CN113736438B - Pressure-bearing degradable temporary plugging agent for well repair and preparation method and application thereof - Google Patents
Pressure-bearing degradable temporary plugging agent for well repair and preparation method and application thereof Download PDFInfo
- Publication number
- CN113736438B CN113736438B CN202111035970.1A CN202111035970A CN113736438B CN 113736438 B CN113736438 B CN 113736438B CN 202111035970 A CN202111035970 A CN 202111035970A CN 113736438 B CN113736438 B CN 113736438B
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- Prior art keywords
- temporary plugging
- agent
- plugging agent
- parts
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- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/50—Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls
- C09K8/501—Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls using spacer compositions
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- C08F112/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F112/02—Monomers containing only one unsaturated aliphatic radical
- C08F112/04—Monomers containing only one unsaturated aliphatic radical containing one ring
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Abstract
The invention relates to a pressure-bearing degradable temporary plugging agent for well repair, a preparation method and application thereof, wherein the temporary plugging agent comprises acrylamide, alpha-phenyl acrylic acid prepolymer, sulfur modified petroleum resin, polypropylene fiber, inorganic reinforcing agent, composite cross-linking agent, initiator and deionized water; the temporary plugging agent has various good performances through the mutual combination and cooperation of a plurality of technical characteristics and a unique preparation method, and has good industrialization potential and popularization value in the technical field of oil exploitation.
Description
Technical Field
The invention relates to a pressure-bearing degradable temporary plugging agent with self-degradation performance for repairing a well, which is used for improving the plugging effect in the exploitation and development of an oil field, and a preparation method and application thereof, and belongs to the technical field of oil exploitation auxiliary agents.
Background
In the field of oil exploitation, the length of a horizontal well section is usually hundreds of meters, for example, the horizontal well section is usually 200-600 meters, and due to many reasons such as production length and reservoir heterogeneity, various problems such as uneven profile of produced fluid, local breakthrough of bottom water or injected water, and too fast rising of water content are easily caused, so that the efficiency and effect of oil exploitation are seriously affected (the most common expression is that the water content in the oil to be exploited is more and more large, and can even reach as high as 90%). In order to solve the problem, the water outlet section is blocked, so that the water outlet can be effectively inhibited, the liquid production profile is balanced, and the potential position which is not used is started, thereby integrally improving the development benefit and the petroleum extraction rate of the high-level well.
The water outlet section can be blocked by adopting a segmented directional blocking method by means of mechanical means, but the method needs severe conditions, such as requirements of good well conditions, tools and the like, and the operation difficulty is high. The general plugging can realize immobile pipe column and direct injection, has the advantages of simple process, low operation difficulty and the like, but the process generally needs low-displacement injection, and the stratum plugging agent inevitably enters a potential section, thereby damaging a reservoir stratum. Besides the two plugging methods, the auxiliary temporary plugging method is one of effective means for reducing reservoir damage and improving the plugging effect.
Generally, the implementation operation of the auxiliary temporary blocking method is: before injecting the high-strength stratum plugging agent to plug the high-permeability water outlet section, the temporary plugging agent is injected firstly, and the temporary plugging agent entering the relatively low-permeability potential section forms temporary plugging on the end face of the oil-containing part, so that the high-strength stratum plugging agent injected subsequently enters the relatively high-permeability water outlet section. After the injection of the high-strength stratum plugging agent is finished, the temporary plugging agent which is injected firstly and forms temporary plugging is gradually degraded, so that the hypotonic potential section is recovered to the initial state, and the subsequent development and exploitation of the potential section are not influenced.
The currently applied temporary plugging agents mainly comprise: organic resin, inert solid (such as oil soluble resin, blocking microsphere) and the like. Among the most widely used are organic resins and/or blocked microspheres. The temporary plugging agent of organic resin polymer has good plugging effect due to the firm chemical cross-linked network structure, but has slow degradation speed, thereby causing certain damage to the oil layer of the potential section. The temporary plugging agent of the plugging microsphere polymer has the characteristics of high plugging strength, small deformation and the like, but has the defect of uncontrollable degradation time.
Therefore, in order to develop a novel temporary plugging agent, a great deal of intensive research is carried out, and a plurality of types of temporary plugging agents with different formulations and different components are obtained, such as:
CN101311243A discloses a fracture temporary plugging agent for fractured hydrocarbon reservoirs. The components are mixed according to the following proportion: 40-85% of 60-1100 mesh superfine calcium carbonate, 10-40% of plant fiber and 5-20% of oxidized asphalt. After the temporary plugging agent enters a stratum along with drilling well fluid, a layer of compact and tough mud cake is quickly formed near a well wall, so that the original permeability of the stratum near the well wall is quickly reduced to be close to zero, and the reduction of oil and gas yield and the reduction of productivity caused by the invasion of drilling fluid filtrate, various treating agents, rock debris and the like in the drilling process are prevented. The temporary plugging agent has a temporary plugging rate of more than 99% on a fractured rock core, a pressure flowback rate and an acidification flowback rate of more than 80%, and a wide temporary plugging range, and is an ideal fractured reservoir protection agent.
CN 101818052A discloses a temporary plugging agent for drilling fluid, which is a polymer prepared from the following raw materials by weight percent: 60-70% of hexadecene, 0.5-1% of catalyst persulfate, 10-20% of phenol, 10-20% of formaldehyde and 1-2% of cationic surfactant. The softening point temperature range of the temporary plugging agent is wide and can almost meet the requirements of all stratums at 70-140 ℃.
CN 102559162A discloses a low-pressure thin oil well leakage-proof temporary plugging agent, which comprises the following raw materials in percentage by weight: 0.4 to 0.6 percent of hydroxypropyl guar gum, 0.2 to 0.4 percent of organic titanium, 5 to 10 percent of petroleum resin, 0.3 to 0.5 percent of dodecyl dimethyl betaine, 0.1 percent of sodium sulfite, 0.02 to 0.04 percent of ammonium persulfate and 88.5 to 93.5 percent of water. The hydroxypropyl guar gum and the organic titanium are crosslinked to form a gel system, and a certain amount of petroleum resin is added to form a composite temporary plugging system, so that the temporary plugging system can break the gel immediately, an oil well cannot be plugged, broken gel fragments cannot cause pump blockage accidents, and the temporary plugging system has the advantages of no pollution, no damage to a reservoir and low cost.
CN 102604627A discloses an acid fracturing temporary plugging agent, which is prepared by combining resin, ozokerite, calcium carbonate, magnesium carbonate, potassium chloride and ammonium chloride, is suitable for stratum temperature of 100 ℃, has a plugging rate of more than 96 percent, an acid dissolution rate of more than 98 percent and a temporary plugging strength of more than 50Mpa, can effectively meet acid fracturing temporary plugging diversion of a long well section of a carbonate reservoir, and improves the acid fracturing construction success rate of the long well section.
