CN120718616A - A resistance-increasing in-situ gel deep profile control agent and its preparation method - Google Patents
A resistance-increasing in-situ gel deep profile control agent and its preparation methodInfo
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- CN120718616A CN120718616A CN202510793908.0A CN202510793908A CN120718616A CN 120718616 A CN120718616 A CN 120718616A CN 202510793908 A CN202510793908 A CN 202510793908A CN 120718616 A CN120718616 A CN 120718616A
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Abstract
The invention belongs to the technical field of oil and gas field development and recovery ratio improvement, and particularly relates to a resistance-increasing in-situ gel deep profile control agent and a preparation method thereof. The invention relates to a resistance-increasing in-situ gel deep profile control agent which is prepared from the following raw materials, by weight, 3-8% of a water-soluble functional monomer, 0.5-2% of functional micro-nano particles, 0.3-1% of a gel forming control agent and the balance of water. The profile control agent reacts in the stratum to form the three-dimensional network structure gel taking the functional micro-nano particles as the cross-linking nodes, so that the temperature resistance is greatly improved, the dehydration rate is lower than 10% after the temperature is kept at 120 ℃ for 90 days, and the profile control agent can be used for deep profile control of a high-temperature oil reservoir at 120 ℃.
Description
Technical Field
The invention belongs to the technical field of oil and gas field development and recovery ratio improvement, and particularly relates to a resistance-increasing in-situ gel deep profile control agent and a preparation method thereof.
Background
The weak gel profile control technology is a deep profile control technology of an oil reservoir based on polymer body gel and polymer flooding development. The weak gel system is the core of the weak gel profile control technology. The weak gel system is usually composed of low concentration (800-3000 mg/L) polymer and cross-linking agent, and the gel forming mechanism is that under certain conditions, the polymer molecules and the cross-linking agent molecules are subjected to physical and chemical actions (such as coordination, condensation, electrostatic attraction, hydrophobic association and the like) to finally form the amorphous free-flowing semi-fluid with a three-dimensional network structure mainly comprising intermolecular cross-linking and intramolecular cross-linking as auxiliary. Compared with polymer bulk gel, the weak gel system has better fluidity, so that the weak gel system moves relatively far in an oil reservoir, and compared with polymer solution, the weak gel system has higher viscosity under the same polymer concentration, so that the weak gel system can play a certain role in plugging the high-permeability channeling area of the oil reservoir. Based on the advantages, the weak gel profile control technology is one of the main technologies for stabilizing and controlling the oil and water in the later period of each water injection development oil field at home and abroad.
Along with the continuous expansion of the application of mines, the defect of profile control of a weak gel system is also highlighted, and the main appearance is that (1) the requirement on liquid preparation water is high, and in high mineralization water (mineralization degree is more than or equal to 10 multiplied by 10 4 mg/L), polymer components in the weak gel system are difficult to fully dissolve, so that the subsequent gel formation of the system is difficult, even not to form gel. (2) The initial viscosity of the system is high, so that the pressure of the system is high in the injection process, and even the phenomenon of injection failure occurs in medium-low permeability reservoirs. (3) In the injection process, the polymer in the system is severely sheared and degraded, so that the gel forming strength of the system is obviously weakened after the system enters the stratum, and the blocking capability of the gel forming to a cross flow area is sharply reduced. (4) The plugging capability in a high-pore high-permeability oil reservoir with the porosity of more than 20 percent and the permeability of more than 1000mD is poor, so that the subsequent water injection is easy to break through, and the effective period is short.
Disclosure of Invention
In order to overcome the defects of the conventional weak gel system profile control, the invention provides a resistance-increasing in-situ gel deep profile control agent and a preparation method thereof.
Specifically, the invention is realized by the following technical scheme:
The drag-increasing in-situ gel deep profile control agent is prepared from the following raw materials, by weight, 3-8% of water-soluble functional monomers, 0.5-2% of functional micro-nano particles, 0.3-1% of gel forming control agents and the balance of water.
The drag-increasing in-situ gel deep profile control agent is prepared from the following raw materials, by weight, 5-8% of water-soluble functional monomers, 0.8-2% of functional micro-nano particles, 0.4-0.8% of gel forming control agents and the balance of water.
