CN117987105A - IPN gel plugging agent and preparation method and application thereof - Google Patents
IPN gel plugging agent and preparation method and application thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 63
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 24
- 229920000642 polymer Polymers 0.000 claims abstract description 24
- 239000005011 phenolic resin Substances 0.000 claims abstract description 20
- 229920001568 phenolic resin Polymers 0.000 claims abstract description 19
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229920003169 water-soluble polymer Polymers 0.000 claims abstract description 12
- 239000000178 monomer Substances 0.000 claims description 40
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 22
- 239000000126 substance Substances 0.000 claims description 21
- 238000010438 heat treatment Methods 0.000 claims description 16
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 239000007864 aqueous solution Substances 0.000 claims description 14
- 239000003999 initiator Substances 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 239000002981 blocking agent Substances 0.000 claims description 11
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 claims description 10
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 9
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 9
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 8
- YCIMNLLNPGFGHC-UHFFFAOYSA-N catechol Chemical compound OC1=CC=CC=C1O YCIMNLLNPGFGHC-UHFFFAOYSA-N 0.000 claims description 8
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000000084 colloidal system Substances 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- DZSVIVLGBJKQAP-UHFFFAOYSA-N 1-(2-methyl-5-propan-2-ylcyclohex-2-en-1-yl)propan-1-one Chemical compound CCC(=O)C1CC(C(C)C)CC=C1C DZSVIVLGBJKQAP-UHFFFAOYSA-N 0.000 claims description 5
- 230000002209 hydrophobic effect Effects 0.000 claims description 5
- 230000000379 polymerizing effect Effects 0.000 claims description 5
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 4
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 4
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims description 4
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims description 4
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 2
- 230000001376 precipitating effect Effects 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 abstract description 17
- 238000006243 chemical reaction Methods 0.000 abstract description 11
- 229920002401 polyacrylamide Polymers 0.000 abstract description 9
- 238000004132 cross linking Methods 0.000 abstract description 7
- 230000001737 promoting effect Effects 0.000 abstract 1
- 239000000499 gel Substances 0.000 description 70
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 18
- 239000000243 solution Substances 0.000 description 16
- 238000005303 weighing Methods 0.000 description 12
- 239000000203 mixture Substances 0.000 description 11
- 239000003513 alkali Substances 0.000 description 8
- 239000003431 cross linking reagent Substances 0.000 description 7
- IRLPACMLTUPBCL-KQYNXXCUSA-N 5'-adenylyl sulfate Chemical compound C1=NC=2C(N)=NC=NC=2N1[C@@H]1O[C@H](COP(O)(=O)OS(O)(=O)=O)[C@@H](O)[C@H]1O IRLPACMLTUPBCL-KQYNXXCUSA-N 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 239000003708 ampul Substances 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 230000033558 biomineral tissue development Effects 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000007599 discharging Methods 0.000 description 4
- 239000012263 liquid product Substances 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 230000003111 delayed effect Effects 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920003987 resole Polymers 0.000 description 3
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 125000003368 amide group Chemical group 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 230000000903 blocking effect Effects 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 150000002989 phenols Chemical class 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- 235000019353 potassium silicate Nutrition 0.000 description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- VZSRBBMJRBPUNF-UHFFFAOYSA-N 2-(2,3-dihydro-1H-inden-2-ylamino)-N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]pyrimidine-5-carboxamide Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C(=O)NCCC(N1CC2=C(CC1)NN=N2)=O VZSRBBMJRBPUNF-UHFFFAOYSA-N 0.000 description 1
