CN118496830B - Self-adaptive chemical water shutoff agent and preparation method thereof - Google Patents
Self-adaptive chemical water shutoff agent and preparation method thereof Download PDFInfo
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 86
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 37
- 239000000126 substance Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000000835 fiber Substances 0.000 claims abstract description 66
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 47
- 239000004005 microsphere Substances 0.000 claims abstract description 40
- 239000002131 composite material Substances 0.000 claims abstract description 21
- 239000007863 gel particle Substances 0.000 claims abstract description 21
- 108010059892 Cellulase Proteins 0.000 claims abstract description 20
- 229940106157 cellulase Drugs 0.000 claims abstract description 20
- CNCOEDDPFOAUMB-UHFFFAOYSA-N N-Methylolacrylamide Chemical compound OCNC(=O)C=C CNCOEDDPFOAUMB-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000000502 dialysis Methods 0.000 claims abstract description 16
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000000661 sodium alginate Substances 0.000 claims abstract description 11
- 235000010413 sodium alginate Nutrition 0.000 claims abstract description 11
- 229940005550 sodium alginate Drugs 0.000 claims abstract description 11
- 229920000371 poly(diallyldimethylammonium chloride) polymer Polymers 0.000 claims abstract description 10
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims description 20
- 229920001214 Polysorbate 60 Polymers 0.000 claims description 15
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 14
- 238000001914 filtration Methods 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- 239000003999 initiator Substances 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 238000004132 cross linking Methods 0.000 claims description 8
- 239000004094 surface-active agent Substances 0.000 claims description 8
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 7
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 7
- 150000001768 cations Chemical class 0.000 claims description 6
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 5
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 claims description 5
- WURBFLDFSFBTLW-UHFFFAOYSA-N benzil Chemical group C=1C=CC=CC=1C(=O)C(=O)C1=CC=CC=C1 WURBFLDFSFBTLW-UHFFFAOYSA-N 0.000 claims description 5
- 230000000977 initiatory effect Effects 0.000 claims description 5
- 229920005610 lignin Polymers 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 238000006116 polymerization reaction Methods 0.000 claims description 5
- 239000001632 sodium acetate Substances 0.000 claims description 5
- 235000017281 sodium acetate Nutrition 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 230000003044 adaptive effect Effects 0.000 claims description 2
- 238000005286 illumination Methods 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 10
- 230000000903 blocking effect Effects 0.000 abstract description 9
- 239000001913 cellulose Substances 0.000 abstract description 3
- 229920002678 cellulose Polymers 0.000 abstract description 3
- 238000013508 migration Methods 0.000 abstract description 3
- 230000005012 migration Effects 0.000 abstract description 3
- 238000012986 modification Methods 0.000 abstract description 3
- 230000004048 modification Effects 0.000 abstract description 3
- 230000009471 action Effects 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 31
- 239000003921 oil Substances 0.000 description 20
- 238000010521 absorption reaction Methods 0.000 description 8
- 238000002347 injection Methods 0.000 description 7
- 239000007924 injection Substances 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 6
- 239000007788 liquid Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 238000010276 construction Methods 0.000 description 4
- 230000035699 permeability Effects 0.000 description 4
- 239000003129 oil well Substances 0.000 description 3
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- -1 aliphatic secondary amine Chemical class 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 229920000136 polysorbate Polymers 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000012800 visualization Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- 229920001410 Microfiber Polymers 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 229920002522 Wood fibre Polymers 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000001493 electron microscopy Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000003658 microfiber Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000002025 wood fiber Substances 0.000 description 1
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- 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
- C09K8/512—Compositions based on water or polar solvents containing organic compounds macromolecular compounds containing cross-linking agents
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F289/00—Macromolecular compounds obtained by polymerising monomers on to macromolecular compounds not provided for in groups C08F251/00 - C08F287/00
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Abstract
The application relates to the technical field of oilfield chemistry, and particularly discloses a self-adaptive chemical water shutoff agent and a preparation method thereof. A self-adaptive chemical water shutoff agent and a preparation method thereof comprise composite fiber gel particles, sodium alginate, dialysis regulator, micro-nano functional fibers and water according to weight percentage; the fiber cationization is realized through polydiallyl dimethyl ammonium chloride, the action effect of cellulase is promoted, the deep migration capacity and adsorptivity of the cellulose are improved, N-methylol acrylamide is adopted to carry out surface modification on acrylamide crosslinked microspheres, active double bonds are introduced, and then the acrylamide crosslinked microspheres are crosslinked with micro-nano functional fibers and acrylamide to prepare composite fiber gel particles, so that the toughness and water blocking capacity of the composite fiber gel particles are improved. The self-adaptive chemical water shutoff agent prepared by the preparation method has the characteristics of self-adaptation of the entering performance and the reservoir diversion capacity, and self-adaptation of the plugging performance and the reservoir oil saturation.
