CN114507515B - Supermolecule gel plugging agent for fractured stratum and preparation method and application thereof - Google Patents
Supermolecule gel plugging agent for fractured stratum and preparation method and application thereof Download PDFInfo
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- CN114507515B CN114507515B CN202210154918.6A CN202210154918A CN114507515B CN 114507515 B CN114507515 B CN 114507515B CN 202210154918 A CN202210154918 A CN 202210154918A CN 114507515 B CN114507515 B CN 114507515B
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- Prior art keywords
- stirring
- plugging agent
- mixed solution
- gel
- combination
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- 239000000178 monomer Substances 0.000 claims abstract description 119
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 118
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- 125000000524 functional group Chemical group 0.000 claims abstract description 47
- 239000006184 cosolvent Substances 0.000 claims abstract description 43
- 239000003999 initiator Substances 0.000 claims abstract description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000004094 surface-active agent Substances 0.000 claims abstract description 38
- 239000002994 raw material Substances 0.000 claims abstract description 26
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- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 34
- 239000000243 solution Substances 0.000 claims description 33
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 32
- KWIUHFFTVRNATP-UHFFFAOYSA-N Betaine Natural products C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 claims description 27
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 22
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- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 20
- 229920000536 2-Acrylamido-2-methylpropane sulfonic acid Polymers 0.000 claims description 19
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- HMZGPNHSPWNGEP-UHFFFAOYSA-N octadecyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)C(C)=C HMZGPNHSPWNGEP-UHFFFAOYSA-N 0.000 claims description 19
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- ZNAOFAIBVOMLPV-UHFFFAOYSA-N hexadecyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCCCCCCOC(=O)C(C)=C ZNAOFAIBVOMLPV-UHFFFAOYSA-N 0.000 claims description 17
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 16
- MMYYTPYDNCIFJU-UHFFFAOYSA-N calix[6]arene Chemical compound C1C(C=2)=CC=CC=2CC(C=2)=CC=CC=2CC(C=2)=CC=CC=2CC(C=2)=CC=CC=2CC(C=2)=CC=CC=2CC2=CC=CC1=C2 MMYYTPYDNCIFJU-UHFFFAOYSA-N 0.000 claims description 15
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- ZQMHJBXHRFJKOT-UHFFFAOYSA-N methyl 2-[(1-methoxy-2-methyl-1-oxopropan-2-yl)diazenyl]-2-methylpropanoate Chemical compound COC(=O)C(C)(C)N=NC(C)(C)C(=O)OC ZQMHJBXHRFJKOT-UHFFFAOYSA-N 0.000 claims description 4
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Classifications
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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
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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
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Abstract
The invention provides a supermolecular gel plugging agent for a fractured stratum, and a preparation method and application thereof. The supermolecule gel plugging agent comprises the following raw materials in percentage by mass: 18-45% of comonomer, 0.5-6.0% of surfactant, 0.1-2.0% of initiator, 0.1-2.0% of cosolvent, 0.05-0.5% of accelerator, 0.5-5% of saline solution and the balance of water; the comonomer is a combination of hydrophilic monomer, hydrophobic monomer and functional group molecule. The invention also provides a preparation method of the plugging agent. The gel plugging agent not only has the advantage of good matching property between gel type leakage-proof plugging materials and cracks, but also has higher temperature resistance and pressure resistance, has unique dynamic reversible characteristics, and can effectively perform plugging to form an integral compact plugging layer; meanwhile, the supermolecule gel plugging agent has excellent mechanical property and environment response capability.
Description
Technical Field
The invention relates to a supermolecular gel plugging agent for a fractured stratum, and a preparation method and application thereof, and belongs to the technical field of drilling fluid plugging.
Background
At present, in complex oil and gas reservoir drilling engineering, the problem of lost circulation becomes particularly prominent, and particularly, the problem of malignant lost circulation of a fractured stratum is solved. Lost circulation often occurs in relatively developed formations such as holes, seams, holes, and the like, and can be categorized into porous, fractured, and karst cave leaks by leak paths. Most lost circulation is associated with fractures. The cost of plugging the fractured leak is counted to be more than 90% of the total lost circulation cost. Because of the serious impediment to drilling work and the serious threat to drilling safety, the plugging of drilling fluid has become a difficult problem of 'neck blocking' which restricts the further development of Chinese exploration and development. Therefore, solving the problem of malignant leakage during drilling has become an urgent issue in the petroleum industry.
The plugging material is the basis and key of plugging technology. The conventional plugging material has better effect in treating permeability and small and medium-sized fracture well leakage, but has poorer adaptability to plugging large cracks or fracture holes and lower one-time plugging success rate. The fiber and the rigid material are plugging materials commonly used in oil fields, have poor compatibility with cracks, are extremely easy to cause the phenomenon of door sealing, and still have to improve the plugging effect. The polymer gel plugging agent is one of the common and effective plugging agents, and the polymer gel plugging agent is used for plugging cracks after solidification by injecting a certain amount of gel plugging agent solution into a leakage zone, so as to play a role in isolating drilling fluid and stratum fluid. Wherein, the performance of the gel plugging agent is the key of the success or failure of plugging. The gel plugging agent adopted at present has better effect in field application, but is deeply expanded along with oil and gas exploration and development, high temperature and high pressure become one of the main problems faced by well drilling plugging, and higher requirements are provided for the temperature resistance, salt tolerance and pressure bearing plugging performance of the gel plugging agent.
Aiming at the problems, the Chinese patent document CN111961452A provides a high-temperature-resistant high-strength touch-type gel plugging agent which has the advantages of high temperature resistance, high strength and thixotropy, but the gel forming controllability is to be improved; the Chinese patent document CN110734751A provides a high-temperature-resistant composite reinforced gel plugging agent which has the characteristics of high temperature resistance and delayed expansion, but has insufficient salt resistance and pressure bearing capacity; chinese patent document CN112480886A provides a polymer gel composite plugging agent which has good water swelling property, but is poor in temperature resistance, salt resistance and gel forming strength.
The supermolecular gel forms a gel network system with reversible structure and high performance characteristics under the self-assembly effect of non-covalent bond interaction. The supermolecule gel plugging agent not only has the advantage of good matching property between the conventional gel plugging material and a crack, but also has excellent temperature resistance, salt resistance and shearing thixotropic property, can realize full filling of a leakage space, has high mechanical strength, can realize long-term plugging of a leakage layer, and can effectively solve the defects of the conventional plugging material.
Therefore, it is necessary to develop a supermolecular gel plugging agent with both mechanical properties and environmental response capability to solve the problem of high-temperature and high-salt formation malignant leakage caused by cracking during drilling.
Disclosure of Invention
Aiming at the defects of the prior art, in particular to the problems of complex preparation process, insufficient pressure-bearing plugging capability, poor temperature resistance and salt resistance and the like of gel leakage-preventing/plugging materials conventionally used in the existing fractured formations, the invention provides a supermolecule gel plugging agent for the fractured formations, and a preparation method and application thereof.
The supermolecular gel plugging agent is formed based on non-covalent bond interaction and has excellent mechanical properties and outstanding environmental response capability, has the advantage of good matching property between gel type leakage-proof plugging materials and cracks, increases gel temperature resistance and pressure resistance through supermolecular structure design, has unique dynamic reversible characteristics, and can effectively perform plugging to form an integral compact plugging layer; meanwhile, the supermolecular gel plugging agent has excellent mechanical property and environment response capability, multiple hydrogen bond structural units are introduced onto a hydrophobic chain of the hydrophobic association polymer, and zwitterionic groups are introduced at the hydrophilic end of the hydrophobic chain, so that the supermolecular gel with high strength and environment response capability is formed, self-adaptive matching can be carried out on the supermolecular gel with cracks with complex dimensions, full filling of a leakage space is realized, and long-term stable plugging is realized.
