CN113265026A - Water-swelling rubber flexible temporary plugging particle and preparation method thereof - Google Patents
Water-swelling rubber flexible temporary plugging particle and preparation method thereof Download PDFInfo
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- CN113265026A CN113265026A CN202110564194.8A CN202110564194A CN113265026A CN 113265026 A CN113265026 A CN 113265026A CN 202110564194 A CN202110564194 A CN 202110564194A CN 113265026 A CN113265026 A CN 113265026A
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- 239000002245 particle Substances 0.000 title claims abstract description 43
- 229920001971 elastomer Polymers 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 54
- RRHGJUQNOFWUDK-UHFFFAOYSA-N Isoprene Chemical compound CC(=C)C=C RRHGJUQNOFWUDK-UHFFFAOYSA-N 0.000 claims abstract description 20
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000003999 initiator Substances 0.000 claims abstract description 13
- 229910000278 bentonite Inorganic materials 0.000 claims abstract description 11
- 239000000440 bentonite Substances 0.000 claims abstract description 11
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000003292 glue Substances 0.000 claims abstract description 10
- 239000000126 substance Substances 0.000 claims abstract description 9
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 8
- 239000000178 monomer Substances 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 5
- 239000003054 catalyst Substances 0.000 claims abstract description 3
- 239000007787 solid Substances 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 10
- 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
- 239000000047 product Substances 0.000 claims description 7
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 5
- 238000005520 cutting process Methods 0.000 claims description 5
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 claims description 5
- OMNKZBIFPJNNIO-UHFFFAOYSA-N n-(2-methyl-4-oxopentan-2-yl)prop-2-enamide Chemical compound CC(=O)CC(C)(C)NC(=O)C=C OMNKZBIFPJNNIO-UHFFFAOYSA-N 0.000 claims description 5
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 5
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims description 5
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 4
- AATHLPHPRXGBAI-UHFFFAOYSA-M sodium;4-ethenylbenzenesulfonate;hydrate Chemical compound O.[Na+].[O-]S(=O)(=O)C1=CC=C(C=C)C=C1 AATHLPHPRXGBAI-UHFFFAOYSA-M 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims description 3
- 235000019345 sodium thiosulphate Nutrition 0.000 claims description 3
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 2
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- 239000007795 chemical reaction product Substances 0.000 claims description 2
- HMZGPNHSPWNGEP-UHFFFAOYSA-N octadecyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)C(C)=C HMZGPNHSPWNGEP-UHFFFAOYSA-N 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- 230000015556 catabolic process Effects 0.000 abstract description 9
- 238000006731 degradation reaction Methods 0.000 abstract description 9
- 238000007789 sealing Methods 0.000 abstract description 8
- 230000015784 hyperosmotic salinity response Effects 0.000 abstract description 3
- 239000003795 chemical substances by application Substances 0.000 description 17
- 206010042674 Swelling Diseases 0.000 description 14
- 238000010521 absorption reaction Methods 0.000 description 12
- 230000033558 biomineral tissue development Effects 0.000 description 8
- 230000000903 blocking effect Effects 0.000 description 6
- 239000003921 oil Substances 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 239000002253 acid Substances 0.000 description 5
- 239000012530 fluid Substances 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 238000013508 migration Methods 0.000 description 4
- 230000020477 pH reduction Effects 0.000 description 4
- 238000010298 pulverizing process Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 230000032683 aging Effects 0.000 description 3
- 238000004132 cross linking Methods 0.000 description 3
- 238000001723 curing Methods 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000008187 granular material Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000000643 oven drying Methods 0.000 description 3
- 238000002604 ultrasonography Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
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- 239000000835 fiber Substances 0.000 description 2
- 239000006260 foam Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000005012 migration Effects 0.000 description 2
- 239000003129 oil well Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
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- 229910052760 oxygen Inorganic materials 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
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- 230000008961 swelling Effects 0.000 description 2
- 239000008399 tap water Substances 0.000 description 2
- 235000020679 tap water Nutrition 0.000 description 2
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000008398 formation water Substances 0.000 description 1
- 238000005098 hot rolling Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000004816 latex Substances 0.000 description 1