Description
Technical Field
The application relates to the technical field of oilfield chemistry, in particular to a self-adaptive chemical plugging agent and a preparation method thereof.
Background
In the low-permeability oil reservoir in China, because of serious reservoir heterogeneity, injected water flows along a high-permeability zone, so that the injection water has poor effect, the water content in the produced liquid of an oil well rises quickly, the water shutoff and profile control technology is always an effective technical means for improving the water injection development effect and realizing the stable production of the oil reservoir in the oil field, the influence of stratum water and injected water on the oil well can be effectively controlled, the water content of the oil well is reduced, the utilization degree of the oil layer is improved, the recoverable reserve of crude oil is increased, and finally the purpose of improving the recovery ratio is achieved.
At present, the water control of the low-permeability oil reservoir horizontal well still faces the technical problems of quick water finding, high-efficiency water shutoff and the like, and mainly comprises (1) the water finding of the low-flow horizontal well is difficult; (2) water patterns are various: factors such as well pattern/pattern of network, water injection mode, injected water/stratum water, reservoir characteristics and the like lead to multiple water-breakthrough intervals, complex water-breakthrough types/directions and difficult recognition of effective characteristics; (3) The horizontal well sections are long, the number of the fracturing sections is large, and the contradiction between the joints is prominent; overflow of inner series flow of the outer layer of the pipe sand discharge, leakage and the like. The adaptability of the conventional water shutoff measures and water shutoff processes is poor, and the effective rate of profile control and water shutoff treatment is low. Chinese patent application CN102040975A discloses a silicate water shutoff agent, which consists of sodium silicate, aluminum sulfate, calcium chloride, starch, and cement. Although convenient and cheap to prepare, the preparation has the defects of lower strength and limited field application.
Disclosure of Invention
The application provides a self-adaptive chemical water shutoff agent and a preparation method thereof, and aims to further solve the technical problem that a horizontal well of a low-permeability oil reservoir is low in water control and water shutoff capability.
In a first aspect, the application provides a self-adaptive chemical water shutoff agent, which adopts the following technical scheme:
The self-adaptive chemical water shutoff agent comprises, by weight, 0.5-1.0% of composite fiber gel particles, 0.3-0.8% of sodium alginate, 0.5-1.5% of dialysis regulator, 0.5-1.5% of micro-nano functional fibers and the balance of water.
By adopting the technical scheme, the self-adaptive chemical water shutoff agent is prepared by taking the composite fiber gel particles, sodium alginate, a dialysis regulator and micro-nano functional fibers as main bodies, and has the characteristics of easiness in entering wide slits, difficulty in entering narrow slits, strong water shutoff capability and high oil phase permeability.
Preferably, the preparation method of the micro-nano functional fiber comprises the following steps: immersing lignin fiber in a polydiallyl dimethyl ammonium chloride solution with the cation concentration of 20-25%, uniformly stirring, adding 50u/mg of cellulase for enzymolysis, filtering, and drying to obtain the micro-nano functional fiber. The cation concentration in the polydiallyl dimethyl ammonium chloride solution is specifically the ammonium cation concentration.