The resistance-increasing in-situ gel deep profile control agent comprises one or more of polyethylene glycol (1000) monomethyl ether methacrylate, polyethylene glycol (2000) monomethyl ether methacrylate, polyethylene glycol (4000) monomethyl ether methacrylate, polyethylene glycol (6000) monomethyl ether methacrylate, polyethylene glycol (8000) monomethyl ether methacrylate and acrylamide.
The drag-increasing in-situ gel deep profile control agent comprises one or two of crosslinked polystyrene micro-nano particles with carbon-carbon double bonds on the surfaces and silica gel micro-nano particles with carbon-carbon double bonds on the surfaces.
According to the drag-increasing in-situ gel deep profile control agent, the particle size distribution of the functional micro-nano particles is 50 nm-10 mu m.
The gel forming control agent comprises one or more of azodiiso Ding Mi hydrochloride, azodiisopropylimidazoline, tert-butyl peroxybenzoate, tert-amyl hydroperoxide and tert-butyl cumyl peroxide.
The resistance-increasing in-situ gel deep profile control agent is characterized in that the water is stratum water or seawater.
The maximum mineralization degree of the water of the drag-increasing in-situ gel deep profile control agent is 30 multiplied by 10 4 mg/L.
A preparation method of a resistance-increasing in-situ gel deep profile control agent comprises the following steps:
(1) Adding water-soluble functional monomers into water according to a proportion, and stirring to completely dissolve the water-soluble functional monomers;
(2) Adding functional micro-nano particles according to the proportion under stirring, and continuing stirring to completely dissolve the functional micro-nano particles;
(3) Adding the gel forming control agent according to the proportion, and stirring to obtain the resistance-increasing in-situ gel deep profile control agent.
According to the preparation method of the resistance-increasing in-situ gel deep profile control agent, the stirring speed in the steps (1) - (3) is more than or equal to 20rpm.
A resistance-increasing in-situ gel deep profile control agent is prepared by the preparation method.
According to the resistance-increasing type in-situ gel deep profile control agent, the initial viscosity of the resistance-increasing type in-situ gel deep profile control agent is 1-2 mPas, the gel forming time in an oil reservoir at 50-120 ℃ is adjustable and controllable for 5-15 days, and the dehydration rate is lower than 10% after gel forming at the constant temperature of 120 ℃ for 90 days.
Compared with the prior art, the technical scheme of the invention has the following beneficial effects:
(1) The resistance-increasing in-situ gel deep profile control agent provided by the invention has good salt tolerance, and can be well dissolved and dispersed even in high-mineralization water with mineralization degree of 30 multiplied by 10 4 mg/L. Therefore, the resistance-increasing in-situ gel deep profile control agent provided by the invention can be prepared by using high-mineralization stratum water or seawater, so that the liquid preparation cost can be greatly reduced;
(2) Compared with the polymer in a weak gel system, the functional monomer has small molecular weight, so the resistance-increasing in-situ gel deep profile control agent provided by the invention has the advantages of low initial viscosity and easiness in injection;
(3) The functional monomer has small molecular weight and the functional micro-nano particles have rigid structures, so that the resistance-increasing in-situ gel deep profile control agent provided by the invention is not influenced by the shearing degradation in the injection process;
(4) The profile control agent is injected into the stratum and reacts in the stratum to form the gel with the three-dimensional network structure taking the functional micro-nano particles as the cross-linking nodes, so compared with the existing weak gel profile control system, the resistance-increasing in-situ gel deep profile control agent provided by the invention has the characteristics of higher blocking strength for a hypertonic channeling area, difficult breakthrough of subsequent injected water and long blocking durability;
(5) The time for generating gel by reaction of the profile control agent in the stratum with the temperature of 50-120 ℃ can be flexibly adjusted within the range of 5-15 days by adjusting the addition amount and combination of the gel forming control agent, so that the deep profile control construction operation with large liquid amount and long well distance can be realized;
(6) The profile control agent reacts in the stratum to form the three-dimensional network structure gel taking the functional micro-nano particles as the cross-linking nodes, so that the temperature resistance is greatly improved, the dehydration rate is lower than 10% after the temperature is kept at 120 ℃ for 90 days, and the profile control agent can be used for deep profile control of a high-temperature oil reservoir at 120 ℃.
Drawings
Various other advantages and benefits will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The drawings are only for purposes of illustrating the preferred embodiments and are not to be construed as limiting the invention.