The technical scheme of the invention is as follows:
the supermolecular gel plugging agent for the fractured stratum comprises the following raw materials in percentage by mass: 18-45% of comonomer, 0.5-6.0% of surfactant, 0.1-2.0% of initiator, 0.1-2.0% of cosolvent, 0.05-0.5% of accelerator, 0.5-5% of saline solution and the balance of water; the comonomer is a combination of hydrophilic monomer, hydrophobic monomer and functional group molecule.
According to the invention, the supermolecular gel plugging agent for the fractured stratum comprises the following raw materials in percentage by mass: 24-35% of comonomer, 3-5% of surfactant, 0.4-1% of initiator, 0.5-1% of cosolvent, 0.2-0.5% of accelerator, 1-3% of saline solution and the balance of water.
According to the invention, the mass ratio of the hydrophilic monomer, the hydrophobic monomer and the functional group molecules in the comonomer is preferably 6-8:1-3:1, and more preferably 7:2:1.
According to the invention, the hydrophilic monomer is preferably selected from two or more of acrylamide, acrylic acid, methacrylic acid, sodium acrylate, polyethylene glycol, N-isopropyl acrylamide, 2-acrylamido-2-methylpropanesulfonic acid, hexadecyldimethylallyl ammonium chloride, N-dodecyl acrylamide, N-vinyl pyrrolidone, 2-vinyl pyridine and N-hydroxyethyl acrylamide; further preferred are combinations of two or more of acrylamide, acrylic acid, methacrylic acid, sodium acrylate, polyethylene glycol, N-isopropylacrylamide, 2-acrylamido-2-methylpropanesulfonic acid, cetyl dimethylallyl ammonium chloride, 2-vinylpyridine, and N-vinylpyrrolidone.
According to the invention, the hydrophobic monomer is preferably selected from the group consisting of stearyl methacrylate, methyl methacrylate, butyl methacrylate, cetyl methacrylate, polyhydroxyethyl methacrylate, dimethylaminoethyl methacrylate, ethyl 2-methacrylate, beta-hydroxyethyl methacrylate, lauryl methacrylate, 4-trifluoro-methyl ethylene carbonate (CAS number: 167951-80-6) and 4-methylstyrene; more preferred are combinations of two or more of octadecyl methacrylate, lauryl methacrylate, cetyl methacrylate, butyl methacrylate, dimethylaminoethyl methacrylate, 4-methylstyrene and polyhydroxyethyl methacrylate.
According to the invention, the functional group molecules are preferably one or more than two of scleroglucan, chitosan, sodium alginate, 18-crown-6, cyclic dipeptide, beta-cyclodextrin, calix [6] arene, diethoxy column [5] arene and cucurbituril; further preferred are combinations of two or more of scleroglucan, chitosan, sodium alginate, beta-cyclodextrin, calix [6] arene and cucurbituril.
According to the invention, the surfactant is preferably one or more of sodium dodecyl benzene sulfonate, sodium dodecyl sulfate, dodecylphenol polyoxyethylene ether, stearic acid, sorbitan fatty acid, betaine and polysorbate.
According to the invention, the initiator is preferably one or more than two of diisopropyl peroxydicarbonate, tert-butyl peroxybenzoate, cumene hydroperoxide, potassium persulfate, ammonium persulfate, azobisisobutyrate, dimethyl azobisisobutyrate, azobisisobutyrate Ding Mi hydrochloride and sodium sulfite.
According to the invention, the cosolvent is preferably sulfate and/or a nitrogenous compound, more preferably a combination of sulfate and a nitrogenous compound, wherein the mass ratio of sulfate to nitrogenous compound is 1-2:1; the sulfate is anhydrous sodium sulfate or anhydrous calcium sulfate, and the nitrogen-containing compound is urea or ammonium chloride.
According to the invention, the accelerator is one or more of 1, 2-bis (dimethylamino) ethane, triethylene diamine, ferric trichloride, tetramethylthiourea, vanadium acetylacetonate, acetylacetone, N-dimethyl-p-toluidine, triethylamine, tetrahydroquinoline, 8-hydroxyquinoline and ferrocene; further preferred is a combination of triethylenediamine and N, N-dimethyl-p-toluidine.
According to the present invention, the brine solution is preferably an aqueous sodium chloride solution and/or an aqueous potassium chloride solution, and more preferably an aqueous sodium chloride solution; the concentration of the aqueous salt solution is 0.5 to 5mol/L, and more preferably 2 to 3mol/L.
According to the invention, the preparation method of the supermolecular gel plugging agent for the fractured stratum comprises the following steps:
(1) Adding hydrophilic monomers in the copolymerization monomers into water, and uniformly stirring to obtain a mixed solution A;
(2) Adding a hydrophobic monomer in the copolymerization monomer into the mixed solution A, and uniformly stirring to obtain a mixed solution B;
(3) Adding functional group molecules and a surfactant into the mixed solution B, and uniformly stirring to obtain a mixed solution C;
(4) Adding an initiator and a cosolvent into the mixed solution C, and stirring until the initiator and the cosolvent are completely dissolved to prepare a mixed solution D;
(5) Adding an accelerator and a saline solution into the mixed solution D, and uniformly stirring to obtain a mixed solution E;
(6) Deoxidizing and degassing the mixed solution E, and standing for reaction to obtain supermolecule gel; and drying and crushing the supermolecular gel to obtain the supermolecular gel plugging agent for the fractured stratum.
According to the invention, in the step (1), the stirring temperature is preferably 20-45 ℃, and more preferably 25-30 ℃; the stirring speed is 300 to 1000 rpm, more preferably 400 to 600 rpm; the stirring time is 10 to 40 minutes, more preferably 20 to 30 minutes.
Preferably according to the invention, in step (2), the stirring temperature is 20-50 ℃, further preferably 23-28 ℃; the stirring speed is 200 to 800 rpm, more preferably 450 to 580 rpm; the stirring time is 5 to 30 minutes, more preferably 24 to 28 minutes.
Preferably according to the invention, in step (3), the stirring temperature is 30-50 ℃, further preferably 35-40 ℃; the stirring speed is 400 to 1000 rpm, more preferably 500 to 700 rpm; the stirring time is 30 to 60 minutes, more preferably 40 to 50 minutes.
According to the invention, in the step (4), the stirring temperature is preferably 30-70 ℃, and more preferably 40-50 ℃; the stirring speed is 400 to 800 rpm, more preferably 500 to 600 rpm; the stirring time is 20 to 40 minutes, more preferably 25 to 35 minutes.
Preferably according to the invention, in step (5), the stirring temperature is 30-70 ℃, further preferably 40-60 ℃; the stirring speed is 400 to 800 rpm, more preferably 450 to 550 rpm; the stirring time is 20 to 40 minutes, more preferably 25 to 30 minutes.
According to the invention, in the step (6), the deoxidization and the deaeration are carried out by introducing nitrogen and vacuum pumping; the temperature of the standing reaction is 50-80 ℃, and more preferably 60-65 ℃; the time for the standing reaction is 5 to 9 hours, more preferably 6 to 7 hours.
According to the invention, the drying in step (6) is preferably performed under vacuum at 55-80 ℃ for 20-30 hours, more preferably at 70-75 ℃ for 24-26 hours. The crushing is to crush the supermolecular gel into particles with different particle diameters by a crusher according to different requirements.
According to the invention, the supermolecular gel plugging agent for the fractured stratum is applied to the plugging of the fractured stratum.
According to the invention, the supermolecular gel plugging agent for the fractured stratum is used as a plugging material for plugging drilling fluid, the addition amount of the supermolecular gel plugging agent is 2% -5% of the mass of the drilling fluid, and the supermolecular gel plugging agent can be injected in a mode of injection while drilling.
