CN110872504A - Acid-resistant strong gel plugging agent and preparation method thereof - Google Patents
Acid-resistant strong gel plugging agent and preparation method thereof Download PDFInfo
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- C09K8/50—Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls
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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
- C09K8/50—Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/50—Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls
- C09K8/504—Compositions based on water or polar solvents
- C09K8/506—Compositions based on water or polar solvents containing organic compounds
- C09K8/508—Compositions based on water or polar solvents containing organic compounds macromolecular compounds
- C09K8/5083—Compositions based on water or polar solvents containing organic compounds macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
Abstract
The invention relates to the technical field of water plugging of oil wells used in oil exploitation, in particular to an acid-resistant strong gel plugging agent and a preparation method thereof, wherein the acid-resistant strong gel plugging agent comprises the following components in percentage by weight: a main agent: 3 to 10 percent; acid-resistant monomers: 0.1 to 1.0 percent; initiator: 0.1 to 0.5 percent; a crosslinking agent: 0.5 to 1.5 percent. The acid-resistant strong gel plugging agent disclosed by the invention is simple in preparation method, wide in raw material source, strong in plugging performance and good in acid resistance, and provides a new technical reserve for a chemical profile control water plugging technology.
Description
Technical Field
The invention relates to the technical field of water plugging of oil wells used in oil exploitation, in particular to an acid-resistant strong gel plugging agent and a preparation method thereof.
Background
In the low-permeability reservoir development process, due to the influence of stratum cracks and heterogeneity and the fracturing transformation operation, water is easily communicated after oil well measures, the water content rise range is large, the water content is high, and the production of the oil well and the long-term stable production of the oil field are seriously influenced by the existence of the wells. The conventional water plugging technology at present has the problems of incapability of plugging a high water-cut well or high difficulty in increasing the yield after plugging, and the like, and can not meet the requirements of water control and yield increase of oil reservoirs.
The water shutoff and acidification combined operation of the oil well is an effective measure for improving the water flooding efficiency and the recovery ratio of the heterogeneous oil reservoir. The oil well firstly blocks water in the water blocking and acidification combined action, and then is acidized, acid used in the oil field acidizing treatment is mainly earth acid, the earth acid can not only cause degradation of polyacrylamide chains, but also cause strength reduction of gel frameworks and branched chains, and the microstructure of gel is sparse and weakened, so that the used plugging agent is required to have acid resistance. The acid resistance of the plugging agent researched and developed in China at present is generally low, and the research of the acid-resistant strong gel plugging agent which is particularly suitable for the water plugging and acidizing combined operation of low-permeability oil reservoirs is almost blank. Therefore, the development of a strong gel blocking agent capable of resisting strong acid is urgent.
Disclosure of Invention
The invention overcomes the defects of the prior art and provides the acid-resistant strong gel plugging agent and the preparation method thereof, in particular the acid-resistant strong gel plugging agent has the characteristics of strong plugging performance and good acid resistance.
The technical problem solved by the invention can be realized by adopting the following technical scheme:
the acid-resistant strong gel plugging agent comprises the following components in percentage by weight:
a main agent: 3 to 10 percent;
acid-resistant monomers: 0.1 to 1.0 percent;
initiator: 0.1 to 0.5 percent;
a crosslinking agent: 0.5 to 1.5 percent.
The acid-resistant strong gel plugging agent comprises the following components in percentage by weight:
a main agent: 7.0 percent;
acid-resistant monomers: 0.5 percent;
initiator: 0.3 percent;
a crosslinking agent: 1.0 percent.
The main agent is one or a mixture of acrylamide, acrylonitrile and acrylic acid.
The acid-resistant monomer is acrylate containing fluorine groups.
The initiator is one or a mixture of potassium persulfate, ammonium persulfate and azodiisobutyronitrile.
The cross-linking agent is one or a mixture of N, N-methylene bisacrylamide and polyethyleneimine.
The preparation method of the acid-resistant strong gel plugging agent comprises the following steps
The method comprises the following steps: firstly, taking the main agent according to the formula amount, putting the temperature-resistant HDPE bottle on a magnetic stirrer in the temperature-resistant HDPE bottle, and uniformly stirring.
Step two: and (3) adding acid-resistant monomers in a formula amount on the basis of the step one, and stirring until the mixture is uniform and transparent.