FIG. 1 is a photograph showing the state of the in-situ gel deep profile control agent prepared in example 1 of the present invention before and after gel formation;
FIG. 2 is a scanning electron microscope photograph of the in-situ gel deep profile control agent of the drag-increasing type prepared in example 1 of the present invention after gel formation;
FIG. 3 is a photograph showing the state of the in-situ gel deep profile control agent prepared in example 2 of the present invention before and after gel formation;
FIG. 4 is a scanning electron microscope photograph of the in-situ gel deep profile control agent with increased resistance prepared in example 2 of the present invention after gelling;
FIG. 5 is a photograph showing the state of the in-situ gel deep profile control agent prepared in example 3 of the present invention before and after gel formation;
FIG. 6 is a scanning electron microscope photograph of the in-situ gel deep profile control agent of the drag-increasing type prepared in example 3 of the present invention after gelling;
FIG. 7 is a photograph showing the state before and after the gel formation of the gel deep profile control agent in situ, which is prepared in example 4 of the present invention;
FIG. 8 is a scanning electron microscope photograph of the in-situ gel deep profile control agent of the drag-increasing type prepared in example 4 of the present invention.
Detailed Description
The present invention will be described in detail with reference to the following embodiments for a full understanding of the objects, features, and effects of the present invention. The process of the present invention is carried out by methods or apparatus conventional in the art, except as described below. The following terms have the meanings commonly understood by those skilled in the art unless otherwise indicated.
When a range of values is disclosed herein, the range is considered to be continuous and includes both the minimum and maximum values for the range, as well as each value between such minimum and maximum values. Further, when a range refers to an integer, each integer between the minimum and maximum values of the range is included. Further, when multiple range description features or characteristics are provided, the ranges may be combined. In other words, unless otherwise indicated, all ranges disclosed herein are to be understood to include any and all subranges subsumed therein.
In particular, in a first aspect, the invention provides a drag-increasing in-situ gel deep profile control agent which is prepared from raw materials including a water-soluble functional monomer, functional micro-nano particles, a gel forming control agent and water.
At a certain temperature, the gel forming control agent is decomposed in water to generate free radicals, so that the water-soluble functional monomer and the functional micro-nano particles are initiated to generate free radical polymerization reaction, and finally, the three-dimensional network structure gel taking the micro-nano particles as cross-linking nodes is formed, and the blocking of the cross-flow channel is realized.
The components of the drag-increasing in-situ gel deep profile control agent of the invention are described in detail below:
Water-soluble functional monomer
The water-soluble functional monomer has the function of providing a hydrophilic chain segment for the three-dimensional network structure of the gel after polymerization.
In some preferred embodiments, the water-soluble functional monomer comprises one or a mixture of several of polyethylene glycol (1000) monomethyl ether methacrylate, polyethylene glycol (2000) monomethyl ether methacrylate, polyethylene glycol (4000) monomethyl ether methacrylate, polyethylene glycol (6000) monomethyl ether methacrylate, polyethylene glycol (8000) monomethyl ether methacrylate, and acrylamide.
Further preferably, the water-soluble functional monomer comprises one or a mixture of more of polyethylene glycol (6000) monomethyl ether methacrylate, polyethylene glycol (8000) monomethyl ether methacrylate and acrylamide.
The drag-increasing in-situ gel deep profile control agent comprises 3-8% of water-soluble functional monomers in percentage by weight. For example, the water-soluble functional monomer is mixed in the drag-increasing in-situ gel deep profile control agent of the present invention at 3%, 4%, 5%, 6%, 7% or 8%.
Through practice, when the proportion of the water-soluble functional monomer in the resistance-increasing in-situ gel deep profile control agent is lower than 3%, the gel forming strength of the profile control agent is lower (the gel forming strength can only reach the A level of Sydansk gel code method), and when the proportion of the water-soluble functional monomer in the resistance-increasing in-situ gel deep profile control agent is higher than 8%, the gel forming time of the profile control agent is too short (the gel forming time is less than 2 days), and the requirement of the in-situ deep profile control on the gel forming time cannot be met.
Further preferably, the proportion of the water-soluble functional monomer in the resistance-increasing in-situ gel deep profile control agent is 5-8%.
Functional micro-nano particles
The function of the functional micro-nano particles is to provide a crosslinking center for the three-dimensional network structure of the gel after polymerization.
In some preferred embodiments, the functional micro-nano particles comprise one or two of crosslinked polystyrene micro-nano particles with carbon-carbon double bonds on the surface and silica gel micro-nano particles with carbon-carbon double bonds on the surface.