The preparation principle of the invention is as follows:
the invention adopts a free radical polymerization method to form the supramolecular gel applicable to the fractured stratum and based on non-covalent bond interaction through self-assembly among the copolymerization reaction monomers. The main raw materials of the copolymerization monomer are hydrophilic monomers, hydrophobic monomers and functional group molecules. The hydrophilic monomer and the hydrophobic monomer can generate hydrophobic association under the action of the surfactant to form a hydrophobic association polymer, and the molecular chain of the hydrophobic association polymer is provided with a small amount of hydrophobic groups, so that a super-molecular structure with a three-dimensional network can be formed in the solution, and the polymer has better temperature resistance, salt resistance and dilution resistance under the conditions of lower concentration and lower molecular weight. Through supermolecular structure design, multiple hydrogen bond structural units formed in the polymerization process of the comonomer are introduced into the hydrophobic chain of the hydrophobic association polymer, and zwitterionic groups are introduced into the hydrophilic end of the hydrophobic association polymer, so that the supermolecular gel with unique dynamic reversible characteristics and self-repairing capability is formed, and the mechanical strength of the supermolecular gel can be effectively improved. Meanwhile, the mechanical property and the environment response capability of the gel can be improved by intertwining functional group molecules, and the supermolecule gel formed based on the host-guest effect can keep good uniformity and environment response within a certain scale range.
The invention has the technical characteristics and beneficial effects that:
1. the supramolecular gel for the fractured stratum is used as a plugging material for plugging drilling fluid, granular gel is injected into a leakage layer while drilling, charged particles in gel particles are adsorbed on the surface of rock under the action of static electricity to plug micro-fracture pores or a hypertonic layer, and high-strength supramolecular gel is formed through the actions of extrusion deformation, water absorption expansion, filling accumulation and the like, so that the bearing capacity of the stratum can be effectively improved, and intelligent plugging is realized.
2. The supermolecular gel for the fractured stratum has excellent mechanical property and environmental response capability, ionic groups on the surface of gel particles can be adsorbed on the surface of stratum rock through hydrogen bond and electrostatic action, chain-shaped blocking layers are formed by mutual connection through aggregation, extrusion, filling and other actions, and ionic bonds are formed through mutual contact among gel particles, so that the supermolecular gel with self-repairing capability is constructed, and the fractured pores can be effectively blocked.
3. The supermolecular gel for the fractured stratum forms a three-dimensional network structure under the hydrophobic association effect, can be automatically adapted to severe and complex fractured stratum with high temperature, high salt and the like, has good compatibility and strong scouring resistance, and can form a high-strength plugging layer in the fractured stratum.
4. The supermolecular gel plugging agent suitable for the fractured stratum can effectively solve the defects of the conventional plugging material, has excellent high-temperature resistance and shearing thixotropic property, can be adaptively matched with the fracture with complex scale, realizes full filling of a leakage space, achieves long-term stable plugging, and has the advantages of simple and feasible preparation method, convenient production operation and small environmental pollution.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other examples of modifications and alterations will be apparent to those skilled in the art based on the examples herein, and are intended to be within the scope of the invention.
The raw materials used in the examples are all conventional raw materials and are commercially available; the methods are prior art unless specified otherwise.
The polyethylene glycol used in the examples is polyethylene glycol 1500;
the molecular weight of the poly (hydroxyethyl methacrylate) is 650.7, which is sold by Shandong Hongkai chemical Co., ltd;
scleroglucan Hebei Xin He Biochemical Co., ltd.
Example 1
The supermolecular gel plugging agent for the fractured stratum comprises the following raw materials in percentage by mass: the comonomer content was 30%; the content of the surfactant is 3.5%; the initiator content is 0.5%; the cosolvent content is 0.8%; the content of the accelerator is 0.25%; the content of the saline solution is 1.5 percent, the balance is water, and the sum of the contents of all the components is hundred percent.
The copolymerization monomer is a combination of a hydrophilic monomer, a hydrophobic monomer and a functional group molecule, wherein the mass ratio of the hydrophilic monomer to the hydrophobic monomer to the functional group molecule is 7:2:1; the hydrophilic monomer is a combination of acrylamide, 2-acrylamido-2-methylpropanesulfonic acid and N-vinyl pyrrolidone, and the mass ratio of the acrylamide to the 2-acrylamido-2-methylpropanesulfonic acid to the N-vinyl pyrrolidone is 5:3:2; the hydrophobic monomer is a combination of octadecyl methacrylate and lauryl methacrylate, and the mass ratio of the octadecyl methacrylate to the lauryl methacrylate is 7:3; the functional group molecules are the combination of scleroglucan, chitosan and beta-cyclodextrin, and the mass ratio of the scleroglucan to the chitosan to the beta-cyclodextrin is 6:3:1.
The surfactant is selected from the combination of sodium dodecyl benzene sulfonate and sodium dodecyl sulfate, and the mass ratio of the sodium dodecyl benzene sulfonate to the sodium dodecyl sulfate is 2:3.
The initiator is selected from the combination of azo-diiso Ding Mi hydrochloride and potassium persulfate, and the mass ratio of the azo-diiso Ding Mi hydrochloride to the potassium persulfate is 2:3.
The cosolvent is a combination of anhydrous sodium sulfate and ammonium chloride, and the mass ratio is 1:1.
The accelerator is selected from the combination of triethylene diamine and N, N-dimethyl-p-toluidine, and the mass ratio of the triethylene diamine to the N, N-dimethyl-p-toluidine is 3:2.
The salt water solution is sodium chloride solution with the concentration of 2.5 mol/L.
The preparation method of the supermolecular gel plugging agent for the fractured stratum comprises the following steps:
(1) Adding hydrophilic monomers in the copolymerization monomers into water, and stirring at a stirring speed of 500 revolutions per minute at 25 ℃ for 25 minutes to obtain a mixed solution A;
(2) Adding a hydrophobic monomer in the copolymerization reaction monomer into the mixed solution A, and stirring at a stirring speed of 500 revolutions per minute for 28 minutes at 25 ℃ to obtain a mixed solution B;
(3) Adding functional group molecules and a surfactant into the mixed solution B, and stirring for 45 minutes at a stirring temperature of 40 ℃ and a stirring speed of 550 r/min to obtain a mixed solution C;
(4) Adding an initiator and a cosolvent into the mixed solution C, stirring for 30 minutes at the stirring temperature of 45 ℃ and the stirring speed of 550 r/min, and stirring until the initiator and the cosolvent are completely dissolved to prepare a mixed solution D;
(5) Adding an accelerator and a saline solution into the mixed solution D, and stirring at a stirring speed of 500 revolutions per minute for 30 minutes at 50 ℃ to obtain a mixed solution E;
(6) Placing the mixed solution E in a three-neck flask, introducing nitrogen, decompressing and vacuumizing, and standing for 6 hours at the temperature of 60 ℃ until free radicals are fully polymerized to obtain supermolecule gel; the supramolecular gel was dried in vacuo at 70 ℃ for 24 hours and then crushed to obtain the supramolecular gel plugging agent for fractured strata, designated as sample S1.
Example 2
The supermolecular gel plugging agent for the fractured stratum comprises the following raw materials in percentage by mass: the comonomer content was 28%; the surfactant content was 4.3%; the initiator content is 0.5%; the cosolvent content is 0.7%; the content of the accelerator is 0.20%; the content of the saline solution is 2.0 percent, the balance is water, and the sum of the contents of all the components is hundred percent.
The copolymerization monomer is a combination of a hydrophilic monomer, a hydrophobic monomer and a functional group molecule, wherein the mass ratio of the hydrophilic monomer to the hydrophobic monomer to the functional group molecule is 7:2:1; the hydrophilic monomer is a combination of acrylic acid, 2-acrylamido-2-methylpropanesulfonic acid and hexadecyl dimethyl allyl ammonium chloride, and the mass ratio of the acrylic acid to the 2-acrylamido-2-methylpropanesulfonic acid to the hexadecyl dimethyl allyl ammonium chloride is 5:3:2; the hydrophobic monomer is a combination of octadecyl methacrylate and hexadecyl methacrylate, and the mass ratio of the octadecyl methacrylate to the hexadecyl methacrylate is 7:3; the functional group molecules are the combination of scleroglucan, chitosan and cucurbituril, and the mass ratio of the scleroglucan, the chitosan and the cucurbituril is 6:3:1.