- APLNAFMUEHKRLM-UHFFFAOYSA-N 2-[5-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]-1,3,4-oxadiazol-2-yl]-1-(3,4,6,7-tetrahydroimidazo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C1=NN=C(O1)CC(=O)N1CC2=C(CC1)N=CN2 APLNAFMUEHKRLM-UHFFFAOYSA-N 0.000 description 1
- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 1
- 241000486679 Antitype Species 0.000 description 1
- 229910014033 C-OH Inorganic materials 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 229910014570 C—OH Inorganic materials 0.000 description 1
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- 238000010793 Steam injection (oil industry) Methods 0.000 description 1
- LXEKPEMOWBOYRF-UHFFFAOYSA-N [2-[(1-azaniumyl-1-imino-2-methylpropan-2-yl)diazenyl]-2-methylpropanimidoyl]azanium;dichloride Chemical compound Cl.Cl.NC(=N)C(C)(C)N=NC(C)(C)C(N)=N LXEKPEMOWBOYRF-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000002843 carboxylic acid group Chemical group 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 238000010528 free radical solution polymerization reaction Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- -1 phenolic aldehyde Chemical class 0.000 description 1
- 229920002239 polyacrylonitrile Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000004289 sodium hydrogen sulphite Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 125000000542 sulfonic acid group Chemical group 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 229920001285 xanthan gum Polymers 0.000 description 1
- 229940082509 xanthan gum Drugs 0.000 description 1
- 235000010493 xanthan gum Nutrition 0.000 description 1
- 239000000230 xanthan gum Substances 0.000 description 1
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- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention provides an IPN gel plugging agent and a preparation method and application thereof, and belongs to the technical field of oil and gas exploitation. According to the performance requirements of the gel plugging agent for plugging water of a high-temperature high-salt carbonate fracture-cavity oil reservoir, a novel temperature-resistant salt-resistant water-soluble polymer and water-soluble phenolic resin are firstly prepared, then the novel temperature-resistant salt-resistant water-soluble polymer and the water-soluble phenolic resin are mixed according to a certain proportion to prepare a gel prepolymer of an Interpenetrating Polymer Network (IPN), and a curing reaction and a crosslinking reaction gradually occur under the high-temperature condition of the oil reservoir. Thus forming an interpenetrating network structure simultaneously containing a phenolic resin rigid crosslinked network and a polyacrylamide flexible crosslinked network in the gel, and promoting the gel to have the characteristics of high strength, temperature resistance, salt resistance, selective water shutoff and the like.
Description
Technical Field
The invention belongs to the technical field of oil and gas exploitation, and particularly relates to an IPN gel plugging agent and a preparation method and application thereof.
Background
The gel plugging agent system using metal ions as a cross-linking agent is a common plugging system and mainly comprises an aluminum, chromium, zirconium cross-linking agent and polyacrylamide. As patent CN1003048B discloses a zirconium gel water shutoff system, but the gel forming time is shorter and the gel strength is weaker; for example, patent CN1046151C discloses an aluminum gel water shutoff system, but the temperature resistance is poor, and the gel forming speed is high under the high temperature condition. The metal ion crosslinking system has short gel forming time and poor high-temperature thermal stability under high-temperature conditions, and is mainly suitable for water plugging of medium-low temperature oil reservoirs.
The water shutoff system made of inorganic gel material has the characteristics of low initial viscosity, high water shutoff strength, high temperature and high salt resistance, and the like. For example, patent CN103627376a discloses a water glass inorganic gel plugging agent, which is formed by compounding water glass and polyacrylamide. But does not have oil-water selectivity and is not suitable for the water plugging requirement of the fractured carbonate reservoir.