CN 103087694A discloses a Microsoft particle oil-soluble temporary plugging agent, which consists of water, carboxymethyl modified cellulose, low-viscosity PAC, linear paraffin oil, linear alkyl polyoxyethylene ether, glycerol and calcareous soil in parts by weight. The temporary plugging agent utilizes functional groups of the temporary plugging agent to enable drilling fluid to generate a molecular film (isolating film) on a well wall, and simultaneously oil-soluble and water-dispersible particles can form shielding temporary plugging on the well wall under a certain pressure difference in a shaft, so that two oil layer protection technologies are organically combined, a firm protective layer is formed on the periphery of the well wall, filtrate and the drilling fluid are prevented from entering a stratum, the stratum is effectively prevented from being hydrated and expanded, stratum bedding cracks are plugged, the migration of clay particles in the stratum is prevented, the problem of poor plugging effect caused by unmatched stratum temperature and product softening points is effectively solved, and the damage of drilling construction operation to oil and gas layers is further reduced.
CN 104419392A discloses a temporary plugging while drilling agent for drilling fluid, which comprises the following raw materials by weight percent: 20-35% of animal and plant fibers, 40-60% of phosphogypsum, 5-20% of triple superphosphate, 1-25% of hydroxymethyl fibers and 1.5-2% of adhesive. In the drilling process, the mud slurry is added according to the measurement of the ratio of 5 per mill to the liquid level which is reduced by 1 percent while drilling, the leakage point is blocked, and the mud slurry is discharged in the well washing operation after the drilling is finished. The temporary plugging agent uses phosphogypsum as a base material, so that the salinization of soil by mud liquid in a reverse discharge environment in the well completion process is effectively improved.
CN 104449613A discloses a water-absorbent resin temporary plugging agent and a preparation method thereof, which is prepared from an acrylic monomer A, an acrylamide monomer B, a powdery acid-soluble inorganic filling material C and a cross-linking agent by aqueous solution polymerization and initiation of an oxidation-reduction initiation system, and the obtained gel product is granulated and dried to obtain the water-absorbent resin temporary plugging agent for drilling fluid. The acid solubility of the temporary plugging agent in 15% hydrochloric acid can reach more than 85%, the temporary plugging agent can resist the temperature of 150 ℃ and has the saturation water absorption multiple of 5-8 times, and the temporary plugging agent has good self-adaptive capacity for leakage channels with different shapes and sizes, the tensile elongation of 800-1200% and the tensile breaking strength of more than 2 MPa. The plugging agent is suitable for plugging in the drilling and completion process, particularly the drilling and completion process of a reservoir, and plugging of leaking layers with different well depths under the condition of high salinity.
CN 104479655A discloses a high pressure-bearing temporary plugging agent, which comprises the following components in parts by weight: 100 parts of water, 3-5 parts of bentonite, 0.3-0.5 part of xanthan gum, 70-110 parts of slag gelling agent, 3-6 parts of filler, 3-5 parts of retarder and 10-200 parts of barite powder. The high-pressure-bearing temporary plugging agent has the advantages of simple formula, low cost, short curing time and convenient operation; the risk of sticking the cement plug is avoided, the tripping required by the cement plug is reduced, the cement plug is prevented from being drilled, the operation time of sealing the open hole section of the conventional tie-back well cementing cement plug is favorably shortened, the construction operation of the temporary plugging agent is simple, and the field pumping requirement is met; can be widely applied to petroleum and natural gas drilling.
CN 1047686A discloses a high temperature resistant temporary plugging completion agent, which is formed by crosslinking a water-soluble organic titanium solution containing a temperature resistant agent or a reducing agent with a sesbania (or modified sesbania) glue solution, and is used for temporarily plugging a permeable or leakage stratum in the well completion or well repair process, automatically hydrating and plugging after an oil pipe and a packer are put off, and not plugging and damaging an oil layer or a production layer. Can be widely applied to the development and drilling, well completion and well repair processes of petroleum, natural gas, geothermal heat and the like.
CN 104831401A discloses an oil-soluble temporary plugging agent and a preparation method thereof. The oil-soluble temporary plugging agent is prepared by melt electrospinning a thermoplastic polymer or a mixture of the thermoplastic polymer and one or more of a surfactant, an antioxidant and a coupling agent as spinning raw materials. The temporary plugging agent has the average diameter of several microns to dozens of microns, even can reach the nanometer level, has wide distribution, is suitable for various oil wells with complex structures, and is particularly suitable for temporary plugging operation of cores with small fracture width; the oil solubility is high, the water and acid are insoluble, and the residual pollution to the stratum is small; the solubility in diesel oil is high, and the blockage is easy to remove; the raw materials are easy to obtain, the preparation process is simple, the cost is low, and the applicability is good.
CN 104927798A discloses a temporary plugging agent for petroleum drilling fluid. The temporary plugging agent comprises the following materials in percentage by weight: 40-60% of 1-hexadecene, 10-20% of formaldehyde solution, 10-20% of phenol, 1-2% of hexadecyl trimethyl ammonium chloride and 1-2% of high sodium sulfate.
CN 105062443A discloses an oil-soluble temporary plugging agent and a preparation method thereof, which solves the technical problem of workover fluid loss in the workover process of a high-temperature leakage oil and gas reservoir. The oil-soluble temporary plugging agent consists of the following components in parts by weight: 0.5-2 parts of carbon five petroleum resin, 0.5-2 parts of modified petroleum resin, 0.1-0.5 part of rosin modified phenolic resin, 0.4-0.6 part of xanthan gum, 2-5 parts of potassium chloride and the balance of water; wherein the softening point of the carbon five petroleum resin is greater than or equal to 140 ℃, the softening point of the modified petroleum resin is greater than or equal to 145 ℃, and the invasion of foreign fluids in a shaft of an oil-gas well with the length of 3500 m and above into a polluted oil layer can be avoided.
CN 105441043A discloses a temporary plugging microsphere, the diameter of which is 50-700 micrometers, which comprises the following components by weight percent: 23-26% of polyvinyl alcohol, 32-36% of gelatin, 4-6% of agar, 25-32% of weighting agent, 0.01-1% of sodium tetraborate and 3-4% of aldehyde curing agent. The temporary plugging microspheres enable the formed temporary plugging agent to be in a microspherical shape with the diameter of 50-700 microns through the synergistic effect of the components, and the strength of the temporary plugging agent is improved. The temporary plugging microsphere absorbs water to expand, the expansion ratio can reach 3.5, pores of a reservoir can be effectively plugged, after plugging is finished, the temperature is increased to 100-120 ℃, the temporary plugging microsphere is degraded, the degradation rate reaches 100% in 4-7 hours, retention in the reservoir is avoided, and the temporary plugging microsphere is safe and harmless to the reservoir.
CN 107090282A discloses a mixed temporary plugging agent, which comprises the following components in parts by weight: 1-9 parts of water-soluble high polymer, 3-29 parts of sand and 0-19 parts of soluble or degradable fiber. The mixed temporary plugging agent is prepared into a temporary plugging agent mixture by using 10-100 parts by weight of carrier fluid, and the temporary plugging agent mixture is replaced by displacement fluid to enter a preset position of a downhole crack, so that a temporary plugging wall with certain viscosity is formed. The plugging agent can be applied to vertical well separate-layer fracturing, horizontal well staged fracturing and old well repeated fracturing, the plugging position can be controlled by controlling the viscosity-raising time and the injection speed, 100% of plugging is raised, the plugging strength is high, the subsequent fracturing new joint is facilitated, and the yield of an oil-gas well is further improved.