The surfactant is a combination of betaine and sodium dodecyl sulfate, and the mass ratio of the betaine to the sodium dodecyl sulfate is 3:2.
The initiator is selected from the combination of ammonium persulfate and potassium persulfate, and the mass ratio of the ammonium persulfate to the potassium persulfate is 3:2.
The cosolvent is a combination of anhydrous sodium sulfate and ammonium chloride, and the mass ratio of the anhydrous sodium sulfate to the ammonium chloride is 2:1.
The accelerator is a combination of triethylene diamine and N, N-dimethyl-p-toluidine, and the mass ratio is 1:1.
The salt water solution is sodium chloride solution with the concentration of 2.5 mol/L.
The preparation method of the supramolecular gel plugging agent for the fractured stratum is as described in the embodiment 1, and the prepared supramolecular gel plugging agent is marked as a sample S2.
Example 3
The supermolecular gel plugging agent for the fractured stratum comprises the following raw materials in percentage by mass: the comonomer content was 26%; the content of the surfactant is 5%; the initiator content is 0.5%; the cosolvent content is 0.8%; the content of the accelerator is 0.30%; the content of the saline solution is 2.0 percent, the balance is water, and the sum of the contents of all the components is hundred percent.
The copolymerization monomer is a combination of a hydrophilic monomer, a hydrophobic monomer and a functional group molecule, wherein the mass ratio of the hydrophilic monomer to the hydrophobic monomer to the functional group molecule is 7:2:1; the hydrophilic monomer is a combination of polyethylene glycol, 2-acrylamido-2-methylpropanesulfonic acid and 2-vinylpyridine, and the mass ratio of the polyethylene glycol to the 2-acrylamido-2-methylpropanesulfonic acid to the 2-vinylpyridine is 5:3:2; the hydrophobic monomer is a combination of octadecyl methacrylate and butyl methacrylate, and the mass ratio of the octadecyl methacrylate to the butyl methacrylate is 3:2; the functional group molecules are the combination of scleroglucan, chitosan and sodium alginate, and the mass ratio of the scleroglucan, the chitosan and the sodium alginate is 3:1:1.
The surfactant is selected from the combination of sodium dodecyl sulfate and fatty acid sorbitan, and the mass ratio of the sodium dodecyl sulfate to the fatty acid sorbitan is 4:1.
The initiator is selected from the combination of ammonium persulfate and potassium persulfate, and the mass ratio of the ammonium persulfate to the potassium persulfate is 2:3.
The cosolvent is a combination of anhydrous calcium sulfate and urea, and the mass ratio of the anhydrous calcium sulfate to the urea is 2:1.
The accelerator is a combination of triethylene diamine and tetramethylthiourea, and the mass ratio is 1:1.
The salt water solution is sodium chloride solution with the concentration of 2.5 mol/L.
The preparation method of the supramolecular gel plugging agent for the fractured stratum is as described in the embodiment 1, and the prepared supramolecular gel plugging agent is marked as a sample S3.
Example 4
The supermolecular gel plugging agent for the fractured stratum comprises the following raw materials in percentage by mass: the comonomer content was 26%; the content of the surfactant is 4.5%; the initiator content was 0.6%; the cosolvent content is 0.9%; the content of the accelerator is 0.40%; the content of the saline solution is 2.0 percent, the balance is water, and the sum of the contents of all the components is hundred percent.
The copolymerization monomer is a combination of a hydrophilic monomer, a hydrophobic monomer and a functional group molecule, wherein the mass ratio of the hydrophilic monomer to the hydrophobic monomer to the functional group molecule is 7:2:1; the hydrophilic monomer is the combination of methacrylic acid, sodium acrylate and N-isopropyl acrylamide, and the mass ratio of the methacrylic acid to the sodium acrylate to the N-isopropyl acrylamide is 4:3:3; the hydrophobic monomer is a combination of cetyl methacrylate and polyhydroxyethyl methacrylate, and the mass ratio of the cetyl methacrylate to the polyhydroxyethyl methacrylate is 4:1; the functional group molecules are the combination of sodium alginate, beta-cyclodextrin and calix [6] arene, and the mass ratio of the sodium alginate to the beta-cyclodextrin to the calix [6] arene is 1:4:1.
The surfactant is selected from the combination of sodium dodecyl sulfate and stearic acid, and the mass ratio of the sodium dodecyl sulfate to the stearic acid is 3:2.
The initiator is selected from the combination of potassium persulfate and dimethyl azodiisobutyrate, and the mass ratio of the potassium persulfate to the dimethyl azodiisobutyrate is 4:1.
The cosolvent is a combination of anhydrous calcium sulfate and ammonium chloride, and the mass ratio of the anhydrous calcium sulfate to the ammonium chloride is 2:1.
The accelerator is a combination of triethylamine and 8-hydroxyquinoline, and the mass ratio is 1:1.
The salt water solution is sodium chloride solution with the concentration of 2.5 mol/L.
The preparation method of the supramolecular gel plugging agent for the fractured stratum is as described in the embodiment 1, and the prepared supramolecular gel plugging agent is marked as a sample S4.
Example 5
The supermolecular gel plugging agent for the fractured stratum comprises the following raw materials in percentage by mass:
the comonomer content was 24%; the content of the surfactant is 5%; the initiator content is 0.5%; the cosolvent content is 0.8%; the content of the accelerator is 0.50%; the content of the saline solution is 2.0 percent, the balance is water, and the sum of the contents of all the components is hundred percent.
The copolymerization monomer is a combination of a hydrophilic monomer, a hydrophobic monomer and a functional group molecule, wherein the mass ratio of the hydrophilic monomer to the hydrophobic monomer to the functional group molecule is 7:2:1; the hydrophilic monomer is a combination of acrylamide, polyethylene glycol and methacrylic acid, and the mass ratio of the acrylamide to the polyethylene glycol to the methacrylic acid is 5:3:2; the hydrophobic monomer is a combination of dimethylaminoethyl methacrylate and 4-methylstyrene, and the mass ratio of the dimethylaminoethyl methacrylate to the 4-methylstyrene is 3:2; the functional group molecules are the combination of scleroglucan, sodium alginate and calix [6] arene, and the mass ratio of the scleroglucan, the sodium alginate and the calix [6] arene is 1:4:1.
The surfactant is selected from the combination of sodium dodecyl sulfate and stearic acid, and the mass ratio of the sodium dodecyl sulfate to the stearic acid is 3:2.
The initiator is selected from the combination of cumene hydroperoxide and azobisisobutylate, and the mass ratio of the cumene hydroperoxide to the azobisisobutylate is 1:4.
The cosolvent is a combination of anhydrous sodium sulfate and urea, and the mass ratio of the anhydrous sodium sulfate to the urea is 3:2.
The accelerator is selected from the combination of 1, 2-bis (dimethylamino) ethane and ferrocene, and the mass ratio of the 1, 2-bis (dimethylamino) ethane to the ferrocene is 4:1.
The salt water solution is sodium chloride solution with the concentration of 2.5 mol/L.
The preparation method of the supramolecular gel plugging agent for the fractured stratum is as described in the embodiment 1, and the prepared supramolecular gel plugging agent is marked as a sample S5.
Example 6
The supermolecular gel plugging agent for the fractured stratum comprises the following raw materials in percentage by mass: the comonomer content was 28%; the surfactant content was 4.3%; the initiator content is 0.5%; the cosolvent content is 0.7%; the content of the accelerator is 0.20%; the content of the saline solution is 2.0 percent, the balance is water, and the sum of the contents of all the components is hundred percent.