Through adopting above-mentioned technical scheme, polydiallyl dimethyl ammonium chloride realizes fibre cationization, can promote the effect of cellulase simultaneously, makes wood fiber present more fine fiber, roughened surface, and has more hole and microfiber, strengthens its adsorption capacity.
Preferably, the cellulase is added in the following amount: adding 120-180mg of cellulase into each kilogram of lignocellulose; the enzymolysis conditions are as follows: the temperature is 45-65deg.C, pH is 4.5-6.5, and the time is 40-70min.
By adopting the technical scheme, under the condition, the obtained micro-nano functional fiber has the length of 2-10 mu m and the diameter of 2-8nm, has one-dimensional attribute of deep migration, has low viscosity, selectively enters high-permeability strips, has good adsorptivity and improves the water shutoff capacity.
Preferably, the preparation method of the composite fiber gel particles comprises the following steps: uniformly mixing an acrylamide solution with the mass content of 15-20%, micro-nano functional fibers and multifunctional group crosslinking microspheres, adding ammonium persulfate, reacting for 2-3 hours at 40-50 ℃, cooling to room temperature, filtering, and vacuum drying.
By adopting the technical scheme, the absorption capacity and strength of the self-adaptive chemical water shutoff agent can be enhanced.
Preferably, the mass volume ratio of the acrylamide solution to the micro-nano functional fiber to the multifunctional group crosslinking microsphere to the ammonium persulfate is (40-60) mL (1.5-2.5) g (3.5-5.5) g (10-15) mg.
By adopting the technical scheme, the composite fiber gel particles have strong water absorption capacity, high toughness and good deformation capacity.
Preferably, the preparation method of the multifunctional group crosslinked microsphere comprises the following steps: s1, uniformly mixing cyclohexane, span80-Tween60 and an acrylamide solution in proportion in a nitrogen environment, heating to 40-50 ℃, adding an initiator, initiating a polymerization reaction by illumination, reacting for 3-4 hours at constant temperature, and adding absolute ethyl alcohol to demulsify to obtain a nanoscale crosslinked microsphere solution; s2, adding p-toluenesulfonic acid into the nano-scale crosslinked microsphere solution, then adding N-methylolacrylamide, heating to 60-65 ℃, reacting for 1-1.5 hours at constant temperature, then adding absolute ethyl alcohol, filtering, washing with acetone, and drying in vacuum to obtain the multifunctional crosslinked microsphere.
By adopting the technical scheme, the obtained multifunctional group crosslinked microsphere has strong crosslinking capability.
Preferably, the volume ratio of the cyclohexane, span80-Tween60 and the acrylamide solution in the S1 is (50-80): (10-12): (20-30), the mass content of the acrylamide in the acrylamide solution is 50%, the mass ratio of Span80 and Tween60 in Span80-Tween60 is 3:1, the initiator is dibenzoyl, and the addition amount is 0.5-0.6% of the mass of the acrylamide; the acrylamide solution also contains sodium acetate with the mass content of 4 percent.
By adopting the technical scheme, the obtained multifunctional group crosslinked microsphere has moderate particle size.
Preferably, the mass of the N-methylol acrylamide in the S2 is 70-80% of the mass of the acrylamide in the S1, and the addition amount of the p-toluenesulfonic acid is 0.5-1% of the mass of the N-methylol acrylamide.
By adopting the technical scheme, the conversion rate of the multifunctional group crosslinked microsphere is high.
Preferably, the dialysis modulator is a gemini surfactant.
By adopting the technical scheme, the oil-water interfacial tension can be effectively reduced, and the oil displacement efficiency is improved.
In a second aspect, the application provides a method for preparing a self-adaptive chemical water shutoff agent, which comprises the following steps: sequentially adding sodium alginate, micro-nano functional fibers, composite fiber gel particles and dialysis regulator into water under stirring, and stirring uniformly to obtain the product.