CN 107828394A discloses a temporary plugging agent and a preparation method thereof, which comprises 20-85 wt% of adhesive, 12-77 wt% of reinforcing agent, 1-3 wt% of lubricant, and 0.2-1 wt% of thermal oxygen stabilizer, the temporary plugging agent has high strength, and the preparation process thereof has high production efficiency, compared with the conventional temporary plugging agent, the production cost is greatly reduced, and the temporary plugging agent can be applied to temporary plugging fracturing and temporary plugging acidification.
CN 108485623A discloses a cleaning temporary plugging agent, which is prepared from the following raw materials in percentage by mass: 10-13% of acrylamide, 10-13% of acrylic acid, 0.3-0.5% of caustic soda flakes, 0.08-0.1% of initiator, 7-9% of low temperature resistant glue epoxy resin, 0.5-0.8% of surfactant and the balance of water. The temporary plugging agent does not contain inorganic solid-phase particles, so that the damage to the stratum after the temporary plugging agent is dissolved is reduced, the preparation method of the temporary plugging agent is simple and safe, has the high-temperature resistance and salt resistance, can bear larger construction pressure, can resist high temperature, is extremely low in insoluble substance residue, controllable in dissolution rate, small in dosage and simple to use.
CN 108865088A discloses a temporary plugging agent and its application in plugging a fractured reservoir while drilling, wherein the temporary plugging agent contains rigid acid-soluble bridging particles, acid-soluble bridging fibers and acid-soluble filler particles, and based on the total weight of the temporary plugging agent, the content of the rigid acid-soluble bridging particles is 40-60 wt%, the content of the acid-soluble bridging fibers is 20-30 wt%, and the content of the acid-soluble filler particles is 20-30 wt%. The temporary plugging agent can be used for plugging reservoir cracks in real time when a fractured reservoir is drilled, is suitable for the temporary plugging technology of partial leakage during drilling of the fractured reservoir of a deep well and an ultra-deep well, has real-time and high-efficiency plugging performance, and is particularly suitable for the condition that the conventional plugging agent while drilling is difficult to meet the leakage of the fractured reservoir at the temperature of over 150 ℃ when the well temperature is over 90 percent of the total acid solubility, such as the acid solubility.
CN 109401739A discloses a high temperature resistant shielding temporary plugging agent, which comprises: 100 parts of particle materials, 5-20 parts of elastic materials, 5-20 parts of filling materials, 5-15 parts of fiber materials and 1-5 parts of micro-nano materials. The temporary plugging agent has small influence on the rheological property of drilling fluid, high temperature resistance, strong plugging property, good temporary plugging effect and high acid solubility, can resist the temperature of 200 ℃, has the pressure bearing capacity of 0.2mm crack of more than 10MPa, has the immersion depth of a 20-40-mesh sand bed of less than 3cm, has the core permeability recovery value of more than 95 percent and the acid solubility of more than 80 percent, can be used in an ultrahigh-temperature reservoir zone, and plays a role in protecting an oil gas layer.
CN 109554172A discloses an acid fracturing temporary plugging agent and application thereof. The formula of the acid fracturing temporary plugging agent comprises the following components in percentage by weight: 0.1-3% of temporary plugging fiber, 0.05-3% of non-expansion type temporary plugging ball A, 0.1-3% of expansion type temporary plugging ball B, 0.1-1% of supporting sand, 0.05-1% of dispersing agent and the balance of carrying fluid. The acid fracturing temporary plugging agent has good compatibility with formation fluid, good chemical stability, high plugging rate and thorough dissolution, and is suitable for high-temperature carbonate reservoirs.
CN 109776728A discloses a temporary plugging agent for drilling fluid and its application. Wherein the temporary plugging agent is obtained by carrying out polymerization reaction on gelatinized starch and vinyl grafting monomers in an activator solution in the presence of a cross-linking agent and an initiator; the vinyl grafting monomer comprises acrylic acid, acrylamide and 2-acrylamide-2-methylpropanesulfonic acid; the gelatinized starch is obtained by adding starch into deionized water for gelatinization reaction. The temporary plugging agent is biodegradable, has a degradation rate of over 50 percent in soil within 90 days, and is environment-friendly; the water-based drilling fluid added with the temporary plugging agent has good rheological fluid loss property, and can adaptively perform temporary plugging on strata with different permeabilities, wherein the permeability temporary plugging rate reaches 100 percent; meanwhile, the temporary plugging agent has high acid solubility, and after acidification and plugging removal, the permeability recovery value can reach over 85 percent, and the reservoir protection capability is remarkable.
CN 110305652A discloses a composite temporary plugging agent for fracturing and a preparation method thereof, wherein the composite temporary plugging agent comprises the following components by taking the total mass of the composite temporary plugging agent as a reference: 5-90% of polyglycolic acid, 0.1-3% of non-crosslinked fracturing fluid thickening agent, 0.1-5% of oxidant, 0.01-2% of activator, 0.2-3% of inorganic base and the balance of solvent. The polyglycolic acid has good blocking performance and complete degradation performance, can be subjected to self-degradation under the condition of reservoir temperature (30-240 ℃), and can also be subjected to synergistic degradation with a gel breaker, so that the aim of artificial controllable complete degradation is fulfilled, the damage to the reservoir is reduced, and the reservoir yield is improved to the maximum extent.
CN 1432620A discloses a shielding temporary plugging agent, which is composed of swelling material, bridging material, filling material, inhibiting material, etc., wherein the swelling material is all materials that can swell and form fibrous gel in water, such as nanmu root powder, cotton boll, etc., and the particle size is 0-838 μm; the bridging material is sheet mica with particle size of 97-381 μm; the filling material can be common calcium carbonate or light calcium carbonate, and the particle size is 0-117 mu m; the inhibiting material can be one or a mixture of several of the following materials: sodium polyacrylonitrile, potassium polyacrylonitrile, ammonium polyacrylonitrile, potassium humate, etc.
CN 113072919A discloses a shielding temporary plugging agent, a preparation method and an application thereof, wherein the shielding temporary plugging agent comprises the following components: a) a temporary blocking material, b) a first modifier, c) a second modifier and d) a solvent, wherein the first modifier is selected from one or more of fatty acid, fatty alcohol and fatty acid ester; the second modifier is selected from one or more of alkane and silicone oil. The shielding temporary plugging agent increases the physical-chemical dual action of the additional pressure of filtrate through physical plugging-hydrophobic modification, reduces the leakage rate of drilling fluid in cracks and pores, and achieves the purposes of reducing the leakage rate and improving the shielding temporary plugging effect.
CN 111534295A discloses a reversible gel temporary plugging agent for a water injection well, which is formed by compounding various raw materials of starch, acrylic acid, acrylamide, chromium acetate, ammonium bisulfite, ammonium persulfate, sodium hydroxide, formaldehyde, graphene particles, walnut shell particles and the like, has the characteristics of controllable gel forming time and gel breaking time, absorbability and slow release, and completely meets the temporary plugging process requirements of the water injection well in a string inspection operation; meanwhile, the reversible gel temporary plugging agent has the effects of high temporary plugging speed, safety and stability and realization of open-hole operation, and the reversible gel temporary plugging agent suitable for different operation requirements is screened by detecting the gelling time, the degradation time of colloid and the compressive strength of colloid of the prepared reversible gel temporary plugging agent, so that the adaptability of the reversible gel is greatly improved.