The copolymerization monomer is a combination of a hydrophilic monomer, a hydrophobic monomer and a functional group molecule, wherein the mass ratio of the hydrophilic monomer to the hydrophobic monomer to the functional group molecule is 7:2:1; the hydrophilic monomer is the combination of acrylamide, 2-acrylamido-2-methylpropanesulfonic acid and hexadecyl dimethyl allyl ammonium chloride, and the mass ratio of the acrylamide to the 2-acrylamido-2-methylpropanesulfonic acid to the hexadecyl dimethyl allyl ammonium chloride is 5:3:2; the hydrophobic monomer is a combination of octadecyl methacrylate and hexadecyl methacrylate, and the mass ratio of the octadecyl methacrylate to the hexadecyl methacrylate is 7:3; the functional group molecules are the combination of chitosan, sodium alginate and beta-cyclodextrin, and the mass ratio of the chitosan to the sodium alginate to the beta-cyclodextrin is 4:3:3.
The surfactant is a combination of betaine and sodium dodecyl sulfate, and the mass ratio of the betaine to the sodium dodecyl sulfate is 4:1.
The initiator is selected from the combination of ammonium persulfate and potassium persulfate, and the mass ratio of the ammonium persulfate to the potassium persulfate is 3:2.
The cosolvent is a combination of anhydrous sodium sulfate and ammonium chloride, and the mass ratio of the anhydrous sodium sulfate to the ammonium chloride is 3:2.
The accelerator is selected from the combination of triethylene diamine and N, N-dimethyl-p-toluidine, and the mass ratio of the triethylene diamine to the N, N-dimethyl-p-toluidine is 2:1.
The salt water solution is sodium chloride solution with the concentration of 2.5 mol/L.
The preparation method of the supramolecular gel plugging agent for the fractured stratum is as described in the embodiment 1, and the prepared supramolecular gel plugging agent is marked as a sample S6.
Example 7
The supermolecular gel plugging agent for the fractured stratum comprises the following raw materials in percentage by mass: the comonomer content was 28%; the surfactant content was 4.3%; the initiator content is 0.5%; the cosolvent content is 0.7%; the content of the accelerator is 0.20%; the content of the saline solution is 2.0 percent, the balance is water, and the sum of the contents of all the components is hundred percent.
The copolymerization monomer is a combination of a hydrophilic monomer, a hydrophobic monomer and a functional group molecule, wherein the mass ratio of the hydrophilic monomer to the hydrophobic monomer to the functional group molecule is 7:2:1; the hydrophilic monomer is the combination of acrylamide, 2-acrylamido-2-methylpropanesulfonic acid and hexadecyl dimethyl allyl ammonium chloride, and the mass ratio of the acrylamide to the 2-acrylamido-2-methylpropanesulfonic acid to the hexadecyl dimethyl allyl ammonium chloride is 5:3:2; the hydrophobic monomer is a combination of octadecyl methacrylate and hexadecyl methacrylate, and the mass ratio of the octadecyl methacrylate to the hexadecyl methacrylate is 7:3; the functional group molecule is the combination of beta-cyclodextrin, calix [6] arene and cucurbituril, and the mass ratio of the beta-cyclodextrin, the calix [6] arene and the cucurbituril is 5:3:2.
The surfactant is a combination of betaine and sodium dodecyl sulfate, and the mass ratio of the betaine to the sodium dodecyl sulfate is 4:3.
The initiator is selected from the combination of ammonium persulfate and potassium persulfate, and the mass ratio of the ammonium persulfate to the potassium persulfate is 3:2.
The cosolvent is a combination of anhydrous sodium sulfate and ammonium chloride, and the mass ratio of the anhydrous sodium sulfate to the ammonium chloride is 3:2.
The accelerator is selected from the combination of triethylene diamine and N, N-dimethyl-p-toluidine, and the mass ratio of the triethylene diamine to the N, N-dimethyl-p-toluidine is 2:1.
The salt water solution is sodium chloride solution with the concentration of 2.5 mol/L.
The preparation method of the supramolecular gel plugging agent for the fractured stratum is as described in the embodiment 1, and the prepared supramolecular gel plugging agent is marked as a sample S7.
Example 8
The supermolecular gel plugging agent for the fractured stratum comprises the following raw materials in percentage by mass: the comonomer content was 28%; the surfactant content was 4.3%; the initiator content is 0.5%; the cosolvent content is 0.7%; the content of the accelerator is 0.20%; the content of the saline solution is 2.0 percent, the balance is water, and the sum of the contents of all the components is hundred percent.
The copolymerization monomer is a combination of a hydrophilic monomer, a hydrophobic monomer and a functional group molecule, wherein the mass ratio of the hydrophilic monomer to the hydrophobic monomer to the functional group molecule is 7:2:1; the hydrophilic monomer is the combination of acrylamide, 2-acrylamido-2-methylpropanesulfonic acid and hexadecyl dimethyl allyl ammonium chloride, and the mass ratio of the acrylamide to the 2-acrylamido-2-methylpropanesulfonic acid to the hexadecyl dimethyl allyl ammonium chloride is 5:3:2; the hydrophobic monomer is a combination of octadecyl methacrylate and hexadecyl methacrylate, and the mass ratio of the octadecyl methacrylate to the hexadecyl methacrylate is 7:3; the functional group molecule is the combination of chitosan, calix [6] arene and cucurbituril, and the mass ratio of beta-cyclodextrin, calix [6] arene and cucurbituril is 6:3:1.
The surfactant is a combination of betaine and sodium dodecyl sulfate, and the mass ratio of the betaine to the sodium dodecyl sulfate is 4:3.
The initiator is selected from the combination of ammonium persulfate and potassium persulfate, and the mass ratio of the ammonium persulfate to the potassium persulfate is 3:2.
The cosolvent is a combination of anhydrous sodium sulfate and ammonium chloride, and the mass ratio of the anhydrous sodium sulfate to the ammonium chloride is 3:2.
The accelerator is selected from the combination of triethylene diamine and N, N-dimethyl-p-toluidine, and the mass ratio of the triethylene diamine to the N, N-dimethyl-p-toluidine is 2:1.
The salt water solution is sodium chloride solution with the concentration of 2.5 mol/L.
The preparation method of the supramolecular gel plugging agent for the fractured stratum is as described in the embodiment 1, and the prepared supramolecular gel plugging agent is marked as a sample S8.
Example 9
The supermolecular gel plugging agent for the fractured stratum comprises the following raw materials in percentage by mass: the comonomer content was 28%; the surfactant content was 4.3%; the initiator content is 0.5%; the cosolvent content is 0.7%; the content of the accelerator is 0.20%; the content of the saline solution is 2.0 percent, the balance is water, and the sum of the contents of all the components is hundred percent.
The copolymerization monomer is a combination of a hydrophilic monomer, a hydrophobic monomer and a functional group molecule, wherein the mass ratio of the hydrophilic monomer to the hydrophobic monomer to the functional group molecule is 7:2:1; the hydrophilic monomer is the combination of acrylamide, 2-acrylamido-2-methylpropanesulfonic acid and hexadecyl dimethyl allyl ammonium chloride, and the mass ratio of the acrylamide to the 2-acrylamido-2-methylpropanesulfonic acid to the hexadecyl dimethyl allyl ammonium chloride is 5:3:2; the hydrophobic monomer is a combination of octadecyl methacrylate and hexadecyl methacrylate, and the mass ratio of the octadecyl methacrylate to the hexadecyl methacrylate is 7:3; the functional group molecules are the combination of sodium alginate, calix [6] arene and cucurbituril, and the mass ratio of the sodium alginate to the calix [6] arene to the cucurbituril is 2:3:5.
The surfactant is a combination of betaine and sodium dodecyl sulfate, and the mass ratio of the betaine to the sodium dodecyl sulfate is 4:3.
The initiator is selected from the combination of ammonium persulfate and potassium persulfate, and the mass ratio of the ammonium persulfate to the potassium persulfate is 3:2.
The cosolvent is a combination of anhydrous sodium sulfate and ammonium chloride, and the mass ratio of the anhydrous sodium sulfate to the ammonium chloride is 3:2.
The accelerator is selected from the combination of triethylene diamine and N, N-dimethyl-p-toluidine, and the mass ratio of the triethylene diamine to the N, N-dimethyl-p-toluidine is 2:1.