Step three: and (5) adding a cross-linking agent and an initiator on the basis of the step two, uniformly stirring, and putting the uniformly stirred solution into a constant-temperature oven to form the gel.
The invention has the beneficial effects that:
compared with the prior art, the main agent is one or a mixture of acrylamide, acrylonitrile and acrylic acid, has the characteristics of wide source and low price, and is used as the main agent of the gel blocking agent; the acid-resistant monomer is acrylate containing fluorine groups, any one of the acrylate containing fluorine groups can be applied to the invention, the acrylate containing fluorine groups has the characteristic of easy dissolution on site, and the acid-resistant monomer has the function of acid resistance; the initiator is one or a mixture of potassium persulfate, ammonium persulfate and azodiisobutyronitrile, has the characteristics of easy obtainment and small dosage, and plays a role in initiating a gel system; the crosslinking agent is one or a mixture of N, N-methylene bisacrylamide and polyethyleneimine, and has the characteristics of good crosslinking effect, difficult dehydration and uniform gelling.
Drawings
The invention is further illustrated with reference to the following figures and examples.
FIG. 1 is a schematic diagram of the effect of the acid resistance test of the present invention at 50 ℃.
FIG. 2 is a schematic diagram showing the effect of the acid resistance test of the present invention at 60 ℃.
FIG. 3 is a schematic diagram showing the effect of the acid resistance test of the present invention at 70 ℃.
FIG. 4 is a schematic diagram of the effect of the acid resistance test of the present invention at 80 ℃.
FIG. 5 is a schematic diagram showing the effect of the acid resistance test of the present invention at 90 ℃.
FIG. 6 is a graph illustrating the injection pressure versus the number of volumes of injection fluid in accordance with the present invention.
FIG. 7 is a graph illustrating the injection pressure versus the number of volumes of injection fluid in accordance with the present invention.
FIG. 8 is a graph illustrating the injection pressure versus the number of volumes of injection fluid in accordance with the present invention.
Detailed Description
Example 1:
the acid-resistant strong gel plugging agent comprises the following components in percentage by weight:
a main agent: 3 to 10 percent;
acid-resistant monomers: 0.1 to 1.0 percent;
initiator: 0.1 to 0.5 percent;
a crosslinking agent: 0.5 to 1.5 percent.
The acid-resistant strong gel plugging agent is prepared by the following method, and comprises the following steps
The method comprises the following steps: firstly, taking the main agent according to the formula amount, putting the temperature-resistant HDPE bottle on a magnetic stirrer in the temperature-resistant HDPE bottle, and uniformly stirring.
Step two: and (3) adding acid-resistant monomers in a formula amount on the basis of the step one, and stirring until the mixture is uniform and transparent.
Step three: and (5) adding a cross-linking agent and an initiator on the basis of the step two, uniformly stirring, and putting the uniformly stirred solution into a constant-temperature oven to form the gel.
Example 2:
the acid-resistant strong gel plugging agent comprises the following components in percentage by weight:
a main agent: 3 percent;
acid-resistant monomers: 0.1 percent;
initiator: 0.1 percent;
a crosslinking agent: 0.5 percent.
The main agent is one or a mixture of acrylamide, acrylonitrile and acrylic acid.
The acid-resistant monomer is acrylate containing fluorine groups.
The initiator is one or a mixture of potassium persulfate, ammonium persulfate and azodiisobutyronitrile.
The cross-linking agent is one or a mixture of N, N-methylene bisacrylamide and polyethyleneimine.
The acid-resistant strong gel plugging agent is prepared by the following method, and comprises the following steps
The method comprises the following steps: firstly, 3 percent of acrylonitrile is taken and put in a temperature-resistant HDPE bottle, and the temperature-resistant HDPE bottle is placed on a magnetic stirrer and is stirred uniformly.
Step two: and (3) adding 0.1% of ethyl fluorohexyl acrylate on the basis of the step one, and stirring until the mixture is uniform and transparent.
Step three: and on the basis of the second step, adding 0.5% of polyethyleneimine and 0.1% of ammonium persulfate, uniformly stirring, and placing the uniformly stirred solution into a constant-temperature oven to form the gel.