- 229920000126 latex Polymers 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- -1 sodium carboxylate Chemical class 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 1
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- 238000006467 substitution reaction Methods 0.000 description 1
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F253/00—Macromolecular compounds obtained by polymerising monomers on to natural rubbers or derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/346—Clay
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/50—Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls
- C09K8/516—Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls characterised by their form or by the form of their components, e.g. encapsulated material
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Abstract
The invention provides water-swelling rubber flexible temporary plugging particles, which are prepared by the following method: dissolving acrylamide, bentonite and functional monomers in water; adding the solution into natural latex, and curing at 45-50 ℃ for 2 h; adding an initiator and a cross-linking agent, and sealing and reacting for 4-5h at 45-50 ℃ to form gel; drying and crushing a product after reaction to obtain the catalyst; the adding amount of each substance is as follows by mass percent: 10-15% acrylamide; 2.5-5% of bentonite; 9.6-12.6% of natural latex by mass of dry glue; 10% of acrylamide and natural latex dry glue mass; 0.28-0.33% of cross-linking agent based on the sum of the mass of acrylamide and natural latex dry glue; 0.22-0.39% of the sum of the dry mass of acrylamide and natural latex; total solid content 28-32%, and water in balance. The water-swelling rubber flexible temporary plugging particles have controllable particle size and can be adjusted according to the requirement of the entering depth; the residue rate after degradation is lower than 3 percent, and the residue is easy to flow back; and has certain temperature resistance and salt tolerance.
Description
Technical Field
The invention belongs to the technical field of oilfield chemistry, and particularly relates to water-swelling rubber flexible temporary plugging particles and a method for preparing the temporary plugging particles.
Background
As the development of oil and gas fields enters the middle and later stages, because of the heterogeneity of the stratum, oil and gas in a high-permeability reservoir are preferentially exploited, and how to improve the crude oil recovery rate of a low-permeability reservoir is always a research hotspot. The fracturing fluid and the acid liquid can preferentially enter the high-permeability layer to improve the physical property of the high-permeability layer, the low-permeability layer is not effectively improved, and the water content of the oil well is greatly increased while the oil is increased. Therefore, the key point for solving the problems is to control the diversion and diversion of the fracturing fluid and the acid liquid to enter a hypotonic reservoir for treatment. In addition, for a compact reservoir stratum and a thicker reservoir stratum, manual temporary plugging is often needed to force fracturing fluid to change the reservoir stratum in a diverting way, and a complex fracture network is manufactured to enlarge the oil drainage area of an oil well and improve the recovery ratio. Compared with mechanical temporary plugging, chemical temporary plugging has lower risk under complex well conditions and higher construction success rate and reservoir transformation effectiveness, so the chemical temporary plugging has better application effect in the working fluid diversion technology.
The chemical temporary plugging technology is widely applied to temporary plugging acidification, repeated fracturing and temporary plugging acid fracturing. The temporary plugging acidification can achieve the purpose of uniform acidification, the rapid increase of the water content in the well is avoided, and after the acidification is finished, the temporary plugging agent can be rapidly degraded without polluting the stratum; during repeated fracturing and temporary plugging of acid fracturing, the temporary plugging agent can hold the static pressure in the fracture to open a new fracture, after fracturing, the temporary plugging agent is dissolved in formation water, and the plugged fracture is unobstructed again. The chemical temporary plugging agent can be divided into acid solubility, water solubility and oil solubility according to the dissolution characteristics; according to the form, the temporary plugging agent can be divided into a fiber temporary plugging agent, a particle temporary plugging agent, a polymer cross-linking temporary plugging agent, a water-absorbing expansion type temporary plugging agent, a foam temporary plugging agent and the like. The fiber temporary plugging agent has low strength, low density and easy dispersion; the polymer crosslinking temporary plugging agent has more residues after being degraded, and the crosslinking process is easily influenced by the PH value and the temperature; the foam type plugging agent has poor high-temperature stability and high cost; the water-absorbing expansion type temporary plugging agent has elasticity, low plugging strength, low cost and good temperature and pressure resistance.