CN 111592871A discloses a shale oil shale gas fracturing temporary plugging agent, which is prepared from the following raw materials: modified polyacrylamide, a high-temperature stabilizer, a toughening agent, a thickening agent and a dispersing agent; the modified polyacrylamide is prepared from the following raw materials: acrylic acid, acrylamide, guarana gum, a cross-linking agent, an oxidizing agent, a reducing agent, graphene oxide, inorganic nanoparticles and a silane coupling agent. The temporary plugging agent can ensure that the temporary plugging agent has a good plugging effect in a short time, can also ensure that the good plugging effect is effective for a long time, and can not only be finally completely degraded or dissolved until the whole repeated fracturing construction is completed, so that the use efficiency of the temporary plugging agent and the repeated fracturing success rate are improved.
CN 112574731A discloses an oil-water mixture dissolving temporary plugging agent and a preparation method thereof, wherein the oil-water mixture dissolving temporary plugging agent comprises the following components in parts by weight: 5-10 parts of hydroxypropyl starch, 10-15 parts of hydroxyethyl starch ether, 3-10 parts of coumarone resin, 5-10 parts of hydrocarbon petroleum resin, 5-15 parts of carbon nine petroleum resin, 2-10 parts of sulfonated phenolic resin, 2-10 parts of ethylene diamine tetraacetic acid tetrasodium salt, 5-15 parts of benzoic acid, 2-4 parts of starch graft copolymer, 3-6 parts of acrylamide-acrylate copolymer, 5-10 parts of acrylic resin and the balance of water. The temporary plugging agent can be designed into different temporary plugging particle sizes according to stratum pore parameters, cannot be dissolved in a single water phase or oil phase, and can be slowly dissolved only in an oil-water mixed phase at a proper temperature.
CN 112625667A discloses an environment-friendly slow/controlled release temporary plugging agent with a hydrophobic modified core-shell structure and a preparation method thereof, wherein the temporary plugging agent comprises a shell and a water-soluble temporary plugging particle core, the shell is coated outside the water-soluble temporary plugging particle core, the shell comprises a degradable framework and a hydrophobic wall material, the degradable framework is modified polyurethane, and the hydrophobic wall material is paraffin. Preheating water-soluble temporary plugging particles, uniformly stirring and mixing toluene diisocyanate, polyether polyol, chitosan, diethyl toluene diamine and epoxy resin, and spraying the mixture on the surfaces of the water-soluble temporary plugging particles to form a degradable framework layer; and spraying molten paraffin on the surface of the degradable skeleton, and forming a shell structure comprising the degradable skeleton and the paraffin outside the water-soluble temporary plugging particle core. The slow release time of the slow/controlled release temporary plugging agent can be adjusted in a large range, so that the effect of adjustable slow release performance is achieved, and meanwhile, the mechanical property of the temporary plugging agent is greatly improved due to the core-shell structure.
As described above, various temporary plugging agents which can be used in the field of oil exploitation are disclosed in the prior art, but there is still a need for improving the temporary plugging effect (for example, slow degradation is required rather than complete degradation in several hours to avoid the failure of reaching a moderate plugging potential section; for example, excellent plugging effect is required to avoid damaging the potential section by a high-strength plugging agent in temporary plugging, etc.), and there is also a pressing need for new temporary plugging agents in the face of the reality of the increasing complexity of the oil well geological conditions and the decreasing oil recovery rate.
Therefore, a controllable temporary plugging agent for a horizontal well needs to be developed, the technical problem that the conventional oil well water plugging temporary plugging agent is degraded too fast and plugged incompletely to damage an oil layer is solved, the technical progress of oil exploration and exploitation has very important industrial value and scientific research significance, and the foundation and power of the invention are achieved.
Disclosure of Invention
In order to solve the above problems, an object of the present invention is to provide a temporary plugging agent for a horizontal well, which has the advantages of high gelling gel viscosity, excellent initial plugging property, appropriate degradation time, and complete degradation, and can simultaneously achieve good plugging of a high permeability layer in an initial stage, but reduce damage to an oil layer in a potential zone due to good degradation with time.
The inventor of the invention has made intensive research, and aiming at the defects and the places needing improvement of the temporary plugging agent in the production of the existing oil and gas well, after a large amount of creative work is paid, a pressure-bearing degradable temporary plugging agent for repairing the horizontal well and a preparation method and application thereof are obtained, and the invention is further completed.
Specifically, the technical solution and contents of the present invention mainly relate to the following aspects.
In a first aspect, the invention relates to a pressure-bearing degradable temporary plugging agent (hereinafter sometimes referred to as "temporary plugging agent") for well repair, which comprises acrylamide, alpha-phenyl acrylic acid prepolymer, sulfur-modified petroleum resin, polypropylene fiber, inorganic reinforcing agent, composite crosslinking agent, initiator and deionized water.
It should be noted that, throughout the present invention, the words "comprise", "comprises", and the like, when referring to a composition, include both open-ended words such as "comprises", "comprising", and the like, and closed-ended words such as "consisting of …", and the like.
In the temporary plugging agent, the content of the specific components is as follows by 100 parts of the total mass:
in the temporary plugging agent of the present invention, the amount of acrylamide is 4 to 15 parts by mass, and may be, for example, 4 parts, 6 parts, 8 parts, 10 parts, 12 parts, 14 parts, or 15 parts.
In the temporary plugging agent of the present invention, the α -phenyl acrylic prepolymer is present in an amount of 2 to 6 parts by mass, for example, 2 parts, 3 parts, 4 parts, 5 parts or 6 parts.
The alpha-phenyl acrylic prepolymer is prepared by the following steps:
(1): reacting alpha-phenylacrylic acid (i.e. CH) 2 C (pH) COOH, also known as 2-phenyl acrylic acid) to an aqueous NaOH solution, reacting at 40-50 ℃ for 20-30 minutes with stirring, and then adjusting the pH to neutral to obtain a solution;
(2): c with the mass percent concentration of 4-8% is added into the solution obtained in the step (1) 3-4 And heating the enol compound aqueous solution to 60-70 ℃ under stirring, slowly adding ammonium persulfate, stirring in a closed manner, keeping the temperature for reaction for 40-50 minutes, and naturally cooling to room temperature to obtain the alpha-phenyl acrylic acid prepolymer (thin glue-like transparent liquid).
Wherein, in the step (1), the mass percentage concentration of the NaOH aqueous solution is 20-30%, and the molar ratio of the alpha-phenyl acrylic acid to the NaOH (i.e. the NaOH in the NaOH aqueous solution) is 1:0.2-0.3, and can be 1:0.2, 1:0.25 or 1:0.3, for example.
In step (1), the pH can be adjusted by well-known means (according to the pH at the end of the reaction, conventional acids and bases such as hydrochloric acid, sulfuric acid, NaOH, KOH, etc. can be used for adjustment), and will not be described in detail herein, and those skilled in the art can perform appropriate operations according to actual situations.