Wherein, the crosslinked polystyrene micro-nano particles with carbon-carbon double bonds on the surface are prepared by an emulsion polymerization method at 45-55 ℃ by taking diethylbenzene as a crosslinking agent, styrene as a hydrophobic monomer, acrylamide as a hydrophilic monomer, fatty alcohol polyoxyethylene ether sulfate (AES) as an emulsifier and azo diisobutyl amidine hydrochloride as an initiator.
In some preferred embodiments, the preparation method of the crosslinked polystyrene micro-nano particles with carbon-carbon double bonds on the surface comprises the steps of weighing 77-79.5 g of deionized water, 0.5-3.0 g of fatty alcohol polyoxyethylene ether sulfate (AES) and 0.5g of acrylamide in a three-neck flask at room temperature, stirring and dissolving at a stirring rate of 200rpm, weighing 1.5g of diethylbenzene and 18g of styrene in the flask, stirring and emulsifying for 30 minutes at a stirring rate of 400-500 rpm, introducing nitrogen into the flask at a speed of 1mL/min while stirring and emulsifying, transferring the flask into a constant-temperature water bath kettle after the emulsification is finished, simultaneously maintaining stirring, adding 0.3-0.5 g of azodiisobutylamidine hydrochloride into the flask to initiate a reaction when the temperature is raised to 55 ℃, after the constant-temperature reaction is carried out for 3 hours, and stopping the reaction at the room temperature to obtain the crosslinked polystyrene micro-nano particles with carbon-carbon double bonds on the surface of 50 nm-10 mu m. .
The silica gel micro-nano particles with carbon-carbon double bonds on the surfaces are prepared by taking vinyltriethoxysilane as a raw material and AES as an emulsifier through hydrolysis at 45-55 ℃.
In some preferred embodiments, the preparation method of the silica gel micro-nano particles with carbon-carbon double bonds on the surface comprises the steps of weighing 84.5-89.0 g of deionized water and 0.5-1.0 g of emulsifier AES in a three-neck flask at room temperature, stirring and dissolving at a stirring rate of 200rpm, then weighing 10-15 g of vinyltriethoxysilane in the flask, stirring and emulsifying for 30 minutes at a stirring rate of 400-500 rpm, transferring the flask into a constant-temperature water bath kettle after the emulsification is finished, maintaining stirring, heating to 50 ℃, reacting at constant temperature for 8 hours, standing the room temperature, and stopping the reaction to obtain the silica gel micro-nano particles with carbon-carbon double bonds on the surface, wherein the particle size distribution of the silica gel micro-nano particles is 1-10 mu m.
In some preferred embodiments, the functional micro-nano particles have a particle size distribution of 50nm to 10 μm.
Through practice, when the particle size of the functional micro-nano particles is smaller than 50nm, too many crosslinking nodes are caused, the flooding system is excessively crosslinked, even floccules are generated, and when the particle size of the functional micro-nano particles is larger than 10 mu m, too few crosslinking nodes are caused, and the gelling strength of the flooding system is reduced.
The drag-increasing in-situ gel deep profile control agent comprises 0.5-2% of functional micro-nano particles by weight percent. For example, the functional micro-nano particles are mixed in the drag-increasing in-situ gel deep profile control agent of the invention in an amount of 0.5%, 1%, 1.5% or 2%.
Through practice, too many crosslinking nodes are caused when the proportion of the functional micro-nano particles is too large, the profile control system is excessively crosslinked and even floccules are generated, and too few crosslinking nodes are caused when the proportion of the functional micro-nano particles is too small, and the gel forming strength of the profile control system is reduced.
Further preferably, the proportion of the functional micro-nano particles in the resistance-increasing in-situ gel deep profile control agent is 0.8-2%.
Glue forming control agent
The gel forming control agent is used for decomposing to generate free radicals, and initiating the water-soluble functional monomer and the functional micro-nano particles to generate free radical polymerization reaction.
In some preferred embodiments, the gel forming control agent comprises one or a mixture of several of azobisiso Ding Mi hydrochloride, azobisisopropylimidazoline, t-butyl peroxybenzoate, t-amyl hydroperoxide, t-butyl cumyl peroxide.
Further preferably, the gum-forming control agent is azobisisopropylimidazoline, tert-butyl peroxybenzoate, tert-amyl hydroperoxide.