The water-swelling flexible temporary plugging particles have flexibility and variability, controllable particle size, temperature resistance and salt tolerance, low cost and good development prospect, and can enter the deep part of a stratum.
Disclosure of Invention
In order to solve the problems, the invention provides the water-swelling rubber flexible temporary plugging particles, the particle size of the water-swelling rubber flexible temporary plugging particles is controllable, the particles can be adjusted according to the requirement of the entering depth, meanwhile, the particles can be degraded, the residue rate after the explanation is low, the particles are easy to flow back, and meanwhile, the reservoir stratum cannot be polluted.
The technical scheme of the invention is as follows: a method for preparing water-swellable rubber flexible temporary plugging particles, comprising the following steps:
1) dissolving or dispersing acrylamide, bentonite and functional monomers in water;
2) adding the solution obtained in the step 1) into natural latex, uniformly stirring, and curing for 2 hours at the temperature of 45-50 ℃;
3) adding an initiator and a cross-linking agent, uniformly stirring, and sealing and reacting for 4-5h at 45-50 ℃ to form gel;
4) drying and crushing a product after reaction to obtain the catalyst;
in the above steps, the addition of each substance is as follows by mass percent: 10-15% acrylamide; 2.5-5% of bentonite; 9.6-12.6% of natural latex by mass of dry glue; 10% of acrylamide and natural latex dry glue mass; 0.28-0.33% of cross-linking agent based on the sum of the mass of acrylamide and natural latex dry glue; 0.22-0.39% of the sum of the dry mass of acrylamide and natural latex; total solid content 28-32%, and water in balance.
One embodiment of the invention is that the functional monomer is one or a mixture of any two of diacetone acrylamide, sodium p-styrene sulfonate hydrate, methyl methacrylate and octadecyl methacrylate.
One embodiment of the invention is that the crosslinking agent is one or two of N' N-methylene bisacrylamide and polyethylene glycol.
One embodiment of the invention is that the initiator consists of a first initiator and a second initiator in a mass ratio of 1:1, wherein the first initiator is one of potassium persulfate or ammonium persulfate, and the second initiator is one of sodium bisulfite or sodium thiosulfate.
One embodiment of the present invention is that, in the step 3), the reaction is performed to form a gel under a closed condition.
One embodiment of the present invention is that the specific operation of step 4) is: cutting the reaction product into small rubber blocks, drying at 90 ℃, and crushing to obtain the product.
Another object of the present invention is to provide water-swellable rubber flexible temporary plugging particles prepared by the method of any one of the above.
In the present invention, in order to make the produced product as uniform as possible, the product located at the top is prevented from moisture loss due to frequent air flow, and thus it is necessary to react it in a sealed state.
In the invention, a rubber molecular chain and a monomer chain are mutually wound, a hydrophilic group firstly adsorbs combined water, and a cross-linked network then binds free water, so that expansion is generated, and blocking is realized. After the temporary plugging agent expanded by water absorption is separated from a water environment, bound free water in a cross-linked network is evaporated in advance, and bound water adsorbed by water absorption groups is not easy to separate and has certain water retention. A small amount of bentonite is added to bring a large amount of hydroxyl (-OH), carboxyl (-COOH) and sodium carboxylate (-COONa), and a plurality of active points exist, when water exists, compensation ions between crystal layers are easily exchanged by other cations in the solution, wherein variable charges and exchangeable cations can enhance the salt resistance of the temporary plugging particles.
