selectivity is not achieved. The existing single water plugging profile control of the horizontal well cannot meet the profile control requirement of the clastic rock oil reservoir horizontal well in the tower river oil field. In order to solve the problems faced at present, a temperature-resistant and salt-resistant super-hydrophobic particle plugging agent needs to be found urgently, so that a good plugging effect is realized.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a porous nano silica particle as a temperature-resistant salt-resistant super-hydrophobic particle plugging agent, which can separate crude oil, paraffin, water and gas from the surface of rock by combining the unique quantum size effect and surface effect of the nano particles and the auxiliary effects of reducing capillary pressure, reversing wettability and changing phase permeation hysteresis effect and the like generated by a system, thereby realizing good plugging effect.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the invention provides a preparation method of a particle plugging agent, which comprises the following steps:
(1) adding tetraethoxysilane into an alcohol solution, adding an acid solution, adjusting the pH, and stirring and refluxing at constant temperature;
(2) adding an alcohol solution into the solution obtained in the step (1), adding an alkali solution to adjust the pH, heating and stirring for reaction;
(3) adding normal hexane into the solution obtained in the step (2), stirring, standing and centrifuging to obtain a solid substance;
(4) and (4) adding the solid substance obtained in the step (3) into a silane coupling agent after hydrolysis, heating and stirring for reaction to obtain the silane coupling agent.
Further, in the step (1), the pH value is 2.5-3, the constant temperature is not higher than 20 ℃, and the stirring reflux time is 24-72 h. Preferably, the constant temperature is 5-10 ℃, and the stirring reflux time is not less than 2 d.
Further, the heating temperature in the step (2) is 40-50 ℃, the pH value is 8-10, and the stirring reaction time is 12-48 h.
Further, the stirring time in the step (3) is 5-7h, the stirring speed is 10-20r/min, and the standing time is at least 12 h.
Further, the heating temperature in the step (4) is 190 ℃ and 210 ℃, and the stirring reaction time is 3-10 h.
Further, the amount of the silane coupling agent used in step (4) is based on immersion of the solid substance, and preferably, the mass ratio of the solid substance to the silane coupling agent after completion of hydrolysis is 1:5 to 10.
Further, the alcohol in the step (1) and the step (2) is methanol or ethanol; the acid in the step (1) comprises hydrofluoric acid, acetic acid or formic acid; the alkali in the step (2) comprises ammonia water, sodium hydroxide or potassium hydroxide.
Furthermore, the mass fraction of the acid solution is 5-10%, so that the acid solution has a certain buffering effect on the system, and the increase of the particle size of the nano silicon dioxide particles caused by the rapid increase of the pH value of the system in the reaction process is avoided.
Further, the mass fraction of the ammonia water is 15-30%, and the concentration of the sodium hydroxide or the potassium hydroxide is 0.1 mol/L.
Further, the mass ratio of the alcohol solution added in the step (1) to the alcohol solution added in the step (2) is 1: 1.5-2.
Further, the molar ratio of the ethyl orthosilicate to the alcohol solution to the acid solution in the step (1) is as follows: 1:1.2:0.05.
Further, the molar ratio of the n-hexane to the ethanol solution in the step (3) is 1: 2.
Further, in the step (4), the silane coupling agent is one or more of methyltrimethoxysilane, gamma- (2, 3-glycidoxy) propyl trimethoxysilane, glycidoxypropyltrimethylsilane, vinyltrimethoxysilane, oxypropyltrimethylsilane methacrylate and amino-primary aminopropyltrimethoxysilane. Preferably, the silane coupling agent is methyl trimethoxy silane and gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane, and the mass ratio of the methyl trimethoxy silane to the gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane is 1:1.
Further, the step (2) also comprises adding a suspension of nano magnetic particles or ferrous hydroxide; adding the suspension of the nano magnetic particles or the ferrous hydroxide after the pH is adjusted; the particle size of the nano magnetic particles is not more than 30 nm; the molar ratio of the nano magnetic particles to the tetraethoxysilane is 0.01-0.05: 1; the suspension of the ferrous hydroxide is prepared by the following method, ferrous sulfate is dissolved in ammonia water and is generated by stirring reaction; the molar ratio of the sulfated ferrous iron to the ethyl orthosilicate is 0.03: 1.
Further, the step (4) may further comprise adding formamide, acetamide, dimethylformamide or glycerol before the heating and stirring.