The main agent is one or a mixture of acrylamide, acrylonitrile and acrylic acid, has the characteristics of wide source and low price, and is used as the main agent of the gel blocking agent in the invention; the acid-resistant monomer is acrylate containing fluorine groups, any one of the acrylate containing fluorine groups can be suitable for the invention, the acrylate containing fluorine groups has the characteristic of easy dissolution on site, the function in the invention is acid resistance, and the acrylate containing fluorine groups is preferably ethyl fluorohexyl acrylate; the initiator is one or a mixture of potassium persulfate, ammonium persulfate and azodiisobutyronitrile, has the characteristics of easy obtainment and small dosage, and plays a role in initiating a gel system; the cross-linking agent is one or the mixture of N, N-methylene bisacrylamide and polyethyleneimine, has the characteristics of good cross-linking effect, difficult dehydration and uniform gelling, and plays a role in cross-linking.
Example 3:
the acid-resistant strong gel plugging agent comprises the following components in percentage by weight:
a main agent: 10 percent; the main agent is acrylic acid;
acid-resistant monomers: 1.0 percent; the acid-resistant monomer is ethyl fluorohexyl acrylate;
initiator: 0.5 percent; the initiator is azodiisobutyronitrile;
a crosslinking agent: 1.5 percent; the cross-linking agent is a mixture of N, N-methylene bisacrylamide and polyethyleneimine.
The acid-resistant strong gel plugging agent is prepared by the following method, and comprises the following steps
The method comprises the following steps: firstly, 10 percent of acrylic acid is taken and put in a temperature-resistant HDPE bottle, and the temperature-resistant HDPE bottle is put on a magnetic stirrer and is stirred uniformly.
Step two: and (3) adding 1.0% of ethyl fluorohexyl acrylate on the basis of the step one, and stirring until the mixture is uniform and transparent.
Step three: and (2) adding 1.5% of a mixture of N, N-methylene bisacrylamide and polyethyleneimine and 0.5% of azodiisobutyronitrile on the basis of the step two, uniformly stirring, and placing the uniformly stirred solution into a constant-temperature oven to form the gel.
Example 4:
the acid-resistant strong gel plugging agent comprises the following components in percentage by weight:
a main agent: 7.0 percent; the main agent is acrylamide;
acid-resistant monomers: 0.5 percent; the acid-resistant monomer is ethyl fluorohexyl acrylate;
initiator: 0.3 percent; the initiator is potassium persulfate;
a crosslinking agent: 1.0 percent; the cross-linking agent is N, N-methylene bisacrylamide.
The acid-resistant strong gel plugging agent is prepared by the following method, and comprises the following steps
The method comprises the following steps: firstly, taking 7.0 percent of acrylamide, putting the acrylamide into a temperature-resistant HDPE bottle, putting the temperature-resistant HDPE bottle on a magnetic stirrer, and uniformly stirring.
Step two: and (3) adding 0.5% of ethyl fluorohexyl acrylate on the basis of the step one, and stirring until the mixture is uniform and transparent.
Step three: and (2) adding 0.3% of N, N-methylene bisacrylamide and 1.0% of potassium persulfate on the basis of the step two, uniformly stirring, and placing the uniformly stirred solution into a constant-temperature oven to form the gel.
The formula for preparing the acid-resistant strong gel plugging agent in the embodiment is experimentally verified:
(1) preparation of acid-resistant monomer solution
465ml of simulated water is measured and put in a beaker, the beaker is placed under a stirrer, a stirring rod is arranged, the bottom end of the stirring rod is about 1cm away from the bottom of the beaker, the stirring speed of the stirrer is adjusted to 400r/min, and the simulated water is stirred to be vortex-shaped. Weighing 35g of ethyl fluorohexyl acrylate, adding the ethyl fluorohexyl acrylate into water in a stirring state at a constant speed, fully stirring for 4 hours until the solution is uniform and transparent, standing for 12 hours to fully hydrolyze the solution to obtain the acid-resistant monomer solution with the mass fraction, and storing the acid-resistant monomer solution in a refrigerator at 5 ℃ for later use.
(2) Synthesis method of acid-resistant strong gel plugging agent
Putting a 7.0% acrylamide solution into a temperature-resistant HDPE bottle, putting a beaker on a magnetic stirrer, adding the prepared 0.5% acid-resistant monomer solution, and stirring until the mixture is uniform and transparent; respectively adding 1.0% of potassium persulfate and 0.3% of N, N-methylene-bisacrylamide into a beaker, and uniformly stirring; placing the mixture in constant temperature ovens with different temperatures to form the gel.