The water absorption process of the water-absorbing expansion type temporary plugging agent is divided into two stages: in the first stage, in the initial stage of water absorption, water molecules enter the interior through surface adsorption, capillary action, diffusion and the like, hydrophilic groups are combined with the water molecules through coordination bonds or hydrogen bonds, bound water is connected with the combined water through the hydrogen bonds or orientation force, a cross-linked network rapidly expands, and rubber undergoes expansion deformation; the water seepage or water absorption of the second stage is caused by the adjustment of network conformation, the expanded macromolecular network comprises a crosslinked network of water absorption components and a rubber network structure, and the adjustment of the conformation cannot keep up with the expansion rate, so the rate is slower. The rubber in the first stage can still maintain certain mechanical property, and in the second stage, due to continuous and large amount of water molecules, the network is gradually destroyed, so that the mechanical property is reduced until the rubber starts to be gradually degraded.
The flexible temporary plugging particles of the water-swellable rubber have degradation performance, and the research of the inventor shows that the preparation method does not remove oxygen in the preparation process, the rubber is in contact with oxygen in the synthesis process and is subjected to thermal oxidation, and in the aging process of the rubber, the heat in the stratum promotes the oxidation of the rubber particles, further aggravates the reduction of the mechanical property of the rubber particles, and finally promotes the degradation of the flexible temporary plugging particles of the water-swellable rubber.
The invention has the beneficial effects that:
the low-ammonia type concentrated natural latex used in the invention has small surface skinning tendency and relatively small rubber loss, and the water-absorbing expansion rubber prepared by the chemical grafting method has excellent water absorption performance and viscoelasticity. The synthesized water-swelling rubber flexible temporary plugging particles have controllable particle size and can be adjusted according to the requirement of the entering depth; the modes of migration, plugging, elastic deformation, re-migration and re-plugging can be realized in the formation pores; meanwhile, the material can be naturally degraded at 70-150 ℃, the residue rate after degradation is lower than 3%, and the material is easy to flow back; and has certain temperature resistance and salt tolerance, and is suitable for the temporary plugging process of water plugging profile control or fracture network fracturing of the heterogeneous oil reservoir.
Drawings
FIG. 1 shows the water absorption times of the water-swellable flexible temporary plugging particles of the present invention at 70 deg.C, 90 deg.C, 125 deg.C and 150 deg.C, respectively.
Fig. 2 is the expansion times of the water-swelling flexible temporary plugging particles in water with mineralization degrees of 10 ten thousand, 15 ten thousand, 20 ten thousand and 25 ten thousand at 125 ℃.
FIG. 3 shows the comparison effect before and after centrifugation of the water-swellable flexible temporary plugging particles of the present invention after degradation.
Detailed Description
In order to make the technical solutions and technical advantages of the present invention clearer, the following will clearly and completely describe the technical solutions in the implementation process of the present invention with reference to the embodiments and the accompanying drawings.
Materials and drugs used in the examples: natural latex (low ammonia type latex, dry glue content 60.12%, majestic sources majestic limited);
acrylamide, diacetone acrylamide, sodium p-styrene sulfonate hydrate, potassium persulfate, ammonium persulfate, sodium bisulfite, sodium chloride (Doctorong Chemicals, Inc., Doctoryon, N.C.);
bentonite (processing plant for Shuolong mineral products in Lingshu county).
Example 1
In this example, the water-swellable rubber flexible temporary plugging particles were prepared by the following steps:
(1) dissolving 10g of acrylamide, 4g of bentonite and 1.8g of diacetone acrylamide in 50g of deionized water by using ultrasound in sequence;
(2) adding the aqueous solution prepared in the step (1) into 16.63g of concentrated natural latex, uniformly stirring, sealing, and curing in a 45 ℃ constant-temperature water bath kettle for 2 hours;
(3) adding 0.035g potassium persulfate, 0.035g sodium bisulfite and 0.06g N' N-methylene bisacrylamide, stirring uniformly, sealing and reacting at 45 ℃ for 4.5h to form gel;
(4) cutting into pieces of about 1cm × 1cm × 1cm with scissors, oven drying in a 90 deg.C oven, and pulverizing with a pulverizer.