The gel blocking agent system using phenolic aldehyde organic matters as a cross-linking agent is a common high-temperature delayed cross-linking system, and is mainly compounded by using phenols, aldehydes or low-molecular-weight phenolic resins as the cross-linking agent and polyacrylamide as a polymer. For example, patent CN108219761a discloses a foam gel water shutoff system composed of 0.25% polyacrylamide, 6% xanthan gum, 0.25% phenolic resin cross-linking agent and 1% surfactant, which has the characteristics of delaying cross-linking and resisting high temperature; for example, patent CN105802598a discloses a gel water shutoff system composed of lignin, formaldehyde, phenol and polyacrylonitrile, which has the characteristic of resisting 150 ℃ and 20 ten thousand mineralizations; for example, patent CN103421475A discloses a gel water shutoff system composed of polyacrylamide, inorganic chromium crosslinking agent and phenolic resin crosslinking agent, which can realize the shutoff during high-temperature steam injection. The crosslinking system has longer gel forming time and better temperature and salt resistance, but has larger toxicity of phenol and formaldehyde, is unfavorable for site construction, has poorer gel strength under high temperature condition and has poorer water blocking performance.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention provides an IPN gel plugging agent and a preparation method and application thereof. Firstly, preparing a temperature-resistant and salt-resistant water-soluble polymer KY and a phenolic resin oligomer WPF with good water solubility; preparing mixed solution of KY and WPF according to different proportions, namely IPN gel prepolymer, and injecting the mixed solution into the ground; under the oil reservoir condition of high temperature and high salt, most of the resol resin is salted out, and the curing reaction of the resol resin is carried out under the high temperature condition, and a small amount of resol resin which does not carry out the curing reaction and amide groups of the KY polymer carry out the delayed crosslinking reaction. Therefore, the gel system contains two interpenetrating network structures of a phenolic resin rigid crosslinked network and a polyacrylamide flexible crosslinked network, the former can greatly improve the strength and the temperature resistance of the gel; the latter may promote selective water blocking properties of the gel.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
firstly, a preparation method of the IPN gel plugging agent is provided, which comprises the following steps:
(1) Preparation of a water-soluble polymer: dissolving monomers in water to prepare a monomer aqueous solution, introducing nitrogen, heating to 20-70 ℃, adding an initiator, polymerizing for 1.5-2.5 hours at constant temperature, taking out a polymer colloid, precipitating with absolute ethyl alcohol, washing with pure water, and vacuum drying to prepare a water-soluble polymer;
(2) Preparing water-soluble phenolic resin: mixing phenolic substances with alkaline aqueous solution, stirring and reacting for 15-25min at 45-55 ℃, adding aldehyde substances, heating to 85-95 ℃, and reacting at constant temperature for 25-35min to obtain water-soluble phenolic resin;
(3) Preparing an IPN gel plugging agent: dissolving the water-soluble polymer obtained in the step (1) and the water-soluble phenolic resin obtained in the step (2) in simulated water to obtain an IPN gel prepolymer, and heating and drying the IPN gel prepolymer to obtain the IPN gel plugging agent; wherein the temperature of heating and drying is 130-150 ℃ and the time is 2-4 hours.
Further, in the step (1), the monomer is one or more of acrylamide, acrylic acid, 2-acrylamide-2-methylpropanesulfonic acid, N-vinyl pyrrolidone and hydrophobic monomer.
Further, the weight ratio of the acrylamide to the acrylic acid to the 2-acrylamide-2-methylpropanesulfonic acid to the N-vinyl pyrrolidone to the hydrophobic monomer is 10-50:10-20:10-60:1-5:0.5-3, preferably 30-48:10-20:30-56:1-3:1.
Further, the initiator in the step (1) is one or more of ammonium persulfate, potassium persulfate, ammonium persulfate-sodium bisulphite and 2,2' -azo diisobutyl amidine dihydrochloride.
Further, the weight ratio of the monomer to the initiator in the step (1) is 100:0.01-0.1, preferably 100:0.02-0.05, the mass percent of the monomer in the monomer aqueous solution is 15-25%, preferably 20-25%.
Further, in the step (2), the phenolic substance is one or more of phenol, resorcinol and catechol, the alkaline substance in the alkaline aqueous solution is one or two of sodium hydroxide and potassium hydroxide, and the aldehyde substance is one or more of formaldehyde, acetaldehyde and urotropine.
Further, the weight ratio of the phenolic substance to the aldehyde substance in the step (2) is 1.1-3.0:1, wherein the alkaline substance accounts for 5-10% of the phenolic substance by mass.
Further, in the step (3), the weight ratio of the water-soluble polymer to the water-soluble phenolic resin to the simulated water is 0.1-2:1.5-10:88-98.4.