The resistance-increasing in-situ gel deep profile control agent comprises 0.3-1% of a gel forming control agent by weight percent. For example, the gel forming control agent is mixed in the drag-increasing in-situ gel deep profile control agent of the present invention in an amount of 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9% or 1%.
Through practice, when the proportion of the glue-forming control agent is too large, the glue-forming time of the profile control system is too short (less than 1 day), the construction requirements cannot be met, and when the proportion of the glue-forming control agent is too small, the profile control system cannot form glue.
Further preferably, the proportion of the gel forming control agent in the resistance-increasing in-situ gel deep profile control agent is 0.4-0.8%.
Water and its preparation method
The water adopted by the resistance-increasing in-situ gel deep profile control agent is stratum water or seawater.
Further preferably, the water used in the present invention has a mineralization of at most 30X 10 4 mg/L.
In a second aspect, the invention also provides a preparation method of the drag-increasing in-situ gel deep profile control agent, which comprises the following steps:
(1) Adding water-soluble functional monomers into water according to a proportion, and stirring to completely dissolve the water-soluble functional monomers;
(2) Adding functional micro-nano particles according to the proportion under stirring, and continuing stirring to completely dissolve the functional micro-nano particles;
(3) Adding the gel forming control agent according to the proportion, and stirring to obtain the resistance-increasing in-situ gel deep profile control agent.
The proportion, the components, the actions and the like of the water-soluble functional monomer, the functional micro-nano particles, the gel forming control agent and the water adopted in the preparation of the drag-increasing in-situ gel deep profile control agent are the same as those in the drag-increasing in-situ gel deep profile control agent provided by the first aspect of the invention, and the invention is not repeated here.
In some preferred embodiments, the preparation method of the resistance-increasing in-situ gel deep profile control agent comprises the steps of adding 3-8% of water-soluble functional monomer into water at normal temperature, stirring for 5 minutes under the condition that the stirring speed is not less than 20rpm to completely dissolve the water-soluble functional monomer, preparing a functional monomer solution, adding 0.5-2% of functional micro-nano particles into the functional monomer solution under the condition of maintaining stirring, stirring for 5 minutes to uniformly disperse the functional micro-nano particles in the functional monomer solution, and finally adding 0.3-1% of a gel forming control agent into the functional monomer solution, and continuing stirring for 5 minutes to obtain the resistance-increasing in-situ gel deep profile control agent.
The initial viscosity of the drag-increasing in-situ gel deep profile control agent prepared by the method is 1-2 mPas, the gel forming time in an oil reservoir at 50-120 ℃ is adjustable and controllable for 5-15 days, and the dehydration rate is lower than 10% after the gel forming is carried out at the constant temperature of 120 ℃ for 90 days.
Examples
The invention is further illustrated by means of the following examples, which are not intended to limit the scope of the invention. The experimental methods without specific conditions noted in the following examples follow conventional methods and conditions.
Example 1
(1) Preparation of crosslinked polystyrene micro-nano particles with carbon-carbon double bonds on surface
At room temperature, 77g of deionized water, 3gAES g of acrylamide and 0.5g of acrylamide are weighed and dissolved in a three-neck flask under stirring at a stirring rate of 200rpm, then 1.5g of diethylbenzene and 18g of styrene are weighed and emulsified in the flask under stirring at a stirring rate of 400-500 rpm for 30 minutes, nitrogen is introduced into the flask at a speed of 1mL/min while stirring and emulsification is finished, the flask is transferred to a constant-temperature water bath kettle while stirring is maintained, when the temperature is raised to 55 ℃, 0.3-0.5 g of azobisisobutylammonium hydrochloride is added into the flask to initiate reaction, after the constant-temperature reaction is carried out for 3 hours, the temperature is raised to room temperature, and the reaction is stopped, so that the crosslinked polystyrene micro-nano particles with carbon-carbon double bonds on the surface and with particle size distribution of 50 nm-2 μm are obtained.
(2) Preparation of resistance-increasing in-situ gel deep profile control agent
At normal temperature, adding 2% of polyethylene glycol (1000) monomethyl ether methacrylate and 3% of acrylamide into simulated formation water with the mineralization degree of 10 multiplied by 10 4 mg/L according to the mass percentage, stirring for 5 minutes under the condition that the stirring speed is more than or equal to 20rpm, completely dissolving to prepare an aqueous solution with the total mass percentage of monomers, adding 1.5% of crosslinked polystyrene micro-nano particles with the particle size distribution of 50 nm-2 mu m and carbon-carbon double bonds on the surface into the aqueous solution of functional monomers under the condition of maintaining stirring, stirring for 5 minutes to uniformly disperse the crosslinked polystyrene micro-nano particles, and adding 0.5% of azobisisopropylimidazoline into the aqueous solution of functional monomers under the condition of maintaining stirring, and continuing stirring for 5 minutes to obtain the resistance-increasing type in-situ gel deep profile control agent.