In summary, the application has the following beneficial effects:
1. The self-adaptive chemical water shutoff agent prepared by taking composite fiber gel particles, sodium alginate, dialysis regulator and micro-nano functional fibers as main bodies has the advantages that the wide slit is easy to enter, and the narrow slit is difficult to enter; strong water blocking capability and high oil phase permeability.
2. According to the application, polydiallyl dimethyl ammonium chloride is preferably adopted to assist cellulose to prepare micro-nano functional fibers, fiber cationization is realized through polydiallyl dimethyl ammonium chloride, the action effect of cellulose can be promoted, micro-nano functional fibers with the length of 2-10 mu m and the diameter of 2-8nm are finally obtained, and the micro-nano functional fibers have the characteristics of one-dimensional property capable of deep migration, selective entry into high-permeability strips and good adsorptivity, and can be matched with components such as composite fiber gel particles, sodium alginate, dialysis regulator and the like to form a net structure, so that the water blocking capacity is improved.
3. In the application, the N-methylol acrylamide is preferably adopted to carry out surface modification on the acrylamide crosslinked microsphere, active double bonds are introduced, and then the acrylamide crosslinked microsphere is crosslinked with the micro-nano functional fiber and the acrylamide to prepare the composite fiber gel particles, so that the toughness and water shutoff capacity of the composite fiber gel particles gel are improved.
4. The self-adaptive chemical water shutoff agent prepared by the preparation method has the characteristics of self-adaptation of the entering performance and the reservoir diversion capacity, and self-adaptation of the plugging performance and the reservoir oil saturation.
Drawings
Fig. 1: the infrared spectrogram of the multifunctional group crosslinked microsphere prepared by the application.
Fig. 2: the electron microscope scanning image of the micro-nano functional fiber prepared by the application.
Fig. 3: the preparation path of the multifunctional group crosslinked microsphere is provided.
Fig. 4: the oil/water phase permeability test chart (upper curve corresponds to water phase and lower curve corresponds to oil phase) of the self-adaptive chemical water shutoff agent prepared by the application.
Fig. 5: the application provides an evaluation chart of the crack plugging effect of the self-adaptive chemical plugging agent.
Fig. 6: the self-adaptive chemical plugging agent prepared by the application is used for plugging a three-dimensional contour map (upper part is before plugging and lower part is after plugging) of a pressure gradient field in a crack before and after plugging.
Fig. 7: the application effect graph (upper curve: water content percentage; middle curve: daily liquid yield; lower curve: daily oil yield) of the self-adaptive chemical water shutoff agent prepared by the application.
Detailed Description
The present application will be described in further detail with reference to examples.
The raw materials of the examples and comparative examples of the present application are commercially available in general except for the specific descriptions.
Examples
Example 1
The self-adaptive chemical water shutoff agent comprises, by weight, 0.5% of composite fiber gel particles, 0.8% of sodium alginate, 0.5% of dialysis regulator, 1.5% of micro-nano functional fibers and the balance of water.
The preparation method of the micro-nano functional fiber comprises the following steps: immersing lignin fiber in a polydiallyl dimethyl ammonium chloride solution with the cation concentration of 20%, uniformly stirring, adding 50u/mg of cellulase for enzymolysis, filtering, and drying to obtain the micro-nano functional fiber. The addition amount of the cellulase is as follows: 120mg of cellulase is added per kilogram of lignocellulose; the enzymolysis conditions are as follows: the temperature is 45 ℃, the pH is 4.5, and the time is 40min; the cellulase is 3000U/g.
The preparation method of the composite fiber gel particles comprises the following steps: uniformly mixing 40mL of acrylamide solution with the mass content of 15%, 1.5g of micro-nano functional fiber and 3.5g of multifunctional group crosslinking microsphere, finally adding 10mg of ammonium persulfate, reacting for 2 hours at 40 ℃, cooling to room temperature, filtering, and drying in vacuum.