The invention also provides the particle plugging agent prepared by the preparation method. The particle plugging agent comprises nano silicon dioxide particles and a hydrophobic material grafted on the nano silicon dioxide particles.
The technical effects obtained by the invention are as follows:
the invention discloses a temperature-resistant salt-resistant super-hydrophobic particle plugging agent and a preparation method thereof, wherein tetraethoxysilane is used as a raw material, nano-silica nano-particles are obtained through gelation, aging and solvent replacement, a silane coupling agent with hydrophobic property is grafted on the surfaces of the nano-silica nano-particles, and the nano-particles with a porous structure are formed through the coupling property of the silane coupling agent.
Detailed Description
It should be noted that the raw materials used in the present invention are all common commercial products, and thus the sources thereof are not particularly limited.
Example 1
The invention discloses a temperature-resistant salt-resistant super-hydrophobic particle plugging agent which is prepared by the following method:
(1) measuring ethanol, and adding water to prepare an ethanol solution with the mass fraction of 20% for later use; diluting hydrofluoric acid with water to 0.05mol/L diluted acid solution for later use; weighing ethyl orthosilicate according to the molar ratio of 1:1.2 of the ethyl orthosilicate to ethanol, adding the ethyl orthosilicate into an ethanol solution, dropwise adding an acetic acid solution with the mass fraction of 10%, and adjusting the pH value to 2.5; stirring and refluxing for 2d at the temperature of 10 ℃;
(2) adding an ethanol solution with the mass fraction of 20% into the system, slowly dropwise adding ammonia water under the stirring condition to adjust the pH value of the system to 8-10, heating and stirring to 50 ℃, and continuously stirring and reacting for 16 hours under the constant temperature condition;
(3) adding n-hexane according to the molar ratio of 1:2 of the n-hexane to the ethanol (the total amount of ethanol used in the step (1) and the step (2)), stirring at low speed for 5h under the condition of 10-20r/min, standing for 24h, and centrifuging to obtain a solid;
(4) and adding the obtained solid into the silane coupling agent after the hydrolysis is finished, and stirring and reacting for 8 hours at the temperature of 200 ℃ to obtain a product, wherein the solid is immersed.
Example 2
The invention discloses a temperature-resistant salt-resistant super-hydrophobic particle plugging agent which is prepared by the following method:
(2) adding an ethanol solution with the mass fraction of 20% into the system, slowly dropwise adding ammonia water under the stirring condition to adjust the pH value of the system to 8-10, adding an ethanol dispersion liquid of nano silver particles after the ammonia water is dropwise added, heating and stirring to 50 ℃, and continuously stirring and reacting for 16 hours under the constant temperature condition; the remaining preparation steps were the same as in example 1, except that the molar ratio of the added amount of the nano-silver particles to the tetraethoxysilane was 0.01: 1.
Example 3
The invention discloses a temperature-resistant salt-resistant super-hydrophobic particle plugging agent which is prepared by the following method:
(2) adding an ethanol solution with the mass fraction of 20% into the system, slowly dropwise adding ammonia water under the stirring condition to adjust the pH value of the system to 8-10, adding a suspension of ferrous hydroxide after the dropwise adding of the ammonia water is finished, heating and stirring to 50 ℃, and continuously stirring and reacting for 16 hours under the constant temperature condition. The remaining preparation steps were the same as in example 1.
The suspension of the ferrous hydroxide is prepared by dissolving ferrous sulfate in ammonia water and stirring for reaction; the molar ratio of ferrous hydroxide to ethyl orthosilicate is 0.03: 1.
Example 4
The only difference from example 1 is that dimethylformamide was added before the heating and stirring, and the amount of dimethylformamide added was 5% by mass of the solid matter.
Comparative example 1
The only difference from example 1 is that the acid addition step of step (1) is omitted.
Comparative example 2
The only difference from example 1 is that the addition of alkali in step (2) is omitted.
Comparative example 3
The only difference from example 1 is that in step (1) acid is added but the reaction temperature is above 40 ℃.
The properties and parameters of the particulate plugging agent of examples 1-4 and comparative example are shown in Table 1.
Wherein, the average particle diameter, the specific surface area and the water contact angle of the particle plugging agent are detected by a conventional method.