The initial viscosity of the profile control agent is 1.37 mPas, the gel forming time at 60 ℃ is 7 days, the gel forming strength can reach E grade specified by Sydansk gel code method, the state before and after gel forming is shown in figure 1, and the microstructure after gel forming is shown in figure 2. As can be seen from fig. 2, the profile control agent has a three-dimensional network structure taking crosslinked polystyrene micro-nano particles as crosslinking nodes after being gelled.
Example 2
(1) Preparation of crosslinked polystyrene micro-nano particles with carbon-carbon double bonds on surface
At room temperature, weighing 79.5g of deionized water, 0.5gAES g of acrylamide and 0.5g of acrylamide in a three-neck flask, stirring and dissolving at a stirring speed of 200rpm, then weighing 1.5g of diethylbenzene and 18g of styrene in the flask, stirring and emulsifying for 30 minutes at a stirring speed of 400-500 rpm, introducing nitrogen into the flask at a speed of 1mL/min while stirring and emulsifying, transferring the flask to a constant-temperature water bath kettle after the emulsification is finished, maintaining stirring, adding 0.3-0.5 g of azo diisobutylamidine hydrochloride into the flask when the temperature rises to 55 ℃ to initiate a reaction, after the constant-temperature reaction is carried out for 3 hours, stopping the reaction at room temperature, and obtaining the crosslinked polystyrene micro-nano particles with the particle size distribution of 1-10 mu m and carbon-carbon double bonds on the surface.
(2) Preparation of resistance-increasing in-situ gel deep profile control agent
At normal temperature, according to mass percent, polyethylene glycol (2000) monomethyl ether methacrylate 2%, polyethylene glycol (4000) monomethyl ether 1% and acrylamide 3% are firstly added into simulated stratum water with mineralization degree of 20 multiplied by 10 4 mg/L, stirred for 5 minutes under the condition that stirring speed is more than or equal to 20rpm, so as to completely dissolve the mixture, and prepare aqueous solution with total monomer mass percent of 6%, under the condition of maintaining stirring, 0.8% of crosslinked polystyrene micro-nano particles with particle size distribution of 1-10 mu m and carbon-carbon double bonds on the surface are added into the aqueous solution of functional monomer, stirred for 5 minutes, so that the particles are uniformly dispersed, and under the condition of maintaining stirring, 0.7% of tert-butyl peroxybenzoate is added into the aqueous solution of functional monomer, and stirring is continued for 5 minutes, so as to obtain the resistance-increasing type in-situ gel deep profile control agent.
The initial viscosity of the profile control agent is 1.51 mPas, the gel forming time at 90 ℃ is 7 days, the gel forming strength can reach E grade specified by Sydansk gel code method, the state before and after gel forming is shown in figure 3, and the microstructure after gel forming is shown in figure 4. As can be seen from fig. 4, the profile control agent has a three-dimensional network structure with crosslinked polystyrene micro-nano particles as crosslinking nodes after being gelled.
Example 3
(1) Preparation of silica gel micro-nano particles with carbon-carbon double bonds on surface
At room temperature, weighing 84.5g of deionized water and 0.5gAES g of deionized water in a three-neck flask, stirring and dissolving at a stirring rate of 200rpm, then weighing 15g of vinyltriethoxysilane in the flask, stirring and emulsifying for 30 minutes at a stirring rate of 400-500 rpm, transferring the flask into a constant-temperature water bath kettle after the emulsification is finished, simultaneously maintaining stirring, raising the temperature to 50 ℃, reacting at constant temperature for 8 hours, then, stopping reacting at room temperature, and obtaining the silica gel micro-nano particles with carbon-carbon double bonds on the surface, wherein the particle size distribution of the silica gel micro-nano particles is 1-10 mu m.