The preparation method of the multifunctional group crosslinked microsphere comprises the following steps:
S1, uniformly mixing 50mL of cyclohexane, 10mL of Span80-Tween and 20mL of acrylamide solution in proportion in a nitrogen environment, heating to 40 ℃, adding an initiator, initiating polymerization reaction by ultraviolet irradiation (ultraviolet light with the wavelength of 365nm and the light intensity of 120mW/cm 2, and the irradiation time of 70S), reacting at constant temperature for 3 hours, and adding absolute ethyl alcohol to demulsify to obtain a nanoscale crosslinked microsphere solution; the mass ratio of Span80 to Tween60 in Span80-Tween60 is 3:1, the mass content of acrylamide in the acrylamide solution is 50%, and the acrylamide solution also contains sodium acetate with the mass content of 4%; the initiator is dibenzoyl, and the addition amount is 0.5 percent of the mass of the acrylamide.
S2, adding p-toluenesulfonic acid into the nano-scale crosslinked microsphere solution, then adding N-methylolacrylamide, heating to 60 ℃, reacting for 1h at constant temperature, then adding absolute ethyl alcohol, filtering, washing with acetone, and drying in vacuum to obtain the multifunctional crosslinked microsphere; the mass of the N-methylol acrylamide in the S2 is 70% of the mass of the acrylamide in the S1, and the addition amount of the p-toluenesulfonic acid is 0.5% of the mass of the N-methylol acrylamide.
The dialysis regulator is a gemini surfactant, preferably a sulfonate gemini surfactant.
Example 2
The self-adaptive chemical water shutoff agent comprises, by weight, 0.8% of composite fiber gel particles, 0.5% of sodium alginate, 1.0% of dialysis regulator, 1.0% of micro-nano functional fibers and the balance of water.
The preparation method of the micro-nano functional fiber comprises the following steps: immersing lignin fiber in a polydiallyl dimethyl ammonium chloride solution with the cation concentration of 23%, uniformly stirring, adding 50u/mg of cellulase for enzymolysis, filtering, and drying to obtain the micro-nano functional fiber. The addition amount of the cellulase is as follows: 150mg of cellulase is added per kilogram of lignocellulose; the enzymolysis conditions are as follows: the temperature is 50 ℃, the pH is 5, and the time is 55min; the cellulase is 3000U/g.
The preparation method of the composite fiber gel particles comprises the following steps: 50mL of acrylamide solution with the mass content of 18%, 2.0g of micro-nano functional fiber and 4.0g of multifunctional group crosslinking microsphere are uniformly mixed, and finally 13mg of ammonium persulfate is added for reaction for 3 hours at 45 ℃, cooled to room temperature, filtered by suction, and dried in vacuum.
The preparation method of the multifunctional group crosslinked microsphere (shown in figure 3) comprises the following steps:
S1, uniformly mixing 65mL of cyclohexane, 80-Tween60 mL of Span and 25mL of acrylamide solution in proportion in a nitrogen environment, heating to 45 ℃, adding an initiator, initiating polymerization reaction by ultraviolet irradiation (ultraviolet light with the wavelength of 365nm, the light intensity of 120mW/cm 2 and the irradiation time of 75S), reacting at constant temperature for 3.5h, and then adding absolute ethyl alcohol to demulsify to obtain a nanoscale crosslinked microsphere solution; the mass ratio of Span80 to Tween60 in Span80-Tween60 is 3:1, the mass content of acrylamide in the acrylamide solution is 50%, and the acrylamide solution also contains sodium acetate with the mass content of 4%; the initiator is dibenzoyl, and the addition amount is 0.55 percent of the mass of the acrylamide.