The salt water solution is sodium chloride solution with the concentration of 2.5 mol/L.
The preparation method of the supramolecular gel plugging agent for the fractured stratum is as described in the embodiment 1, and the prepared supramolecular gel plugging agent is marked as a sample S9.
Example 10
The supermolecular gel plugging agent for the fractured stratum comprises the following raw materials in percentage by mass: the comonomer content was 28%; the surfactant content was 4.3%; the initiator content is 0.5%; the cosolvent content is 0.7%; the content of the accelerator is 0.20%; the content of the saline solution is 2.0 percent, the balance is water, and the sum of the contents of all the components is hundred percent.
The copolymerization monomer is a combination of a hydrophilic monomer, a hydrophobic monomer and a functional group molecule, wherein the mass ratio of the hydrophilic monomer to the hydrophobic monomer to the functional group molecule is 7:2:1; the hydrophilic monomer is the combination of acrylamide, 2-acrylamido-2-methylpropanesulfonic acid and hexadecyl dimethyl allyl ammonium chloride, and the mass ratio of the acrylamide to the 2-acrylamido-2-methylpropanesulfonic acid to the hexadecyl dimethyl allyl ammonium chloride is 5:3:2; the hydrophobic monomer is a combination of octadecyl methacrylate and hexadecyl methacrylate, and the mass ratio of the octadecyl methacrylate to the hexadecyl methacrylate is 7:3; the functional group molecule is the combination of chitosan, beta-cyclodextrin and calix [6] arene, and the mass ratio of the chitosan, the beta-cyclodextrin and the calix [6] arene is 7:2:1.
The surfactant is a combination of betaine and sodium dodecyl sulfate, and the mass ratio of the betaine to the sodium dodecyl sulfate is 4:3.
The initiator is selected from the combination of ammonium persulfate and potassium persulfate, and the mass ratio of the ammonium persulfate to the potassium persulfate is 3:2.
The cosolvent is a combination of anhydrous sodium sulfate and ammonium chloride, and the mass ratio of the anhydrous sodium sulfate to the ammonium chloride is 3:2.
The accelerator is selected from the combination of triethylene diamine and N, N-dimethyl-p-toluidine, and the mass ratio of the triethylene diamine to the N, N-dimethyl-p-toluidine is 2:1.
The salt water solution is sodium chloride solution with the concentration of 2.5 mol/L.
The preparation method of the supramolecular gel plugging agent for the fractured stratum is as described in the embodiment 1, and the prepared supramolecular gel plugging agent is marked as a sample S10.
Comparative example 1
A supramolecular gel plugging agent for fractured formations, the composition of the materials being as described in example 1, except that: no functional group molecules are added.
The specific raw materials comprise the following components: the content of the comonomer is 30 percent (the mass ratio of the hydrophilic monomer to the hydrophobic monomer is 7:2); the content of the surfactant is 3.5%; the initiator content is 0.5%; the cosolvent content is 0.8%; the content of the accelerator is 0.25%; the content of the saline solution is 1.5 percent, the balance is water, and the sum of the contents of all the components is hundred percent; the types of the above components are as described in example 1.
The preparation method of the supermolecular gel plugging agent is as described in example 1, and the obtained product is designated as D1.
Comparative example 2
A supramolecular gel plugging agent for fractured formations, the composition of the materials being as described in example 1, except that: no surfactant was added.
The specific raw materials comprise the following components: the comonomer content was 30%; the initiator content is 0.5%; the cosolvent content is 0.8%; the content of the accelerator is 0.25%; the content of the saline solution is 1.5 percent, the balance is water, and the sum of the contents of all the components is hundred percent; the types of the above components are as described in example 1.
The preparation method of the supermolecular gel plugging agent is as described in example 1, and the obtained product is designated as D2.
Comparative example 3
A supramolecular gel plugging agent for fractured formations, the composition of the materials being as described in example 1, except that: no initiator was added.
The specific raw materials comprise the following components: the comonomer content was 30%; the content of the surfactant is 3.5%; the cosolvent content is 0.8%; the content of the accelerator is 0.25%; the content of the saline solution is 1.5 percent, the balance is water, and the sum of the contents of all the components is hundred percent; the types of the above components are as described in example 1.
The preparation method of the supermolecular gel plugging agent is as described in example 1, and the obtained product is designated as D3.
Comparative example 4
A supramolecular gel plugging agent for fractured formations, the composition of the materials being as described in example 1, except that: no co-solvent was added.
The specific raw materials comprise the following components: the comonomer content was 30%; the content of the surfactant is 3.5%; the initiator content is 0.5%; the content of the accelerator is 0.25%; the content of the saline solution is 1.5 percent, the balance is water, and the sum of the contents of all the components is hundred percent; the types of the above components are as described in example 1.
The preparation method of the supermolecular gel plugging agent is as described in example 1, and the obtained product is designated as D4.
Comparative example 5
A supramolecular gel plugging agent for fractured formations, the composition of the materials being as described in example 1, except that: no accelerator was added.
The specific raw materials comprise the following components: the comonomer content was 30%; the content of the surfactant is 3.5%; the initiator content is 0.5%; the cosolvent content is 0.8%; the content of the saline solution is 1.5 percent, the balance is water, and the sum of the contents of all the components is hundred percent; the types of the above components are as described in example 1.
The preparation method of the supermolecular gel plugging agent is as described in example 1, and the obtained product is designated as D5.
Comparative example 6
A supramolecular gel plugging agent for fractured formations, the composition of the materials being as described in example 1, except that: the comonomer content was 15%.
The specific raw materials comprise the following components: the comonomer content was 15%; the initiator content is 0.5%; the cosolvent content is 0.8%; the content of the accelerator is 0.25%; the content of the saline solution is 1.5 percent, the balance is water, and the sum of the contents of all the components is hundred percent; the types of the above components are as described in example 1.
The preparation method of the supermolecular gel plugging agent is as described in example 1, and the obtained product is designated as D6.
Comparative example 7
A supramolecular gel plugging agent for fractured formations, the composition of the materials being as described in example 1, except that: the content of the comonomer is 10%; the types of the above components are as described in example 1.
The specific raw materials comprise the following components: the content of the comonomer is 10%; the initiator content is 0.5%; the cosolvent content is 0.8%; the content of the accelerator is 0.25%; the content of the saline solution is 1.5 percent, the balance is water, and the sum of the contents of all the components is hundred percent.
The preparation method of the supermolecular gel plugging agent is as described in example 1, and the obtained product is designated as D7.
Comparative example 8
A supramolecular gel plugging agent for fractured formations, the composition of the materials being as described in example 1, except that: the mass ratio of the hydrophilic monomer to the hydrophobic monomer to the functional group molecule is 5:1:1.
The preparation method of the supermolecular gel plugging agent is as described in example 1, and the obtained product is designated as D8.
Comparative example 9
A supramolecular gel plugging agent for fractured formations, the composition of the materials being as described in example 1, except that: the mass ratio of the hydrophilic monomer to the hydrophobic monomer to the functional group molecule is 9:1:1.
The preparation method of the supermolecular gel plugging agent is as described in example 1, and the obtained product is designated as D9.
Test examples
The supermolecule gel plugging agent prepared in the examples and the comparative examples is subjected to rheological property, compression resistance and high-temperature high-pressure plugging property test.
Test 1. Rheological Property test of supramolecular gel plugging agent
The rheological property of the supermolecular gel was tested by using a HAAKE MARS model 60 rheometer, the model of the conical rotor is C35-1 DEG/Ti (the cone angle of the rotor is 1 DEG and the diameter is 35 mm), and the gap between the rotor and a sample stage is 0.053mm during the test. In the experiment, the supermolecule gel plugging agent is cut into round sample slices with the diameter of 30mm and the thickness of 10mm by using a vernier caliper, wherein the test conditions of the storage modulus (G ') and the loss modulus (G') are 1.0% constant strain, the oscillation scanning frequency is set to be 1Hz, and the angular frequency range is set to be 0.01-100 rad.s -1 . The temperature of the test sample is balanced for at least 30 minutes, the temperature error is controlled to be +/-0.1 ℃, and a solvent catcher is adopted to reduce the evaporation of water in the experimental process.