(3) Operation method of acid resistance experiment
Preparing 15% of earth acid by using 12% of hydrochloric acid and 3% of hydrofluoric acid, uniformly stirring, and mixing the colloid blocking agent and the acid solution according to the volume ratio of 1: 1, slowly adding the mixture into a temperature-resistant HDPE bottle containing the gel-forming plugging agent, respectively placing the temperature-resistant HDPE bottle into a baking oven at 50 ℃, 60 ℃, 70 ℃, 80 ℃ and 90 ℃, soaking the temperature-resistant HDPE bottle in 15% earth acid for 24 hours, and observing the acid-resistant dehydration shrinkage rate of the temperature-resistant HDPE bottle; referring to fig. 1, 2, 3, 4 and 5, the acid resistance syneresis at different temperatures is shown in table 1.
TABLE 1 Table of acid dehydration shrinkage resistance at different temperatures
This example provides the blocking performance of the acid resistant strong gel blocking agent prepared in accordance with the present invention. The plugging performance experiment is to simulate the rock environment of an oil layer by the core, and the plugging capability of the acid-resistant strong gel plugging agent in the core is inspected by adopting the physical simulation experiment of conventional dynamic core plugging. In the embodiment, the permeability of the rock core is set to be 0.5 μm2, 0.8 μm2 and 1.2 μm2, the injection flow is 0.8mL/min, the confining pressure of the rock core holder is 4MPa, the gel is injected into the rock core at normal temperature, and the injection amount is unified to be 0.6 VP. Gelatinizing at 90 deg.C for 4 hr, and performing water flooding experiment.
The plugging performance of the acid-resistant strong gel plugging agent prepared in the embodiment is experimentally verified: the method comprises the measurement and processing of core physical property parameters and a physical simulation core plugging experiment.
The permeability was first measured for water. Putting the dried rock core into a rock core holder, applying a stable confining pressure of 4MPa, connecting the rock core holder to a vacuum system, and vacuumizing for about 12 h; fully saturating the vacuumized core with simulated water at one end of an inlet and an outlet, filling the simulated water into a storage tank, and connecting an experimental device; the core holder keeps stable confining pressure of 4MPa, partial leakage before the inlet end of the core of an experimental system is checked, simulated water is injected into the core at a certain flow rate (such as 0.4mL/min and 1mL/min), a pressure measuring system is opened to track and measure the pressure at the inlet end of the core at the same time until the monitored pressure is stable, and the stable pressure is recorded to be 4.5KPa, 2.8KPa and 1.9KPa respectively. The permeability was calculated according to the Darcy formula to be 0.5 μm2, 0.8 μm2, 1.2 μm2, respectively. The water tank and the high-pressure container tank are filled with the site simulation water and the prepared acid-resistant strong gel plugging agent, and the corresponding pipeline equipment is kept filled with all the fluids. The effective permeability of the rock core is measured by the same method as that of water. Injecting water until the pressure is kept stable, and recording the stable pressure at the moment as 1.2KPa, 2.0KPa and 2.5 KPa. Then changing to gel injection base liquid with the injection amount of 0.6VP, gelling at 90 ℃ for 4h, continuing injecting water until the pressure is stable, and recording the pressure at this time as 970 KPa. The plugging rate is calculated by the pressure data and is more than 99 percent, and the breakthrough pressure gradient is more than or equal to 20 MPa/m.
Fig. 6 is a graph of injection pressure versus volume of injected fluid, showing the plugging performance of an acid resistant strong gel plugging agent in a core. As is clear from fig. 2, the pressure slightly increased with the injection of the gel base liquid at the early stage of the injection of the gel base liquid, and the maximum injection pressure at this time was 8.7 KPa. After gelling for 4h, water flooding is continued, the pressure is sharply increased at the moment, the breakthrough pressure is 3.2MPa, after water flooding for 3PV, the pressure is stabilized at about 3.0MPa at the moment, and the final plugging rate reaches 99.9%, which shows that the acid-resistant strong gel can form effective plugging in a rock core of 0.5 mu m 2.