S2, adding p-toluenesulfonic acid into the nano-scale crosslinked microsphere solution, then adding N-methylolacrylamide, heating to 65 ℃, reacting for 1h at constant temperature, then adding absolute ethyl alcohol, filtering, washing with acetone, and drying in vacuum to obtain the multifunctional crosslinked microsphere; the mass of the N-methylol acrylamide in the S2 is 75% of that of the acrylamide in the S1, and the addition amount of the p-toluenesulfonic acid is 0.8% of that of the N-methylol acrylamide.
The dialysis regulator is a gemini surfactant, preferably a sulfonate gemini surfactant.
Example 3
The self-adaptive chemical water shutoff agent comprises, by weight, 1.0% of composite fiber gel particles, 0.3% of sodium alginate, 1.5% of dialysis regulator, 0.5% of micro-nano functional fibers and the balance of water.
The preparation method of the micro-nano functional fiber comprises the following steps: immersing lignin fiber in polydiallyl dimethyl ammonium chloride solution with the cation concentration of 25%, stirring uniformly, adding 50u/mg of cellulase for enzymolysis, filtering, and drying to obtain the micro-nano functional fiber. The addition amount of the cellulase is as follows: 180mg of cellulase is added per kilogram of lignocellulose; the enzymolysis conditions are as follows: the temperature is 65 ℃, the pH is 6.5, and the time is 70min; the cellulase is 3000U/g.
The preparation method of the composite fiber gel particles comprises the following steps: and (3) uniformly mixing 60mL of acrylamide solution with the mass content of 20%, 2.5g of micro-nano functional fibers and 5.5g of multifunctional group crosslinking microspheres, adding 15mg of ammonium persulfate, reacting for 3 hours at 50 ℃, cooling to room temperature, filtering, and drying in vacuum.
The preparation method of the multifunctional group crosslinked microsphere comprises the following steps:
S1, uniformly mixing 80mL of cyclohexane, 12mL of Span80-Tween and 30mL of acrylamide solution in proportion in a nitrogen environment, heating to 50 ℃, adding an initiator, initiating polymerization reaction by ultraviolet irradiation (ultraviolet light with the wavelength of 365nm and the light intensity of 120mW/cm 2, and the irradiation time of 80S), reacting at constant temperature for 4 hours, and adding absolute ethyl alcohol to demulsify to obtain a nanoscale crosslinked microsphere solution; the mass ratio of Span80 to Tween60 in Span80-Tween60 is 3:1, the mass content of acrylamide in the acrylamide solution is 50%, and the acrylamide solution also contains sodium acetate with the mass content of 4%; the initiator is dibenzoyl, and the addition amount is 0.6 percent of the mass of the acrylamide.
S2, adding p-toluenesulfonic acid into the nano-scale crosslinked microsphere solution, then adding N-methylolacrylamide, heating to 65 ℃, reacting for 1.5 hours at constant temperature, then adding absolute ethyl alcohol, filtering, washing with acetone, and drying in vacuum to obtain the multifunctional crosslinked microsphere; the mass of the N-methylol acrylamide in the S2 is 80% of that of the acrylamide in the S1, and the addition amount of the p-toluenesulfonic acid is 1% of that of the N-methylol acrylamide.
The dialysis regulator is a gemini surfactant, preferably a sulfonate gemini surfactant.
The preparation method of the self-adaptive chemical water shutoff agent comprises the following steps: sequentially adding sodium alginate, micro-nano functional fibers, composite fiber gel particles and dialysis regulator into water under stirring, and stirring uniformly to obtain the product.
Performance test
(1) The infrared analysis was performed on the multi-functional crosslinked microspheres obtained in example 1, and the results are shown in fig. 1, and it can be seen from fig. 1 that a strong absorption peak at a wave number of 1630.1cm -1 is caused by stretching vibration of a c=c double bond; the absorption peak at 1686.3cm -1 at wavenumber is due to the c=o bond in the amide; the absorption peak at 3194.7cm -1 is aliphatic secondary amine NH stretch; other absorption peaks are also: the absorption peak of the wave number at 2913.5cm -1 is caused by alkane antisymmetric expansion; the absorption peak at 1448.0cm -1 at wavenumber is caused by CH2 alkane angulation. Therefore, it was confirmed that a reactive c=c double bond was smoothly introduced into the multi-functional group crosslinked microsphere structure.