Wherein, in the step (2), C 3-4 The molar ratio of enol compound to α -phenylacrylic acid in step (1) is 1:0.2 to 0.6, and may be, for example, 1:0.2, 1:0.3, 1:0.4, 1:0.5 or 1: 0.6.
Wherein, the C 3-4 The enol compound can be 2-propen-1-ol (CH) 2 ＝CHCH 2 OH), 3-buten-1-ol (CH) 2 ＝CHCH 2 CH 2 OH), 2-buten-1-ol (CH) 3 CH＝CHCH 2 OH) or 2-methyl-2-propen-1-ol (CH) 2 ＝C(CH 3 )CH 2 OH), most preferably 2-buten-1-ol (CH) 3 CH＝CHCH 2 OH)。
Wherein, in the step (2), the ammonium persulfate is 0.02-0.04% by mass of the alpha-phenylacrylic acid.
In the temporary plugging agent of the present invention, the sulfur-modified petroleum resin is 1.5 to 2.5 parts by mass, and may be 1.5 parts, 2 parts or 2.5 parts, for example.
Wherein the sulfur modified petroleum resin is prepared by the following method: c is to be 5 Fully dissolving petroleum resin in a proper amount of n-hexane, adding organic sulfide, heating to 80-100 ℃ in a sealed manner, keeping the temperature, stirring, reacting for 30-40 minutes, releasing pressure to completely volatilize the n-hexane, and naturally cooling to room temperature to obtain the sulfur modified petroleum resin.
Wherein, C 5 Petroleum resins are well known and commercially available and are not described in detail herein.
Wherein the organosulfide is bis (3-carboxypropyl) disulfide.
Wherein the C is dissolved 5 The amount of n-hexane used for the petroleum resin is not particularly restricted so long as C can be converted into C 5 The petroleum resin is completely and sufficiently dissolved, and those skilled in the art can make appropriate selections and determinations.
Wherein, C 5 The mass ratio of petroleum resin to organosulfide is 100:1-3, and may be, for example, 100:1, 100:2 or 100: 3.
In the temporary plugging agent of the present invention, the polypropylene fiber is present in an amount of 0.5 to 3 parts by mass, for example, 0.5 part, 1 part, 1.5 parts, 2 parts, 2.5 parts, or 3 parts.
Wherein the polypropylene fiber has a length of 6-8mm and a diameter of 5-10 μm, for example, a length of 6mm, 7mm or 8mm, and a diameter of 5 μm, 6 μm, 7 μm, 8 μm, 9 μm or 12 μm.
In the temporary plugging agent of the present invention, the inorganic reinforcing agent is 1.5 to 4 parts by mass, and may be, for example, 1.5 parts, 2 parts, 2.5 parts, 3 parts, 3.5 parts or 4 parts.
Wherein the inorganic reinforcing agent is any one of ultrafine calcium carbonate (particle size of 0.02-0.1 μm), sepiolite wool (fiber length of 2-5mm, for example, 2mm, 3mm, 4mm or 5mm) or attapulgite powder (particle size of 200-400 mesh, for example, 200 mesh, 300 mesh or 400 mesh), but preferably sepiolite wool because sepiolite wool has a fine and long fiber structure, can serve as a filler in the temporary plugging agent, can fill up fine pores formed when it is absent, and at the same time, improves the strength of the temporary plugging agent, thereby allowing a significant anti-scouring effect to be exerted.
In the temporary plugging agent of the present invention, the mass part of the composite crosslinking agent is 0.5 to 1 part, and may be, for example, 0.5 part, 0.6 part, 0.7 part, 0.8 part, 0.9 part or 1 part.
The composite cross-linking agent is a mixture of polyethylene glycol diacrylate and N, N '-methylene bisacrylamide, and the mass ratio of the polyethylene glycol diacrylate to the N, N' -methylene bisacrylamide is 10:1-4, and can be 10:1, 10:2, 10:3 or 10:4, for example.
The inventors found that when the composite cross-linking agent is used, a technical effect far superior to that of a single component can be obtained, and it is supposed that when the two are subjected to respective cross-linking reactions, due to the high uniformity of the system, a composite cross-linked network intertwined, embedded and entangled with each other is generated, so that the plugging strength can be more excellent during plugging, but as time goes on and under the action of high temperature and high salt in the stratum, once degradation occurs, the whole intertwined network is subjected to 'decomplexing' or 'grid collapse' in a short time, so that plugging is released, and the potential oil layer is prevented from being damaged.
In the temporary plugging agent of the present invention, the mass part of the initiator is 0.1 to 0.2 part, and may be, for example, 0.1 part, 0.15 part or 0.2 part.
The initiator is a persulfate compound, and can be any one or combination of any more of sodium persulfate, ammonium persulfate and potassium persulfate.
In the temporary plugging agent of the present invention, the mass part of the deionized water is 100 parts by mass of the total mass, and the mass remaining after removing the above components can be calculated according to the sum of the above components, and will not be described in detail herein.
In a second aspect, the invention relates to a preparation method of the pressure-bearing degradable temporary plugging agent for well repair, which comprises the following steps:
s1: weighing the above components in respective parts by mass, namely weighing acrylamide, alpha-phenyl acrylic acid prepolymer, sulfur modified petroleum resin, polypropylene fiber, inorganic reinforcing agent, composite cross-linking agent, initiator and deionized water in respective parts by mass;
s2: sequentially adding acrylamide, alpha-phenyl acrylic acid prepolymer, composite cross-linking agent accounting for 50% of the total mass and initiator into deionized water at room temperature, heating to 45-55 ℃ under stirring, stirring for reaction for 20-30 minutes, adding sulfur modified petroleum resin, polypropylene fiber, inorganic reinforcing agent and the remaining 50% of the composite cross-linking agent in parts by mass, and continuing stirring for reaction until the reaction system is uniform viscous liquid, thus obtaining the pressure-bearing degradable temporary plugging agent for well repair.
It should be noted that the addition of "50% of the composite crosslinking agent and the initiator by mass" in step S2 means that only 50% of the composite crosslinking agent by mass is added, and the initiator is still added all at once, i.e., "50%" is used only to limit the composite crosslinking agent and not to limit the initiator after it.
In the preparation method, in step S2, the composite crosslinking agent is added in batches, so that partial crosslinking can be achieved after the first addition under the action of the initiator, and although the remaining composite crosslinking agent is added, the continuous crosslinking and the entanglement interpenetration between the partial crosslinking system and the sulfur-modified petroleum resin, the polypropylene fiber and the inorganic reinforcing agent which are added later are achieved, so that the temporary plugging agent with viscosity and crosslinking degree can be obtained, and when the temporary plugging agent is completely added, the defect that the plugging effect is good but the degradation rate is too slow can be caused, which is described in detail below.
In a third aspect, the invention relates to the application of the pressure-bearing degradable temporary plugging agent for well repair in oil exploitation.
The pressure-bearing degradable temporary plugging agent for well repair has excellent plugging performance at the initial stage, can protect a potential section oil layer from being damaged by a high-strength plugging agent, can be completely degraded after a certain time (but not too short time in the prior art), and therefore subsequent exploitation of the potential section oil layer is not influenced.