Secondly, an IPN gel plugging agent obtained by the preparation method is provided.
Finally, the IPN gel plugging agent obtained by the preparation method or the application of the IPN gel plugging agent in reservoir water plugging is provided.
In some specific embodiments, the method for preparing the IPN gel blocking agent comprises the following steps:
1. preparation of temperature-resistant and salt-resistant water-soluble polymer
(1) Monomer composition
Monomers such as acrylamide and acrylic acid are used for improving the water solubility of the polymer; in order to improve the temperature resistance and salt resistance of the polymer, functional monomers such as AMPS (2-acrylamide-2-methylpropanesulfonic acid), NVP (N-vinyl pyrrolidone), hydrophobic monomer (MJ-16) and the like are used, and the reaction chemical equation is as follows:
(2) Synthesis process
KY polymers are prepared by a free radical solution polymerization process. Weighing quantitative monomers to prepare an aqueous solution, stirring until the quantitative monomers are completely dissolved, introducing nitrogen and discharging oxygen for 30min, heating and adding an initiator; after 2h of constant temperature polymerization, the polymer colloid was taken out, precipitated with absolute ethanol and washed with pure water to remove unreacted monomers, and the polymer sample was dried under vacuum at 70 ℃ for 6h to constant weight to obtain KY white solid powder.
2. Preparation of water-soluble phenolic resin WPF
Weighing quantitative phenols in a three-neck flask, and stirring at 50 ℃; weighing quantitative alkaline substances, dissolving in water, preparing an alkali solution, adding the alkali solution into a reaction system, and stirring and reacting for 20min at 50 ℃. Aldehyde substances are added into the mixture by a constant pressure dropping funnel, the temperature is raised to 90 ℃, and the mixture is reacted for 30min at constant temperature. A bright reddish brown transparent liquid product was obtained.
3. Preparation and gel formation of IPN gel prepolymer
Preparing water solutions with certain concentration from the anti-type polymer KY and the phenolic resin WPF respectively by using simulated water, and mixing the water solutions with the simulated water according to a preset proportion to obtain the IPN gel prepolymer. The prepolymer was then sealed in an ampoule and stored in a high temperature oven for heating.
Compared with the prior art, the invention has the following beneficial effects:
(1) The gel blocking agent is formed by interpenetrating a rigid network of phenolic resin and a flexible network of crosslinked polyacrylamide;
(2) Both polymer networks have better temperature resistance and salt resistance;
(3) The rigid network skeleton formed by the phenolic resin is favorable for maintaining higher mechanical strength of the gel, and can effectively block larger cracks and karst cave;
(4) The flexible network formed by the crosslinked polyacrylamide is inserted into the rigid framework, which is helpful for enhancing the elasticity of the gel and realizing the oil-water selectivity;
(5) The initial viscosity of the gel prepolymer is low, and the curing and crosslinking reactions can only occur at high temperature, so that the injection of the plugging agent and the delay of gel formation are facilitated, and the construction safety is improved.
To sum up: the IPN gel plugging agent has the advantages of low initial viscosity, delayed gel formation, strong temperature resistance and salt resistance, high gel strength and the like. The oil-water selective passing is realized, so that the problems of reduced oil yield and the like caused by the conventional plugging agent when plugging water are avoided.
Drawings
FIG. 1 is an infrared spectrum of the IPN gel of example 3;
FIG. 2 is a graph showing the variation of water flooding pressure of a low-strength 1# gel plug with water flooding PV number;
FIG. 3 is a graph showing the variation of water flooding pressure of a medium strength 2# gel plugging agent with the number of water flooding PVs;
FIG. 4 shows the variation of water flooding pressure of the high strength 3# gel plugging agent with the water flooding PV number.
Detailed Description
It is to be noted that the raw materials used in the present invention are all common commercial products, and the sources thereof are not particularly limited.