(2) The multi-functional crosslinked microspheres obtained in example 1 were analyzed for particle size by using a laser particle size analyzer, and 73% of the particles were found to have a particle size of less than 40. Mu.m.
(3) The micro-nano functional fiber obtained in example 2 was subjected to electron microscopy and analysis, and the result is shown in fig. 2. As can be seen from FIG. 2, the micro-nano functional fiber has a length of between 2 and 10 μm and a diameter of between 2 and 8nm.
(4) The oil/water phase permeability test was performed on the adaptive chemical water shutoff agent prepared in example 3, and the results are shown in fig. 4 (upper curve corresponds to water phase, lower curve corresponds to oil phase). As can be seen from fig. 4, the capacity of the prepared self-adaptive chemical water shutoff agent for blocking the water phase is far higher than that of the oil phase, and the oil phase passing capacity is 100 times that of the water phase.
(5) Meanwhile, the self-adaptive chemical plugging agent prepared in the embodiment 2 is subjected to complex fracture plugging effect evaluation under different injection rates by using a parallel double-fracture visualization model (the large fracture width is 5mm and the small fracture width is 1 mm) and a parallel double-fracture visualization model (the large fracture width is 5mm and the small fracture width is 2 mm), and the result is shown in fig. 5. As can be seen from fig. 5, the self-adaptive chemical water shutoff agent mainly enters the wide slit at different injection rates, and the larger the slit width difference of the parallel slits is, the more obvious the shielding effect of the wide slit on the narrow slit is.
(6) The degree of influence on the pressure gradient in the crack before and after the plugging of the self-adaptive chemical plugging agent: the self-adaptive chemical plugging agent prepared in example 3 has a plugging residence size of 0.5PV in a seam, the water flooding pressure before and after plugging is tested, and a pressure gradient contour map is shown in FIG. 6 (upper: before plugging; lower: after plugging). As can be seen from fig. 6, after plugging, the water flooding pressure gradient value in the crack is obviously increased, which indicates that more water is injected into the strong flooding zone and the weak flooding zone subsequently due to the plugging effect of the plugging agent, so that the water flooding sweep coefficient is enlarged, and the recovery degree of residual oil is improved.
(7) The self-adaptive chemical plugging agent prepared in the embodiment 2 prepared by the application is used for plugging water test on an iron 90-95 well (sand-added 25-square fracturing after perforation of a section of length 6 layers 2198.0-2203.0m (5.0 m); the early-stage production of the well is higher, the production of the adjacent well is better, and the water content is lower. The initial oil production period of the rising period of water content is more than 2t, and then the water blocking is performed due to the reduction of the blocking liquid amount, the pressure cracking blocking is still high, the water content is stopped, the water blocking construction is performed, the dosage is 350m 3, the accumulated injection liquid amount is 500m 3, and the discharge capacity is 15-18m 3/h; injection pressure of 10-13MPa, year 2032 of 10 and (5) water blocking construction is carried out on the fixed pipe column. High water content well stopping before water shutoff construction, 5.36m 3 of daily production liquid after water shutoff construction, 0.67t of daily production oil and 87.6% of water content (shown in figure 7).
The present embodiment is merely illustrative of the present application and is not intended to be limiting, and those skilled in the art, having read the present specification, may make modifications to the present embodiment without creative contribution as required, provided that they are protected by patent laws within the scope of protection of the present application.