The pressure-bearing degradable temporary plugging agent for well repair of the invention is preferably prepared in situ, for example, can be produced uniformly at a production site or a nearby factory, then transported and transported to an oil well and further diluted to the viscosity convenient for filling an injection well, and the operation can be carried out appropriately according to the actual production situation, and the detailed description is omitted.
As described above, the invention provides a pressure-bearing degradable temporary plugging agent for well repair, a preparation method and an application thereof, and the pressure-bearing degradable temporary plugging agent for well repair has various good performances through the mutual combination and cooperation of a plurality of technical characteristics and a unique preparation method, and has good industrialization potential and popularization value in the technical field of oil exploitation.
Drawings
Fig. 1 is a graph of the core permeability recovery (%) versus time (days) for temporary plugging agents Z1, D3, D5, D8, and D12.
Detailed Description
The present invention is described in detail below with reference to specific examples, but the use and purpose of these exemplary embodiments are merely to exemplify the present invention, and do not set forth any limitation on the actual scope of the present invention in any form, and the scope of the present invention is not limited thereto.
Preparation example 1: preparation of alpha-phenyl acrylic acid prepolymer
(1): reacting alpha-phenylacrylic acid (i.e. CH) 2 Adding the carbon (Ph) COOH) into a NaOH aqueous solution with the mass percentage concentration of 25%, stirring and reacting for 25 minutes at 45 ℃, and then adjusting the pH value to be neutral to obtain a solution;
wherein the molar ratio of the alpha-phenylacrylic acid to the NaOH is 1: 0.25;
(2): adding 6 percent 2-butene into the solution obtained in the step (1)-1-ol (CH) 3 CH＝CHCH 2 OH) aqueous solution, heating to 65 ℃ under stirring, then slowly adding ammonium persulfate, stirring in a closed manner, keeping the temperature, reacting for 45 minutes, naturally cooling to room temperature, and naming the obtained alpha-phenyl acrylic acid prepolymer in a thin glue state as Y1;
wherein the molar ratio of the 2-methyl-2-propylene-1-ol to the alpha-phenyl acrylic acid in the step (1) is 1:0.4, and the mass of the ammonium persulfate is 0.03 percent of the mass of the alpha-phenyl acrylic acid.
Comparative preparation examples 1 to 3: preparation of alpha-phenyl acrylic acid prepolymer
The 2-buten-1-ol (CH) in preparation example 1 was separately added 3 CH＝CHCH 2 OH) to 2-propen-1-ol (CH) 2 ＝CHCH 2 OH), 3-buten-1-ol (CH) 2 ＝CHCH 2 CH 2 OH), 2-methyl-2-propen-1-ol (CH) 2 ＝C(CH 3 )CH 2 OH), and the other operations are not changed, and the obtained alpha-phenyl acrylic acid prepolymer is named as DY1, DY2 and DY3 in sequence.
Preparation example 2: preparation of sulfur-modified petroleum resin
C is to be 5 Dissolving petroleum resin in n-hexane, and adding organic sulfide bis (3-carboxypropyl) disulfide (C) 5 The mass ratio of the petroleum resin to the di (3-carboxypropyl) disulfide is 100:2), the temperature is raised to 90 ℃ in a closed way, the temperature is kept and the stirring is carried out for 35 minutes, the normal hexane is completely volatilized after the pressure is released, and the reaction product is naturally cooled to the room temperature, so that the sulfur modified petroleum resin which is a high-viscosity solid is obtained.
In the following embodiment, each component used in step S2 is the corresponding component weighed in step S1, and is not repeated in step S2 for brevity.
Example 1: preparation of pressure-bearing degradable temporary plugging agent for well repair
S1: respectively weighing 9.5 parts of acrylamide, 4 parts of alpha-phenylacrylic acid prepolymer Y1, 2 parts of sulfur modified petroleum resin (obtained in preparation example 2), 1.75 parts of polypropylene fiber (the length is between 6 and 8mm and the diameter is between 5 and 10 mu m), 2.75 parts of inorganic reinforcing agent sepiolite wool (the fiber length is between 2 and 5mm), 0.75 part of composite cross-linking agent (a mixture of polyethylene glycol diacrylate and N, N' -methylene bisacrylamide with a mass ratio of 10: 2.5), 0.15 part of initiator sodium persulfate and the balance of deionized water by mass part and total mass of 100 parts by mass;
s2: sequentially adding acrylamide, alpha-phenyl acrylic acid prepolymer, 50% of composite cross-linking agent and initiator into deionized water at room temperature, heating to 50 ℃ under stirring, stirring for reacting for 25 minutes, adding sulfur modified petroleum resin, polypropylene fiber, inorganic reinforcing agent and the rest 50% of composite cross-linking agent, and continuously stirring for reacting until a reaction system is uniform viscous liquid, thus obtaining the pressure-bearing degradable temporary plugging agent for well repair, which is named as Z1.
Example 2: preparation of pressure-bearing degradable temporary plugging agent for well repair
S1: respectively weighing 4 parts of acrylamide, 6 parts of alpha-phenylacrylic acid prepolymer Y1, 1.5 parts of sulfur modified petroleum resin (obtained in preparation example 2), 3 parts of polypropylene fibers (the length is 6-8mm and the diameter is 5-10 mu m), 1.5 parts of inorganic reinforcing agent sepiolite wool (the length of the fibers is 2-5 mm), 1 part of composite cross-linking agent (a mixture of polyethylene glycol diacrylate and N, N' -methylene bisacrylamide with a mass ratio of 10: 1), 0.1 part of initiator sodium persulfate and the balance of deionized water by mass part and total mass of 100 parts;
s2: sequentially adding acrylamide, alpha-phenyl acrylic acid prepolymer, 50% of composite cross-linking agent and initiator into deionized water at room temperature, heating to 45 ℃ under stirring, stirring for reaction for 30 minutes, adding sulfur modified petroleum resin, polypropylene fiber, inorganic reinforcing agent and the remaining 50% of composite cross-linking agent by mass, and continuously stirring for reaction until the reaction system is uniform viscous liquid, thus obtaining the pressure-bearing degradable temporary plugging agent for well repair, which is named as Z2.
Example 3: preparation of pressure-bearing degradable temporary plugging agent for well repair
S1: respectively weighing 15 parts of acrylamide, 2 parts of alpha-phenylacrylic acid prepolymer Y1, 2.5 parts of sulfur modified petroleum resin (obtained in preparation example 2), 0.5 part of polypropylene fiber (the length is between 6 and 8mm and the diameter is between 5 and 10 mu m), 4 parts of inorganic reinforcing agent sepiolite wool (the fiber length is between 2 and 5mm), 0.5 part of composite cross-linking agent (a mixture of polyethylene glycol diacrylate and N, N' -methylene bisacrylamide in a mass ratio of 10: 4), 0.2 part of initiator sodium persulfate and the balance of deionized water by mass part and total mass of 100 parts;
s2: sequentially adding acrylamide, alpha-phenyl acrylic acid prepolymer, 50% of composite cross-linking agent and initiator into deionized water at room temperature, heating to 55 ℃ under stirring, stirring for reaction for 20 minutes, adding sulfur modified petroleum resin, polypropylene fiber, inorganic reinforcing agent and the remaining 50% of composite cross-linking agent by mass, and continuously stirring for reaction until the reaction system is uniform viscous liquid, thus obtaining the pressure-bearing degradable temporary plugging agent for well repair, which is named as Z3.