Example 1 preparation of temperature and salt resistant IPN gel blocking agent 1#
(1) Preparation of KY polymers
Weighing quantitative monomers to prepare 25% aqueous solution, stirring until the monomers are completely dissolved, introducing nitrogen and discharging oxygen for 30 minutes, heating to 60 ℃, and adding an initiator; after polymerizing at constant temperature for 2 hours, the polymer colloid was taken out, precipitated with absolute ethanol and washed with pure water to remove unreacted monomers, and the polymer sample was dried under vacuum at 70 ℃ for 6 hours to constant weight to obtain KY white solid powder. The monomer composition is as follows: acrylamide: 48%; acrylic acid 20%; AMPS:30%; NVP:1%; MJ-16:1% of initiator, namely ammonium persulfate with the monomer content of 0.02%. The molecular weight of the KY polymer prepared was 620 ten thousand.
(2) Preparation of WPF
Weighing quantitative phenol in a three-neck flask, and stirring at 50 ℃; weighing a certain amount of potassium hydroxide, dissolving in water, preparing a 20% alkali solution, adding the alkali solution into a reaction system, and stirring and reacting for 20min at 50 ℃. Formaldehyde is added into the mixture by a constant pressure dropping funnel, the temperature is raised to 90 ℃, and the mixture is reacted for 30min at constant temperature. A bright reddish brown transparent liquid product was obtained. Wherein the proportion of phenol to formaldehyde is 1.5, the potassium hydroxide accounts for 4 percent of the mass of the phenol, and the formaldehyde is 37 percent of aqueous solution;
(3) Preparation of IPN gel
KY and WPF in certain proportion are prepared into water solution by using simulated water with the mineralization degree of 22 ten thousand respectively, and the KY and the WPF are mixed with the simulated water to obtain the IPN gel prepolymer. The prepolymer was then sealed in an ampoule and stored in a 140 ℃ high temperature oven for heating. In the IPN prepolymer, the KY ratio was 0.5%, the WPF ratio was 2%, and the remainder was simulated water.
Gel time was 72 hours and gel strength was determined to be grade G by code.
Example 2 preparation of temperature and salt resistant IPN gel blocking agent # 2
(1) Preparation of KY polymers
Weighing quantitative monomers to prepare 25% aqueous solution, stirring until the monomers are completely dissolved, introducing nitrogen and discharging oxygen for 30 minutes, heating to 60 ℃, and adding an initiator; after polymerizing at constant temperature for 2 hours, the polymer colloid was taken out, precipitated with absolute ethanol and washed with pure water to remove unreacted monomers, and the polymer sample was dried under vacuum at 70 ℃ for 6 hours to constant weight to obtain KY white solid powder. The monomer composition is as follows: acrylamide: 30%; acrylic acid 20%; AMPS:47%; NVP:2%; MJ-16:1% of initiator, namely ammonium persulfate with the monomer content of 0.05%. The molecular weight of the KY polymer prepared was 820 ten thousand.
(2) Preparation of WPF
Weighing quantitative phenol in a three-neck flask, and stirring at 50 ℃; weighing a certain amount of sodium hydroxide, dissolving in water, preparing a 20% alkali solution, adding the alkali solution into a reaction system, and stirring and reacting for 20min at 50 ℃. Formaldehyde is added into the mixture by a constant pressure dropping funnel, the temperature is raised to 90 ℃, and the mixture is reacted for 30min at constant temperature. A bright reddish brown transparent liquid product was obtained. Wherein the proportion of phenol to formaldehyde is 2.0, sodium hydroxide accounts for 8 percent of the mass of phenol, and formaldehyde is 37 percent of aqueous solution;
(3) Preparation of IPN gel
KY and WPF in certain proportion are prepared into water solution by using simulated water with the mineralization degree of 22 ten thousand respectively, and the KY and the WPF are mixed with the simulated water to obtain the IPN gel prepolymer. The prepolymer was then sealed in an ampoule and stored in a 140 ℃ high temperature oven for heating. In the IPN prepolymer, the KY ratio was 0.5%, the WPF ratio was 3%, and the remainder was simulated water.
Gel time was 10 hours and gel strength was determined to be H-scale by code method.