Fig. 7 is a graph of injection pressure versus volume of injected fluid, showing the plugging performance of an acid resistant strong gel plugging agent in a core. As is clear from fig. 3, the pressure slightly increased as the injection of the gel base liquid continued at the early stage of the injection of the gel base liquid, and the maximum injection pressure at this time was 7.0 KPa. After gelling for 4h, water flooding is continued, the pressure is increased sharply at the moment, a breakthrough is formed when the pressure reaches 3.1MPa, and the pressure fluctuates in an ascending manner along with the continuous water flooding, which shows that the acid-resistant strong gel plugging agent has better flushing resistance and good plugging property in a 0.8 mu m2 core.
Fig. 8 is a graph of injection pressure versus volume of injected fluid, showing plugging performance of the acid resistant strong gel plugging agent in the core. As can be seen from fig. 4, the pressure during the primary water flooding process was small and almost zero, and the pressure slightly increased with the injection of the gel base liquid, and the maximum injection pressure at this time was 5.5 KPa. After gelling for 4h, water flooding is continued, the pressure rises sharply at the moment, a breakthrough is formed when the pressure reaches 2.8MPa, the pressure has a rising fluctuation trend of different degrees along with the continuous progress of the water flooding, when the water flooding is carried out for 7PV, the pressure is stabilized at about 2.0MPa at the moment, and the blocking rate reaches 99.9 percent, which shows that the acid-resistant strong gel has better scouring resistance and good blocking performance in a rock core of 1.2 mu m 2.
Therefore, the acid-resistant strong gel plugging agent disclosed by the invention is simple in preparation method, wide in raw material source, strong in plugging performance and good in acid resistance, and provides a new technical reserve for a chemical profile control water plugging technology.
While the embodiments of the present invention have been described in detail with reference to the drawings, the present invention is not limited to the above embodiments, and various changes can be made without departing from the spirit of the present invention within the knowledge of those skilled in the art, and the scope of the present invention is within the scope of the claims.
It should be noted that all the directional indicators (such as up, down, left, right, front, and rear … …) in the embodiment of the present invention are only used to explain the relative position relationship between the components, the movement situation, etc. in a specific posture (as shown in the drawing), and if the specific posture is changed, the directional indicator is changed accordingly.
Technical solutions between various embodiments may be combined with each other, but must be realized by those skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination should not be considered to exist, and is not within the protection scope of the present invention.
Claims (7)
1. An acid-resistant strong gel plugging agent is characterized in that: the composite material comprises the following components in percentage by weight:
a main agent: 3 to 10 percent;
acid-resistant monomers: 0.1 to 1.0 percent;
initiator: 0.1 to 0.5 percent;
a crosslinking agent: 0.5 to 1.5 percent.
2. The acid-resistant strong gel plugging agent of claim 1, which is characterized in that: the composite material comprises the following components in percentage by weight:
a main agent: 7.0 percent;
acid-resistant monomers: 0.5 percent;
initiator: 0.3 percent;
a crosslinking agent: 1.0 percent.
3. The acid-resistant strong gel plugging agent of claim 1, which is characterized in that: the main agent is one or a mixture of acrylamide, acrylonitrile and acrylic acid.
4. The acid-resistant strong gel plugging agent of claim 1, which is characterized in that: the acid-resistant monomer is acrylate containing fluorine groups.
5. The acid-resistant strong gel plugging agent of claim 1, which is characterized in that: the initiator is one or a mixture of potassium persulfate, ammonium persulfate and azodiisobutyronitrile.
6. The acid-resistant strong gel plugging agent of claim 1, which is characterized in that: the cross-linking agent is one or a mixture of N, N-methylene bisacrylamide and polyethyleneimine.
7. A method for preparing acid-resistant gel blocking agent, which comprises the acid-resistant gel blocking agent of any one of claims 1 to 5, and is characterized in that: comprises the following steps
The method comprises the following steps: firstly, taking the main agent according to the formula amount, putting the temperature-resistant HDPE bottle on a magnetic stirrer in the temperature-resistant HDPE bottle, and uniformly stirring.
Step two: and (3) adding acid-resistant monomers in a formula amount on the basis of the step one, and stirring until the mixture is uniform and transparent.
Step three: and (5) adding a cross-linking agent and an initiator on the basis of the step two, uniformly stirring, and putting the uniformly stirred solution into a constant-temperature oven to form the gel.
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