Comparative examples 1 to 3: preparation of pressure-bearing degradable temporary plugging agent for well repair
Comparative examples 1 to 3 were obtained by replacing the α -phenylacrylic acid prepolymer Y1 of examples 1 to 3 with DY1, DY2 and DY3 in this order, respectively, and the obtained temporary plugging agents were named D1, D2 and D3 in this order.
Comparative examples 4 to 6: preparation of pressure-bearing degradable temporary plugging agent for well repair
Each of the sulfur-modified petroleum resins of preparation examples 2 of examples 1 to 3 was replaced with the same parts by mass of C 5 The petroleum resin (i.e., not modified with organic sulfide) was not changed in other operations, thereby obtaining comparative examples 4 to 6, and the obtained temporary plugging agents were named D4, D5 and D6 in this order.
Comparative examples 7 to 12: preparation of pressure-bearing degradable temporary plugging agent for well repair
Comparative examples 7 to 9 were obtained by changing the composite crosslinking agents of examples 1 to 3 with the single crosslinking agent of polyethylene glycol diacrylate in the same parts by mass, respectively, and the obtained temporary plugging agents were named D7, D8 and D9 in this order.
Comparative examples 10 to 12 were obtained by changing the composite crosslinking agents of examples 1 to 3 with the same mass parts of the single crosslinking agent N, N' -methylenebisacrylamide, respectively, and the resulting temporary plugging agents were named D10, D11 and D12 in this order.
Performance testing
The respective temporary plugging agents obtained in the above examples and comparative examples were subjected to performance tests of different indexes, specifically, as follows.
1. Testing of gelling Properties of temporary plugging agent
An appropriate amount of Z1-Z3 of examples 1-3 are respectively taken and placed in a jar with a stopper, the gelling condition is observed in a constant temperature drying oven at 60 ℃, experiments show that primary gelling is carried out after 6 hours, and the measured apparent viscosity is 35000 +/-100 mPa.s, so that the gel is proved to have good gelling performance and can be used for blocking rocks in oil layers.
The apparent viscosity of D1-D12 after gelling is reduced by 1250-2000 mPas compared with that of Z1-Z3, which proves that the D1-D12 can be used for plugging reservoir rocks (although the viscosity is reduced).
2. Testing of plugging Performance
The quartz sand of 80-120 mesh was packed into a sand-packed tube of 2.5cm in diameter and 60cm in length and sufficiently compacted, and then the permeability of each sand-packed tube with respect to water at room temperature was measured.
Each temporary plugging agent is injected into the sand pack immediately after being prepared immediately (per cm relative to the sand pack) 2 Sectional area, injection speed of 0.1 ml/min, pressure of 0.2MPa and injection time of 4 hours), then sealing two ends of the sand-packed pipe, placing the sand-packed pipe in a constant-temperature drying box at 60 ℃ for keeping constant temperature for 10 hours to gelatinize the temporary plugging agent in the sand-packed pipe, finally injecting water for a displacement experiment, and measuring the permeability of each sand-packed pipe again, thereby obtaining the formula: the plugging capacity of each temporary plugging agent is calculated by (%) (permeability before plugging-permeability after plugging)/permeability before plugging × 100%, the test is a very well-known investigation means, and the specific operation details are not described in detail herein.
The results are shown in Table 1 below.
TABLE 1 blocking Rate of the respective temporary blocking agents
Among them, the plugging rates of Z1-Z3, D4-D6, D7-D9 and D10-D12 were averaged because the difference between the samples was not large (the actual value of each was not more than 5% from the average value). The D1/D2/D3 has a large deviation, so that the plugging rates of D1, D2 and D3 are respectively 94.4%, 88.1% and 90.3%. In the following tables, the same meanings and the same correspondence relationships are given for the same type of representation, and are not described one by one below.
As can be seen from the above table: 1. the temporary plugging agent of the present invention has excellent plugging properties (see Z1-Z3). 2. However, it is significantly different that when 2-buten-1-ol in the preparation of α -phenylpropenoic acid prepolymer is replaced with 2-propen-1-ol, 3-buten-1-ol or 2-methyl-2-propen-1-ol, the blocking rate is considerably decreased, and the inventors speculate that this should be because hydrophilic terminal methylol group (-CH) when 2-buten-1-ol is used 2 OH) directly to the polymeric backbone, -OH is via only one-CH 2 And the plugging agent is connected with the main chain, so that the plugging agent can be tightly combined with the tiny fine hole walls in the reservoir rock, and a good plugging effect is realized. And when replaced with 2-propen-1-ol, it is-, [ in the polymeric backbone ] * CH 2 -CH(CH 2 OH)]-, although the terminal hydroxyl group is also via a-CH group 2 Is linked to the main chain, but * the-CH present on C not being present as 2-buten-10-ol 3 The density of groups on a network formed by entanglement of the whole polymer main chain and the whole polymer is reduced, and the blocking property is reduced. When substituted with 3-buten-1-ol, then the terminal hydroxyl groups are bonded to the backbone via the-CH 2 CH 2 Links, which have a reduced hydrophilicity and a reduced bonding strength to the walls of the fine pores owing to the increased chain length. And when replaced with 2-methyl-2-propen-1-ol, due to CH 2 ＝C * (CH 3 )CH 2 C in OH * The steric hindrance existing in the connection of methyl and hydroxymethylene at the same time can reduce the polymerization degree of the aromatic diamine, thereby reducing the polymerization degree of the aromatic diamineThe hydrophilic-OH content on the final polymeric backbone is reduced, ultimately resulting in a reduction in overall hydrophilic bonding. In view of such differences, the applicant will make further intensive studies in combination with actual exploitation conditions of oil fields in the future, and will seek to disclose the principles thereof so as to make corresponding further improvements and studies. 3. When C is 5 The petroleum resin is not modified by organic sulfide and a single cross-linking agent is used, so that the plugging performance is reduced to a certain extent (see D4-D12, particularly the D4-D6 is obviously reduced), which proves that the modification of the organic sulfide can obviously improve the plugging effect (the modification of the organic sulfide improves the C 5 The swelling property, the scouring strength and the like of petroleum resin), and the final plugging effect can be improved to a certain extent by using the composite cross-linking agent.