The rheological evaluation criteria of the supermolecular gel plugging agent are shown in table 1. Wherein, the ratio of the storage modulus to the loss modulus is defined as beta, which represents the elastic strength; defining the ratio of the loss modulus to the storage modulus as delta, and representing the adhesive strength; the rheological property results of the supramolecular gel plugging agents prepared in the above examples and comparative examples are shown in table 2.
Test 2. Test of compression resistance of supramolecular gel plugging agent
Preparing the supermolecule gel plugging agent into a cylinder with the bottom surface diameter of 20mm and the height of 10mm, adopting an electronic universal testing machine to carry out gel compression mechanical property test, setting the compression speed to be 3mm/min, and recording the stress-strain value of the supermolecule gel plugging agent sample when the supermolecule gel plugging agent sample is compressed. The compression ratio ω refers to the ratio of the compressed height of the gel to the original height of the gel prior to compression; the compressive stress τ is a value obtained by dividing the compressive load applied to the sample by the original cross-sectional area of the sample during the compression test, and can be directly measured.
The compression resistance evaluation criteria of the supermolecule gel plugging agent are shown in table 3; the compression resistance results of the supramolecular gel plugging agents prepared in the above examples and comparative examples are shown in table 4.
Test 3. High temperature and high pressure leakage blocking Performance test of supermolecule gel leakage blocking agent
And (3) researching the pressure-bearing plugging performance of the supermolecule gel plugging agent on the cracks by using a high-temperature high-pressure crack physical simulation device. The simulated fracture core is made of steel, the appearance is columnar, the fracture penetrates through the longitudinal section of the steel column, the length of the fracture is 30cm, the height of the fracture is 3cm, and the widths of the fracture are 3, 5, 7 and 9mm respectively.
The high-temperature high-pressure plugging test steps are as follows: (a) The temperature of the heating box is adjusted to 160 ℃ of the simulated stratum according to the requirement; (b) Placing a steel crack core with the required seam width into a core holder, and adding confining pressure to 16MPa; (c) Injecting simulated drilling fluid into the fracture core at an injection rate of 5.0mL/min until the simulated drilling fluid is saturated; (d) Injecting the supermolecule gel solution (namely the mixed solution E) into the fracture core at the injection rate of 5.0mL/min until the fracture outlet completely produces the gel solution; (e) Sealing the crack core model, and standing for 2 hours until the supermolecule gel solution is reacted; (f) And reversely injecting simulated drilling fluid into the fracture core at the injection rate of 5.0mL/min, recording the injection pressure change in real time by using data software, and obtaining the highest pressure when the drilling fluid leaks from the outlet end of the fracture model, namely the pressure-bearing plugging strength of the supramolecular gel plugging agent to the fracture.
The high-temperature high-pressure plugging performance results of the supramolecular gel plugging agent prepared in each of the above examples and comparative examples are shown in table 5.
Test 4. Test of salt resistance and temperature resistance of supramolecular gel plugging agent
The salt resistance testing method of the supermolecule gel plugging agent comprises the following steps: 200000 mg.L -1 Sodium chloride solution with concentration of 10000 mg.L -1 The super-molecular gel plugging agent is prepared by replacing water to simulate the formation water mineralization degree after the concentration of the calcium chloride solution is compounded, and is placed into a high-temperature oven with the temperature of 160 ℃ for observation and recording of gel forming time, and after gel forming, a Hark rheometer is used for testing the storage modulus. The supermolecular gel prepared by the above-described examples 1-2 was subjected to salt resistance test according to the salt resistance test method, and the test results are shown in Table 6.
The temperature resistance testing method of the supermolecule gel plugging agent comprises the following steps: the supermolecular gel sample prepared in example 1 is put into a steel crack rock with a crack width of 3mm, and is respectively put into a constant temperature ageing furnace with a temperature of 150 ℃, 160 ℃, 170 ℃ and 180 ℃ for hot rolling for 72 hours, and then high-temperature high-pressure plugging performance test is carried out to observe the temperature resistance. The results of the temperature resistance of example 1 under different temperature conditions are shown in Table 7.
TABLE 1 supermolecular gel rheology evaluation criteria
TABLE 2 rheological results of supermolecular gel plugging agents prepared in examples and comparative examples
TABLE 3 evaluation criteria for compression resistance of supramolecular gel plugging agents
| Compression ratio omega/% | Compressive stress τ/N | Compressive Strength |
| ω≥90 | τ≥400 | Strong strength |
| 80≤ω＜90 | 300≤τ＜400 | Medium and medium |
| ω＜80 | τ＜300 | Weak and weak |
Table 4 results of compression resistance of the supramolecular gel plugging agent prepared in examples and comparative examples
Table 5 results of high temperature high pressure leakage blocking properties of the supramolecular gels prepared in examples and comparative examples
TABLE 6 results of salt resistance test of supermolecular gel plugging agent
TABLE 7 results of temperature resistance test of supramolecular gel plugging agents at different temperatures
According to the method, the supermolecular gel plugging agent prepared in each embodiment and the comparative embodiment is subjected to different performance evaluation tests, functional group molecules are added into the supermolecular gel raw materials to facilitate the construction of a three-dimensional network structure of the supermolecular gel, hydrophobic association interaction between hydrophilic monomers and hydrophobic monomers is promoted by adding the surfactant, meanwhile, the mutual entanglement strength between the supermolecular gel can be improved by introducing multiple hydrogen bonds, host guest molecules and the like through the design of the supermolecular structure, the pressure-bearing plugging capability and compression resistance of the supermolecular gel plugging agent in stratum with different crack widths can be effectively improved, the pressure-bearing capability is more than 14MPa, the compression ratio is more than 91%, and the compression resistance is strong; the supermolecule gel plugging agent has higher temperature resistance and salt resistance. The storage modulus G' of the supermolecule gel plugging agent prepared by the invention is more than 4000Pa, and can meet better use conditions.
Claims (9)
1. The supermolecular gel plugging agent for the fractured stratum is characterized by comprising the following raw materials in percentage by mass: 18-45% of comonomer, 0.5-6.0% of surfactant, 0.1-2.0% of initiator, 0.1-2.0% of cosolvent, 0.05-0.5% of accelerator, 0.5-5% of saline solution and the balance of water; the copolymerization monomer is a combination of a hydrophilic monomer, a hydrophobic monomer and a functional group molecule; the mass ratio of the hydrophilic monomer to the hydrophobic monomer to the functional group molecules in the copolymerization monomer is 6-8:1-3:1;
the hydrophilic monomer is a combination of more than three of acrylamide, acrylic acid, methacrylic acid, sodium acrylate, polyethylene glycol, N-isopropyl acrylamide, 2-acrylamido-2-methylpropanesulfonic acid, cetyl dimethyl allyl ammonium chloride, N-vinyl pyrrolidone, 2-vinyl pyridine and N-hydroxyethyl acrylamide;
the hydrophobic monomer is a combination of two or more than three of octadecyl methacrylate, methyl methacrylate, butyl methacrylate, hexadecyl methacrylate, polyhydroxyethyl methacrylate, dimethylaminoethyl methacrylate, 2-ethyl methacrylate, beta-hydroxyethyl methacrylate, lauryl methacrylate, 4-trifluoro methyl ethylene carbonate and 4-methyl styrene;
The functional group molecules are the combination of more than three of scleroglucan, chitosan, sodium alginate, beta-cyclodextrin, calix [6] arene and cucurbituril;
the surfactant is one or a combination of more than two of sodium dodecyl benzene sulfonate, sodium dodecyl sulfate, dodecylphenol polyoxyethylene ether, stearic acid, fatty acid sorbitan, betaine and polysorbate;
the cosolvent is sulfate and/or a nitrogen-containing compound, wherein the sulfate is anhydrous sodium sulfate or anhydrous calcium sulfate, and the nitrogen-containing compound is urea or ammonium chloride;
the accelerator is one or more than two of 1, 2-bis (dimethylamino) ethane, triethylene diamine, ferric trichloride, tetramethylthiourea, vanadium acetylacetonate, acetylacetone, N-dimethyl-p-toluidine, triethylamine, tetrahydroquinoline, 8-hydroxyquinoline and ferrocene;
the preparation method of the supermolecular gel plugging agent for the fractured stratum comprises the following steps:
(1) Adding hydrophilic monomers in the copolymerization monomers into water, and uniformly stirring to obtain a mixed solution A;
(2) Adding a hydrophobic monomer in the copolymerization monomer into the mixed solution A, and uniformly stirring to obtain a mixed solution B;
(3) Adding functional group molecules and a surfactant into the mixed solution B, and uniformly stirring to obtain a mixed solution C;
(4) Adding an initiator and a cosolvent into the mixed solution C, and stirring until the initiator and the cosolvent are completely dissolved to prepare a mixed solution D;
(5) Adding an accelerator and a saline solution into the mixed solution D, and uniformly stirring to obtain a mixed solution E;
(6) Deoxidizing and degassing the mixed solution E, and standing for reaction to obtain supermolecule gel; and drying and crushing the supermolecular gel to obtain the supermolecular gel plugging agent for the fractured stratum.