Example 3 preparation of temperature and salt resistant IPN gel blocking agent 3#
(1) Preparation of KY polymers
Weighing quantitative monomers to prepare 25% aqueous solution, stirring until the monomers are completely dissolved, introducing nitrogen and discharging oxygen for 30 minutes, heating to 30 ℃ and adding an initiator; after polymerizing at constant temperature for 2 hours, the polymer colloid was taken out, precipitated with absolute ethanol and washed with pure water to remove unreacted monomers, and the polymer sample was dried under vacuum at 70 ℃ for 6 hours to constant weight to obtain KY white solid powder. The monomer composition is as follows: acrylamide: 30%; acrylic acid 10%; AMPS:56% of a glass fiber; NVP:3%; MJ-16:1% of initiator, namely ammonium persulfate-sodium bisulfite with the monomer content of 0.02%. The molecular weight of the KY polymer prepared was 1350 ten thousand.
(2) Preparation of WPF
Weighing quantitative catechol in a three-neck flask, and stirring at 50 ℃; weighing a certain amount of sodium hydroxide, dissolving in water, preparing a 20% alkali solution, adding the alkali solution into a reaction system, and stirring and reacting for 20min at 50 ℃. Adding urotropine into the constant pressure dropping funnel, heating to 90 ℃, and reacting for 60min at constant temperature. A bright reddish brown transparent liquid product was obtained. Wherein the proportion of catechol to urotropine is 1.5, and potassium hydroxide accounts for 3 percent of the mass of phenol;
(3) Preparation of IPN gel
KY and WPF in certain proportion are prepared into water solution by using simulated water with the mineralization degree of 22 ten thousand respectively, and the KY and the WPF are mixed with the simulated water to obtain the IPN gel prepolymer. The prepolymer was then sealed in an ampoule and stored in a 140 ℃ high temperature oven for heating. In the IPN prepolymer, the KY ratio was 1.5%, the WPF ratio was 8%, and the remainder was simulated water.
Gel time was 6 hours and gel strength was determined as grade I by code.
(4) Structural characterization of IPN gels
Structural characterization of dry powder samples of IPN gel was performed using fourier transform infrared spectroscopy, the results are shown in fig. 1: stretching vibration belonging to O-H or N-H at 3423cm -1, asymmetric stretching vibration belonging to C-H 2 or stretching vibration of O-H at 2922cm -1; 2305cm -1 and 1634cm -1 are the triple bond and cumulative double bond stretching vibration region, and 1470cm -1 are the saturated C-H in-plane bending vibration region on the main chain. Stretching vibration of C-O in C-OH at 1121cm -1, 1143cm -1 and 1021cm -1, and out-of-plane bending vibration of C-H on benzene ring at 872cm -1 and 774cm -1. In summary, it was confirmed that the IPN gel contains an amide group, a carboxylic acid group, a sulfonic acid group, a benzene ring, and a phenolic hydroxyl group.
Example 4 preparation of temperature and salt resistant IPN gel blocking agent 4#
Unlike example 3, the KY ratio in step (3) was 2%, the WPF ratio was 9%, and the remainder was simulated water.
Example 5 preparation of temperature and salt resistant IPN gel blocking agent 5#
The difference from example 3 is that the monomer composition in step (1) is: acrylamide: 50%; acrylic acid 22%; AMPS:25%; NVP:1%; MJ-16:2%.
Example 6 preparation of temperature and salt resistant IPN gel blocking agent 6#
Unlike example 3, the initiator in step (1) was ammonium persulfate-sodium bisulfite having a monomer content of 0.1%.
Experimental example
Performing a water shutoff experiment on the 1-6# gel plugging agent by using an artificial fracture core model with a fracture width of 2mm, wherein various water shutoff indexes are shown in table 1; the pressure curves of the gel blocking agents 1-3# are also shown in figures 2-4.