The water plugging performance at 120 ℃ is detected by adopting the following method: the blocking agent adopts formation water and an emulsifying system (3.5% oleic acid imidazoline) to prepare a blocking system with the mass fraction of 5%, and then water blocking performance evaluation is carried out through a simulation experiment, wherein the injection amount is 0.1PV, the constant-temperature aging temperature is 120 ℃, and the constant-temperature aging time is 12 h.
200000 degree of mineralization water shutoff performance adopts the following method: the blocking agent adopts formation water and an emulsification system (3.5% oleic acid imidazoline) to prepare a blocking system with the mass fraction of 5%, and then water blocking performance evaluation is carried out through a simulation experiment, wherein the injection amount is 0.1PV, and the mineralization degree of water used for water flooding is 200000 mg/L.
TABLE 1
As shown in Table 1, the average particle size of the particulate plugging agent obtained in the present invention is small, within the range of 6.9-8.2nm, the specific surface area is large, and can reach 466-2The water plugging performance at 120 ℃ is as high as 80.9-85.2%, the water plugging performance at 200000 mineralization degree is as high as 82.9-85.9%, and the water contact angle is 126.9-127.7 degrees, so that the particle plugging agent has a good plugging effect. When acid or alkali is not added or the reaction temperature is changed in the preparation process, the blocking effect of the particle blocking agent is obviously reduced.
Finally, it should be noted that the above-mentioned contents are only used for illustrating the technical solutions of the present invention, and not for limiting the protection scope of the present invention, and that the simple modifications or equivalent substitutions of the technical solutions of the present invention by those of ordinary skill in the art can be made without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. A preparation method of the particle plugging agent is characterized by comprising the following steps: the method comprises the following steps:
(1) adding tetraethoxysilane into an alcohol solution, adding an acid solution, adjusting the pH, and stirring and refluxing at constant temperature;
(2) adding an alcohol solution into the solution obtained in the step (1), adding an alkali solution to adjust the pH, heating and stirring for reaction;
(3) adding normal hexane into the solution obtained in the step (2), stirring, standing and centrifuging to obtain a solid substance;
(4) and (4) adding the solid substance obtained in the step (3) into a silane coupling agent after hydrolysis, heating and stirring for reaction to obtain the silane coupling agent.
2. The method of claim 1, wherein: and (2) in the step (1), the pH value is 2.5-3, the constant temperature is not higher than 20 ℃, and the stirring reflux time is 24-72 h.
3. The production method according to claim 1, characterized in that: in the step (2), the heating temperature is 40-50 ℃, the pH value is 8-10, and the stirring reaction time is 12-48 h.
4. The method of claim 1, wherein: and (3) stirring for 5-7h, and standing for at least 12 h.
5. The method of claim 1, wherein: the heating temperature in the step (4) is 190 ℃ and 210 ℃, and the stirring reaction time is 3-10 h.
6. The method of claim 1, wherein: the alcohol in the step (1) and the step (2) is methanol or ethanol; the acid in the step (1) comprises hydrofluoric acid, acetic acid or formic acid; the alkali in the step (2) comprises ammonia water, sodium hydroxide or potassium hydroxide.
7. The method of claim 1, wherein: in the step (4), the silane coupling agent is one or more of methyltrimethoxysilane, gamma- (2, 3-glycidoxy) propyl trimethoxysilane, glycidoxypropyltrimethylsilane, vinyl trimethoxysilane, oxypropyltrimethylsilane methacrylate and primary amino propyl trimethoxysilane.
8. The method of claim 1, wherein: the step (2) also comprises adding suspension of nano magnetic particles or ferrous hydroxide.
9. The method of claim 1, wherein: the step (4) also comprises the addition of formamide acetamide, dimethylformamide or glycerol.
10. A particulate plugging agent prepared by the method of preparation according to any one of claims 1 to 9.
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Cited By (2)
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| CN116218488A (en) * | 2022-12-27 | 2023-06-06 | 中国石油天然气集团有限公司 | Low-hydrophilicity nano silicon dioxide plugging agent for drilling fluid and green preparation method thereof |
| CN118206973A (en) * | 2024-05-22 | 2024-06-18 | 成都理工大学 | In-situ self-generated super-hydrophobic interface layer drag reducer and preparation method thereof |
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| CN118206973A (en) * | 2024-05-22 | 2024-06-18 | 成都理工大学 | In-situ self-generated super-hydrophobic interface layer drag reducer and preparation method thereof |
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