Example 2
In this example, the water-swellable rubber flexible temporary plugging particles were prepared by the following steps:
(1) dissolving 10g of acrylamide, 4g of bentonite and 1.8g of sodium p-styrenesulfonate hydrate in 50g of deionized water by using ultrasound in sequence;
(2) adding the aqueous solution prepared in the step (1) into 16.63g of concentrated natural latex, uniformly stirring, sealing, and curing in a 45 ℃ constant-temperature water bath kettle for 2 hours;
(3) adding 0.035g potassium persulfate, 0.035g sodium bisulfite and 0.06g N' N-methylene bisacrylamide, stirring uniformly, sealing and reacting at 45 ℃ for 4.5h to form gel;
(4) cutting into pieces of about 1cm × 1cm × 1cm with scissors, oven drying in a 90 deg.C oven, and pulverizing with a pulverizer.
Example 3
In this example, the water-swellable rubber flexible temporary plugging particles were prepared by the following steps:
(1) dissolving 10g of acrylamide, 4g of bentonite and 1.8g of diacetone acrylamide in 50g of deionized water by using ultrasound in sequence;
(2) adding into 16.63g of concentrated natural latex, stirring, sealing, and aging in a 45 deg.C constant temperature water bath kettle for 2 hr;
(3) adding 0.035g ammonium persulfate, 0.035g sodium thiosulfate and 0.06g N' N-methylene bisacrylamide, stirring uniformly, and sealing and reacting at 45 ℃ for 4.5h to form gel;
(4) cutting into pieces of about 1cm × 1cm × 1cm with scissors, oven drying in a 90 deg.C oven, and pulverizing with a pulverizer.
The effect of the water-swellable rubber flexible temporary blocking particles prepared in the above examples is further illustrated by the following method.
Preparing the mixture with the degree of mineralization of 10 multiplied by 104mg/L、15×104mg/L、20×104mg/L、25×104mg/L NaCl water is used for standby.
1. Water-swelling property of water-swelling rubber flexible temporary blocking particles
The dried flexible particles of example 1 were put into an aging tank, an appropriate amount of tap water was added, hot-rolled at 70 ℃, 90 ℃, 125 ℃ and 150 ℃ for 48 hours, respectively, taken out at intervals, excess water on the surface was removed by suction, and the water-swelling factor was measured.
After 48 hours, the expansion times at 70 ℃, 90 ℃, 125 ℃ and 150 ℃ are respectively 15.1 times, 18.9 times, 30.46 times and 37.26 times, and the higher the temperature is, the faster the expansion is, and the earlier the water absorption balance is reached. As can be seen in fig. 1, the initial 9h expansion rate was fast and after 9h the expansion rate gradually slowed down. In the first stage of the temporary blocking particle water absorption process, water molecules enter the inside through surface adsorption, capillary action, diffusion and the like, hydrophilic groups are combined with the water molecules through coordination bonds or hydrogen bonds, bound water is connected with the combined water through the hydrogen bonds or orientation force, a cross-linked network rapidly expands, and rubber undergoes expansion deformation; the conformation of the macromolecular network after the second stage of swelling does not follow the rate of swelling and is therefore slower than in the first stage.
Respectively placing the dried flexible particles into 10 × 10 at 125 deg.C4mg/L、15×104mg/L、20×104mg/L、25×104And (3) hot rolling the water with the mineralization degree of mg/L for 48 hours, taking out the water at intervals, sucking excess water on the surface, and measuring the water absorption expansion times of the water.