Claims (6)
1. The self-adaptive chemical water shutoff agent is characterized by comprising, by weight, 0.5-1.0% of composite fiber gel particles, 0.3-0.8% of sodium alginate, 0.5-1.5% of dialysis regulator, 0.5-1.5% of micro-nano functional fibers and the balance of water; the preparation method of the micro-nano functional fiber comprises the following steps: immersing lignin fiber in a polydiallyl dimethyl ammonium chloride solution with the cation concentration of 20-25%, uniformly stirring, adding 50u/mg of cellulase for enzymolysis, filtering, and drying to obtain micro-nano functional fiber; the preparation method of the composite fiber gel particles comprises the following steps: uniformly mixing an acrylamide solution, micro-nano functional fibers and multifunctional group crosslinking microspheres, adding ammonium persulfate, reacting at 40-50 ℃ for 2-3 hours, cooling to room temperature, filtering, and vacuum drying; the mass content of acrylamide in the acrylamide solution is 15% -20%; the multifunctional group crosslinked microsphere has a multi-alkenyl structure; the dialysis regulator is a twin-type surfactant.
2. The adaptive chemical plugging agent according to claim 1, wherein the cellulase is added in an amount of: adding 120-180mg of cellulase into each kilogram of lignocellulose; the enzymolysis conditions are as follows: the temperature is 45-65deg.C, pH is 4.5-6.5, and the time is 40-70min.
3. The self-adaptive chemical water shutoff agent according to claim 2, wherein the mass volume ratio of the acrylamide solution, the micro-nano functional fiber, the multifunctional group crosslinking microsphere and the ammonium persulfate is (40-60) mL (1.5-2.5) g (3.5-5.5) g (10-15) mg.
4. The self-adaptive chemical plugging agent according to claim 3, wherein the preparation method of the multifunctional group crosslinked microsphere comprises the following steps: s1, uniformly mixing cyclohexane, span80-Tween60 and an acrylamide solution in proportion in a nitrogen environment, heating to 40-50 ℃, adding an initiator, initiating a polymerization reaction by illumination, reacting for 3-4 hours at constant temperature, and adding absolute ethyl alcohol to demulsify to obtain a nanoscale crosslinked microsphere solution; s2, adding p-toluenesulfonic acid into the nano-scale crosslinked microsphere solution, then adding N-methylolacrylamide, heating to 60-65 ℃, reacting for 1-1.5 hours at constant temperature, then adding absolute ethyl alcohol, filtering, washing with acetone, and drying in vacuum to obtain the multifunctional crosslinked microsphere.
5. The self-adaptive chemical water shutoff agent according to claim 4, wherein the volume ratio of cyclohexane, span80-Tween60 and acrylamide solution in S1 is (50-80): (10-12): (20-30), the mass content of acrylamide in the acrylamide solution is 50%, the mass ratio of Span80 and Tween60 in Span80-Tween60 is 3:1, the initiator is dibenzoyl, and the addition amount is 0.5-0.6% of the mass of acrylamide; the acrylamide solution also contains sodium acetate with the mass content of 4 percent.
6. The self-adaptive chemical water shutoff agent according to claim 5, wherein the mass of the N-methylol acrylamide in the S2 is 70-80% of the mass of the acrylamide in the S1, and the addition amount of the p-toluenesulfonic acid is 0.5-1% of the mass of the N-methylol acrylamide.
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| CN102516431A (en) * | 2011-12-15 | 2012-06-27 | 中国石油天然气股份有限公司 | Macromolecular cross-linking agent for acrylamide gel for water shutoff and preparation method thereof |
| CN104594114A (en) * | 2015-01-15 | 2015-05-06 | 齐鲁工业大学 | Method for regulating viscosity of dissolving pulp by enhancing cellulase treatment |
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| US8887808B2 (en) * | 2011-11-09 | 2014-11-18 | Halliburton Energy Services, Inc. | Engineered methods and materials for wellbore strengthening in subterranean operations |
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| CN104594114A (en) * | 2015-01-15 | 2015-05-06 | 齐鲁工业大学 | Method for regulating viscosity of dissolving pulp by enhancing cellulase treatment |
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