2. The supramolecular gel plugging agent for fractured formations of claim 1, comprising the following raw materials in mass percent: 24-35% of comonomer, 3-5% of surfactant, 0.4-1% of initiator, 0.5-1% of cosolvent, 0.2-0.5% of accelerator, 1-3% of saline solution and the balance of water.
3. The supramolecular gel plugging agent for fractured formations of claim 1, wherein the mass ratio of hydrophilic monomers, hydrophobic monomers to functionalized group molecules in the co-reactive monomers is 7:2:1.
4. The supramolecular gel plugging agent for fractured formations of claim 1, wherein the initiator is one or a combination of two or more of diisopropyl peroxydicarbonate, t-butyl peroxybenzoate, cumene hydroperoxide, potassium persulfate, ammonium persulfate, azobisisobutyrate, dimethyl azobisisobutyrate, azobisiso Ding Mi, hydrochloride.
5. The supramolecular gel plugging agent for fractured formations of claim 1, wherein the co-solvent is a combination of sulfate and nitrogen-containing compounds, wherein the mass ratio of sulfate to nitrogen-containing compounds is 1-2:1;
the accelerator is a combination of triethylene diamine and N, N-dimethyl-p-toluidine;
the saline solution is sodium chloride water solution and/or potassium chloride water solution; the concentration of the saline solution is 0.5-5mol/L.
6. A method of preparing the supramolecular gel plugging agent for fractured formations of any of claims 1-5 comprising the steps of:
(1) Adding hydrophilic monomers in the copolymerization monomers into water, and uniformly stirring to obtain a mixed solution A;
(2) Adding a hydrophobic monomer in the copolymerization monomer into the mixed solution A, and uniformly stirring to obtain a mixed solution B;
(3) Adding functional group molecules and a surfactant into the mixed solution B, and uniformly stirring to obtain a mixed solution C;
(4) Adding an initiator and a cosolvent into the mixed solution C, and stirring until the initiator and the cosolvent are completely dissolved to prepare a mixed solution D;
(5) Adding an accelerator and a saline solution into the mixed solution D, and uniformly stirring to obtain a mixed solution E;
(6) Deoxidizing and degassing the mixed solution E, and standing for reaction to obtain supermolecule gel; and drying and crushing the supermolecular gel to obtain the supermolecular gel plugging agent for the fractured stratum.
7. The method for preparing a supramolecular gel plugging agent for fractured formations according to claim 6, wherein in step (1), the stirring temperature is 20-45 ℃; the stirring speed is 300-1000 rpm; stirring for 10-40 min;
in the step (2), the stirring temperature is 20-50 ℃; the stirring speed is 200-800 rpm; stirring for 5-30 min;
in the step (3), the stirring temperature is 30-50 ℃; stirring speed is 400-1000 rpm; stirring for 30-60 min;
in the step (4), the stirring temperature is 30-70 ℃; stirring at 400-800 rpm; stirring for 20-40 min;
in the step (5), the stirring temperature is 30-70 ℃; stirring at 400-800 rpm; stirring for 20-40 min;
in the step (6), the deoxidization and the deaeration are carried out by introducing nitrogen and vacuum pumping; the temperature of the standing reaction is 50-80 ℃; standing for 5-9 hours; the drying is carried out for 20-30 hours under the condition that the vacuum degree is 0.08-0.1MPa and the temperature is 55-80 ℃.
8. The method for preparing a supramolecular gel plugging agent for fractured formations according to claim 6, wherein in step (1), the stirring temperature is 25-30 ℃; stirring at 400-600 rpm; stirring for 20-30 minutes;
In the step (2), the stirring temperature is 23-28 ℃; the stirring speed is 450-580 r/min; stirring for 24-28 min;
in the step (3), the stirring temperature is 35-40 ℃; the stirring speed is 500-700 rpm; stirring for 40-50 min;
in the step (4), the stirring temperature is 40-50 ℃; the stirring speed is 500-600 rpm; stirring for 25-35 min;
in the step (5), the stirring temperature is 40-60 ℃; the stirring speed is 450-550 rpm; stirring for 25-30 min;
in the step (6), the temperature of the standing reaction is 60-65 ℃; standing for 6-7 hours; the drying is carried out for 24-26 hours under the condition that the vacuum degree is 0.08-0.1MPa and the temperature is 70-75 ℃.
9. Use of the supramolecular gel plugging agent for fractured formations of any of claims 1-5 in fractured formation plugging; the specific application method is as follows: the plugging material is used for plugging drilling fluid, the addition amount of the plugging material is 2% -5% of the mass of the drilling fluid, and the plugging material is injected in a mode of injection while drilling.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
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| CN113698535A (en) * | 2020-05-21 | 2021-11-26 | 江苏百赛飞生物科技有限公司 | Polymer, composition, coating thereof and product |
| CN113943558A (en) * | 2021-10-15 | 2022-01-18 | 中国石油大学(华东) | Self-healing gel leakage preventer with covalent bond-non-covalent bond combined effect while drilling and preparation method and application thereof |
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| FR2926548B1 (en) * | 2008-01-21 | 2010-09-03 | Centre Nat Rech Scient | ENCAPSULATION OF VITAMIN C IN WATER-SOLUBLE DENDRIMERS |
| CN106190087B (en) * | 2016-07-07 | 2019-02-12 | 赵立强 | A kind of temporary stall of thermotropic supermolecular gel is to fracturing fluid |
| CN106381138B (en) * | 2016-09-14 | 2019-04-02 | 中国石油集团渤海钻探工程有限公司 | A kind of high pressure-bearing is without crosslinking supermolecule plural gel sealing agent and preparation method thereof |
| WO2021257505A1 (en) * | 2020-06-15 | 2021-12-23 | Saudi Arabian Oil Company | Method for well treatment, using a reversible aminal gel composition |
| CN112794946A (en) * | 2020-12-31 | 2021-05-14 | 中国石油大学(华东) | Novel hydrophobic association plugging agent and preparation method and application thereof |
| CN113501910B (en) * | 2021-09-09 | 2021-11-30 | 中国石油大学(华东) | Multiple non-covalent bond synergistic self-healing gel plugging agent and preparation and application thereof |
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| CN113698535A (en) * | 2020-05-21 | 2021-11-26 | 江苏百赛飞生物科技有限公司 | Polymer, composition, coating thereof and product |
| CN113943558A (en) * | 2021-10-15 | 2022-01-18 | 中国石油大学(华东) | Self-healing gel leakage preventer with covalent bond-non-covalent bond combined effect while drilling and preparation method and application thereof |
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