After 48 hours, 10X 104mg/L、15×104mg/L、20×104mg/L、25×104The expansion times of the water-absorbing expansion rubber in the water with the mineralization of mg/L are respectively 12.45 times, 12 times, 11.17 times and 10.75 times, as shown in figure 2, the higher the mineralization is, the slower the expansion rate is, and the expansion time can still reach more than 10 times under the high mineralization.
2. Flexibility of water-swelling rubber flexible temporary blocking particles
The water-swellable rubber reacted to gel in example 1 was cut into pieces of 1cm × 0.2cm × 0.2cm with scissors, and the maximum stretchability was measured to be 4.5 times and reached grade E; the dried rubber block can be stretched by 3.24 times at most after absorbing water and expanding for 24 hours again, and still can reach above D level, and the synthesized water-absorbing expansion temporary plugging particles have better flexibility, can deform in the stratum according to the sizes of pores, and realize the modes of migration, plugging, elastic deformation, re-migration and re-plugging, thereby achieving the purpose of penetrating into the stratum.
3. Degradation performance of water-swelling rubber flexible temporary plugging particles
The dried gum blocks in example 1 were pulverized into particles of 20-60 mesh by a pulverizer,placing the granules in tap water at 125 ℃ for water absorption and expansion, and completely degrading the granules after 60 hours; pulverizing the dried gel block into 20-60 mesh granules, and standing at 125 deg.C for 15 × 104The water with the mineralization degree of mg/L absorbs water to swell, and is completely degraded within 110 hours. And (3) centrifuging the degraded liquid at 3500 rpm for 30 minutes (the centrifugation result is shown in figure 3), weighing the residue at the lower part, wherein the residue rate is less than 3%, and the degradation rate is more than 97%, so that the temporary plugging agent can be basically and completely degraded after temporary plugging is realized in the stratum, does not pollute the stratum and is easy to flow back.
In fact, the water-swellable rubber flexible temporary blocking particles prepared in the above examples are degradable at 70-150 ℃ and follow the following law: the lower the temperature, the slower the degradation speed; the higher the degree of mineralization, the slower the rate of degradation.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (7)
1. A method for preparing water-swellable rubber flexible temporary plugging particles is characterized by comprising the following steps:
1) dissolving or dispersing acrylamide, bentonite and functional monomers in water;
2) adding the solution obtained in the step 1) into natural latex, uniformly stirring, and curing for 2 hours at the temperature of 45-50 ℃;
3) adding an initiator and a cross-linking agent, uniformly stirring, and reacting for 4-5h at 45-50 ℃ to form gel;
4) drying and crushing a product after reaction to obtain the catalyst;
in the above steps, the addition of each substance is as follows by mass percent: 10-15% acrylamide; 2.5-5% of bentonite; 9.6-12.6% of natural latex by mass of dry glue; 10% of acrylamide and natural latex dry glue mass; 0.28-0.33% of cross-linking agent based on the sum of the mass of acrylamide and natural latex dry glue; 0.22-0.39% of the sum of the dry mass of acrylamide and natural latex; total solid content 28-32%, and water in balance.
2. The method according to claim 1, wherein the functional monomer is one or a mixture of any two of diacetone acrylamide, sodium p-styrene sulfonate hydrate, methyl methacrylate and octadecyl methacrylate.
3. The method according to claim 1, wherein the cross-linking agent is one or both of N' N-methylene bisacrylamide and polyethylene glycol.
4. The method according to claim 1, wherein the initiator consists of a first initiator and a second initiator in a mass ratio of 1:1, the first initiator is one of potassium persulfate or ammonium persulfate, and the second initiator is one of sodium bisulfite or sodium thiosulfate.
5. The method as claimed in claim 1, wherein in the step 3), the whole reaction is carried out under a closed condition.
6. The method according to claim 1, wherein the specific operation of step 4) is: cutting the reaction product into small rubber blocks, drying at 90 ℃, and crushing to obtain the product.
7. A water-swellable rubber flexible temporary plugging particle characterized by being prepared by the method of any one of claims 1 to 6.
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