TABLE 1
| Scheme numbering | Sample numbering | Gel strength | Highest plugging pressure/MPa | Water shutoff rate | Oil plugging rate |
| Example 1 | 1# | Low strength | 0.030 | 98.33％ | 12.23％ |
| Example 2 | 2# | Medium strength | 0.064 | 99.22％ | 18.78％ |
| Example 3 | 3# | Higher strength of | 0.335 | 99.88％ | 24.03％ |
| Example 4 | 4# | Higher strength of | 0.411 | 99.94％ | 27.47％ |
| Example 5 | 5# | Higher strength of | 0.209 | 99.35％ | 20.15％ |
| Example 6 | 6# | Low strength | 0.106 | 98.53％ | 15.02％ |
Finally, it should be noted that the above description is only for illustrating the technical solution of the present invention, and not for limiting the scope of the present invention, and that the simple modification and equivalent substitution of the technical solution of the present invention can be made by those skilled in the art without departing from the spirit and scope of the technical solution of the present invention.
Claims (10)
1. The preparation method of the IPN gel plugging agent is characterized by comprising the following steps:
(1) Preparation of a water-soluble polymer: dissolving monomers in water to prepare a monomer aqueous solution, introducing nitrogen, heating to 20-70 ℃, adding an initiator, polymerizing for 1.5-2.5 hours at constant temperature, taking out a polymer colloid, precipitating with absolute ethyl alcohol, washing with pure water, and vacuum drying to prepare a water-soluble polymer;
(2) Preparing water-soluble phenolic resin: mixing phenolic substances with alkaline aqueous solution, stirring and reacting for 15-25min at 45-55 ℃, adding aldehyde substances, heating to 85-95 ℃, and reacting at constant temperature for 25-35min to obtain water-soluble phenolic resin;
(3) Preparing an IPN gel plugging agent: and (3) dissolving the water-soluble polymer obtained in the step (1) and the water-soluble phenolic resin obtained in the step (2) in simulated water to obtain an IPN gel prepolymer, and heating and drying the IPN gel prepolymer to obtain the IPN gel plugging agent.
2. The preparation method according to claim 1, wherein the monomer in the step (1) is one or more of acrylamide, acrylic acid, 2-acrylamide-2-methylpropanesulfonic acid, N-vinyl pyrrolidone and hydrophobic monomer.
3. The preparation method according to claim 2, wherein the weight ratio of the acrylamide, the acrylic acid, the 2-acrylamide-2-methylpropanesulfonic acid, the N-vinyl pyrrolidone and the hydrophobic monomer is 10-50:10-20:10-60:1-5:0.5-3, preferably 30-48:10-20:30-56:1-3:1.
4. The method according to claim 1, wherein the initiator in the step (1) is one or more of ammonium persulfate, potassium persulfate, ammonium persulfate-sodium bisulfite, 2' -azobisisobutylamidine dihydrochloride.
5. The process of claim 1, wherein the weight ratio of monomer to initiator in step (1) is 100:0.01-0.1, preferably 100:0.02-0.05, the mass percent of the monomer in the monomer aqueous solution is 15-25%, preferably 20-25%.
6. The preparation method of claim 1, wherein in the step (2), the phenolic substance is one or more of phenol, resorcinol and catechol, the alkaline substance in the alkaline aqueous solution is one or two of sodium hydroxide and potassium hydroxide, and the aldehyde substance is one or more of formaldehyde, acetaldehyde and urotropine.
7. The method according to claim 6, wherein the weight ratio of the phenolic substance to the aldehyde substance in the step (2) is 1.1 to 3.0:1, wherein the alkaline substance accounts for 5-10% of the phenolic substance by mass.
8. The method according to claim 1, wherein the weight ratio of the water-soluble polymer, the water-soluble phenol resin, and the simulated water in the step (3) is 0.1 to 2:1.5-10:88-98.4.
9. The IPN gel blocking agent obtained by the method of any one of claims 1-8.
10. The use of an IPN gel plugging agent obtained by the preparation method of any one of claims 1-8 or the IPN gel plugging agent of claim 9 in plugging water of a reservoir.
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