(2) Preparation of resistance-increasing in-situ gel deep profile control agent
At normal temperature, adding 3% of polyethylene glycol (6000) monomethyl ether methacrylate, 3% of polyethylene glycol (8000) monomethyl ether methacrylate and 2% of acrylamide into simulated stratum water with mineralization degree of 30 multiplied by 10 4 mg/L according to mass percentage, stirring for 5 minutes under the condition that stirring speed is more than or equal to 20rpm to completely dissolve the mixture to prepare an aqueous solution with total monomer mass percentage of 8%, adding 1% of silica gel micro-nano particles with particle size distribution of 1-10 mu m and carbon-carbon double bonds on the surface into the aqueous solution of the functional monomer under the condition of maintaining stirring, stirring for 5 minutes to uniformly disperse the silica gel micro-nano particles, and adding 0.3% of tertbutyl hydrogen peroxide and 0.3% of tert-butyl cumyl peroxide into the aqueous solution of the functional monomer under the condition of maintaining stirring to ensure that the total concentration of a gel forming control agent in the aqueous solution of the functional monomer is 0.6%, and continuing stirring for 5 minutes to obtain the drag-increasing type in-situ gel deep profile control agent.
The initial viscosity of the profile control agent is 1.63 mPas, the gel forming time at 120 ℃ is 7 days, the gel forming strength can reach E grade specified by Sydansk gel code method, the state before and after gel forming is shown in figure 5, and the microstructure after gel forming is shown in figure 6. As can be seen from fig. 6, the profile control agent has a three-dimensional network structure taking silica gel micro-nano particles as crosslinking nodes after gel formation.
Example 4
Preparation of resistance-increasing in-situ gel deep profile control agent
At normal temperature, according to mass percent, polyethylene glycol (1000) monomethyl ether methacrylate 2% and acrylamide 4% are firstly added into simulated stratum water with the mineralization degree of 10 multiplied by 10 4 mg/L, the mixture is stirred for 5 minutes under the condition that the stirring speed is more than or equal to 20rpm, the mixture is completely dissolved to prepare an aqueous solution with the total mass percent of monomers of 6%, under the condition of maintaining stirring, 1% of silicon dioxide gel micro-nano particles with the particle size distribution of 1-10 mu m and the surface with carbon-carbon double bonds are added into the aqueous solution of functional monomers (the preparation method is the same as that of example 3) and 0.8% of crosslinked polystyrene micro-nano particles with the particle size distribution of 1-10 mu m and the surface with carbon-carbon double bonds are stirred for 5 minutes, the azo diiso Ding Mi-ine hydrochloride is added into the aqueous solution of functional monomers and the mixture is continuously stirred for 5 minutes, and the block-increasing type in-site gel deep profile control agent is obtained.
The initial viscosity of the profile control agent is 1.36 mPas, the gel forming time at 50 ℃ is 7 days, the gel forming strength can reach E grade specified by Sydansk gel code method, the state before and after gel forming is shown in figure 7, and the microstructure after gel forming is shown in figure 8. As can be seen from fig. 8, the profile control agent has a three-dimensional network structure with silica gel micro-nano particles and crosslinked polystyrene micro-nano particles as crosslinking nodes after gel formation.
Test example 1 measurement of the injectability and the blocking Property of the resistance-increasing in-situ gel deep Profile control agent
To illustrate the beneficial effects of the present invention, an artificial core having a porosity of 23.6%, a permeability of 1500mD, and a size of Φ2.5cm×10cm was used, and the injection and blocking properties of the drag-increasing in-situ gel deep profile control agent and the existing weak gel profile control system prepared in examples 1 to 4 (the system is composed of 0.3% polyacrylamide having a molecular weight of 1000 ten thousand, 0.3% water-soluble phenolic resin cross-linking agent, and 0.3% ammonium chloride.) were determined as follows, to ensure adequate dissolution of the polymer, the system was formulated in deionized water, and the initial viscosity of the system was 175mpa·s:
Firstly, vacuumizing saturated water from a core, then placing the core into a core holder, injecting a profile control agent with 1 Pore Volume (PV) into the core at an injection speed of 3mL/min, recording the maximum injection pressure, closing valves at two ends of the core holder after the injection of the profile control agent is finished, keeping the temperature at a set temperature for 7 days, opening valves at two ends of the core holder after the constant temperature is finished, injecting water into the core at an injection speed of 3mL/min, measuring breakthrough pressure and permeability K 1 after blockage, and calculating the blockage rate.
The blocking rate was calculated using the following formula:
the measurement results are shown in Table 1.
TABLE 1 results of in situ gel deep profile control agent with increased resistance and injection and blocking of weak gel profile control system
The results in Table 1 show that the maximum injection pressure of the resistance-increasing in-situ gel deep profile control agent prepared in examples 1-4 injected with 1PV is 0.4-0.8 MPa, and the maximum injection pressure of the weak gel profile control system injected with 1PV is 1.5MPa. This shows that in the oil reservoir with the same porosity and permeability, the resistance-increasing in-situ gel deep profile control agent provided by the invention is obviously superior to the existing weak gel profile control system in terms of injectability, and can realize profile control of the deeper part of the oil reservoir. After the drag-increasing in-situ gel deep profile control agent prepared in examples 1-4 is formed into gel in a core at a set temperature, the blocking rate of the core is higher than 97%, the breakthrough pressure is higher than 15MPa, the blocking rate of the existing weak gel profile control agent is 80.7%, and the breakthrough pressure is 2.3MPa. This shows that in the oil reservoir with the same porosity and permeability, the resistance-increasing in-situ gel deep profile control agent provided by the invention is obviously superior to the existing weak gel profile control system in terms of plugging property, and can effectively plug a strong water channeling channel in the oil reservoir.
Test example 2 measurement of temperature resistance of resistance-increasing in-situ gel deep profile control agent
In order to demonstrate the beneficial effects of the present invention, the temperature resistance of the enhanced in situ gel deep profile control agent prepared in examples 1-4 and the existing weak gel profile control system (which is composed of 0.3% polyacrylamide with a molecular weight of 1000 ten thousand, 0.3% water-soluble phenolic resin cross-linking agent and 0.3% ammonium chloride, and is prepared in deionized water) was measured to ensure that the polymer was sufficiently dissolved. The specific measurement steps are as follows:
firstly, 100mL of the resistance-increasing in-situ gel deep profile control agent prepared in examples 1-4 and the existing weak gel profile control system are respectively filled into a high-temperature high-pressure aging tank, the temperature is kept constant for 7 days at a set temperature to form gel, after the gel is formed, the high-temperature high-pressure aging tank is placed in a 120 ℃ environment to age for 90 days, the water precipitation quantity V 1 is measured, the dehydration rate is calculated, and the dehydration rate is used as an index for measuring the temperature resistance of the profile control agent.
The water separation rate of the profile control agent is calculated by adopting the following formula:
The measurement results are shown in Table 2.
TABLE 2 temperature resistance measurement results of resistance-increasing in-situ gel deep profile control agent and weak gel profile control system
The results shown in Table 2 demonstrate that after the gel formation of the resistance-increasing in-situ gel deep profile control agent prepared in examples 1-4, the dehydration rate at a constant temperature of 120 ℃ for 90 days is lower than 7%, while the weak gel profile control system is completely dehydrated after the constant temperature of 120 ℃ for 90 days. The invention shows that the resistance-increasing in-situ gel deep profile control agent provided by the invention has excellent temperature resistance and can be used for deep profile control of 120 ℃ high-temperature oil reservoirs.
Test example 3 measurement of the control Performance of the gel Forming time of the resistance-increasing in-situ gel deep Profile control agent
In order to illustrate the beneficial effects of the present invention, the time required for the gel strength to reach the E level specified by the Sydansk gel code method was taken as the gel forming time, and the gel forming time was measured at 90 ℃ in the case that the addition amount and composition of the functional monomer and the functional micro-nano particles were kept unchanged, and only the addition amount of the gel control agent was changed. The measurement results are shown in Table 3.
TABLE 3 measurement of the control Performance of the gel Forming time of the resistance increasing in situ gel deep profile control agent
The results shown in Table 3 demonstrate that the gel forming time of the drag-increasing in-situ gel deep profile control agent prepared in example 2 increases with decreasing addition of the gel forming control agent. The time for generating gel by the resistance-increasing in-situ gel deep profile control agent in the stratum can be flexibly adjusted within 5-15 days by adjusting the addition amount and combination of the gel forming control agent.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited to the specific details of the above embodiments, and various simple modifications can be made to the technical solution of the present invention within the scope of the technical concept of the present invention, and all the simple modifications belong to the protection scope of the present invention.
In addition, the specific features described in the above embodiments may be combined in any suitable manner, and in order to avoid unnecessary repetition, various possible combinations are not described further.
Moreover, any combination of the various embodiments of the invention can be made without departing from the spirit of the invention, which should also be considered as disclosed herein.
Claims (12)
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