3. Test of core permeability recovery capability of temporary plugging agent
Filling 80-120 mesh quartz sand into a sand filling pipe with the diameter of 2.5cm and the length of 60cm, and measuring the initial permeability K of the core 0 Then, respectively injecting the temporary plugging agents into a sand filling pipe, sealing two ends of the sand filling pipe, placing the sand filling pipe in a constant-temperature drying box at 60 ℃ for a period of time, injecting water for a displacement experiment, and measuring K 1 、K 2 Time dependent variation (K) 1 For the permeability of each of the temporary blocking agents of examples 1-3 (i.e., any of Z1-Z3), K 2 The permeability of the temporary plugging agent in each comparative example) in K 1 /K 0 、K 2 /K 0 And calculating the permeability recovery value of the core, and making a graph of the calculated permeability recovery value, for example, fig. 1 is a graph of the permeability recovery value (%) of the temporary plugging agents Z1, D3, D5, D8 and D12 as a function of time (days), the permeability recovery value graphs of other temporary plugging agents are similar to Z1, D3, D5, D8 and D12 respectively because of the change trend thereof (Z2-Z3 is similar to Z1, D1-D2 is similar to D3, D4 and D6 are similar to D12, D7, D9 is similar to D8 and D10-D11 are similar to D5) and are not shown in the graph (too dense to be visually shown) one by one and are shown in the following table 2 (only main time points at intervals of 5 days are listed, and the change trends of other specific time points are similar to fig. 1).
TABLE 2 Permeability recovery values for each temporary plugging agent
As can be seen by combining the table 2 and the figure 1, the temporary plugging agent has very excellent core permeability recovery value, the recovery value increases basically linearly before 14 days, but suddenly and sharply increases to about 95.9% in about 15 days, the temporary plugging agent is degraded basically and completely, and the subsequent exploitation of a potential section is not influenced any more at this moment. When the enol compound is changed, the recovery value is still lower than 30% at 15 days, but the recovery value is sharply increased to about 80% at about 17 days, namely the recovery value is delayed and the gel degradation rate is reduced compared with that of Z1-Z3. Compared with Z1-Z3, the change of the composite cross-linking agent has a very significant influence on the permeability recovery value, particularly, D10-D12 still recovers to about 42% in 20 days, and the subsequent exploitation of the potential zone cannot be carried out at the time, which proves that the degradation of the finally obtained polymer is very difficult when the single-component cross-linking agent is used, and the permeability recovery value is unexpectedly and significantly improved when the mixture of the polyethylene glycol diacrylate and the N, N' -methylene bisacrylamide is used as the cross-linking agent, so that the obtained polymer is more easily degraded under the condition of a stratum, the temporary plugging function is realized, and the normal exploitation of the subsequent potential zone oil layer is not influenced.
4. Examination of gel viscosity Retention at high temperature
Respectively filling each temporary plugging agent prepared immediately into an opaque glass bottle, sealing, then placing in a thermostat at 150 ℃, respectively measuring apparent viscosity (hereinafter referred to as "initial apparent viscosity") during initial gelling after 24 hours, continuously keeping the temperature for 5 days, 10 days, 15 days and 20 days, respectively measuring apparent viscosity after aging for each day, and finally calculating the gel viscosity retention rate, wherein the calculation formula is as follows:
gel viscosity retention (%) { (apparent viscosity after aging-initial apparent viscosity) ÷ initial apparent viscosity } × 100%.
The results are given in Table 3 below.
TABLE 3 gel viscosity Retention for each temporary plugging agent
It can be seen that the gel viscosity retention of the temporary plugging agent Z1-Z3 decreases dramatically with time. The retention rates of D1-D3 of enol compounds in 5 days are changed to be similar, but the retention rate is obviously higher than that of Z1-Z3 along with the prolonging of time, so that the enol compounds always keep stronger plugging capability in potential rock strata. More significantly, this very high viscosity retention, especially D10-D12, is maintained when a single component crosslinker is used, with retention of up to about 80% after 20 days.
In conclusion, the results of the gel viscosity retention rate were also matched with those of table 2, and the same trend was verified.
Examination of production method step S2
As described above, when the production method of the present invention is employed, the temporary plugging agent Z1-Z3 having excellent technical effects can be obtained. On the other hand, when the composite crosslinking agent in step S2 was added all at once, it was found that the effect was reduced (only Z1-Z3 of examples 1 to 3 were examined because the practical oil well application effect of D1-D12 was not good), as follows: all the composite crosslinking agents are added in step S2 (i.e., acrylamide, α -phenylacrylic acid prepolymer, all the composite crosslinking agents and initiator … are added to deionized water in sequence) at one time, and the other operations are the same, and the obtained temporary plugging agents are named as DZ1, DZ2 and DZ 3.
Their blocking rates, core permeability recovery values and gel viscosity retention at elevated temperatures were tested in the same manner as described above and the results are shown in tables 4-6, respectively, along with data for Z1-Z3 for more visual comparison.
TABLE 4 occlusion rates for Z1-Z3 and DZ1-DZ3
It can be seen that there is no reduction in the blocking rate of DZ1-DZ3, which demonstrates that the same crosslinking strength is achieved with all composite crosslinking agents added at once as with the stepwise addition, and a similar blocking rate is achieved.
TABLE 5 permeability recovery values for Z1-Z3 and DZ1-DZ3
Therefore, the core permeability recovery value of DZ1-DZ3 is obviously inferior to that of Z1-Z3, and the gel degradation performance is proved to be obviously reduced and is not higher than 80% even after 20 days.
TABLE 6 gel viscosity retention of Z1-Z3 and DZ1-DZ3
It can be seen that the retention of the high temperature gel viscosity of DZ1-DZ3 is also significantly higher than that of Z1-Z3, which is mutually corroborated with the data in Table 5.
From the above tables 4-6, it can be seen that when the complex cross-linking agent is added all at once, the initial plugging rate is not changed, but the gel degrades slowly and has a higher gel viscosity retention rate with the time, so that the core recovery value is significantly lower than that of Z1-Z3. This demonstrates that the gel degradation can be improved by adding the complex cross-linking agent in steps.
As described above, the pressure-bearing degradable temporary plugging agent for well repair has various good performances by the mutual combination and cooperation of a plurality of technical characteristics and a unique preparation method, and can keep the plugging time of the potential section just about 15 days, and at the moment, the exploitation of the oil layer of the potential section can be usually carried out, so that the oil recovery period of most oil wells is matched, the technical effect of controllable degradation is obtained, and the pressure-bearing degradable temporary plugging agent for well repair has good industrialization potential and popularization value in the technical field of oil recovery.
It will be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Moreover, it should also be understood that various alterations, modifications and/or variations can be made to the present invention by those skilled in the art after reading the technical content of the present invention, and all such equivalents fall within the scope of protection defined by the claims appended to this application.
Claims (9)
1. The utility model provides a pressure-bearing degradable temporary plugging agent for well workover which characterized in that: the temporary plugging agent comprises acrylamide, alpha-phenyl acrylic acid prepolymer, sulfur modified petroleum resin, polypropylene fiber, inorganic reinforcing agent, composite cross-linking agent, initiator and deionized water;
the temporary plugging agent comprises the following specific components in parts by mass based on 100 parts of the total mass:
the alpha-phenyl acrylic prepolymer is prepared by the following steps:
(1): adding alpha-phenyl acrylic acid into NaOH aqueous solution, stirring and reacting for 20-30 minutes at 40-50 ℃, and then adjusting the pH value to be neutral to obtain solution;
(2): c with the mass percent concentration of 4-8% is added into the solution obtained in the step (1) 3-4 Heating an enol compound aqueous solution to 60-70 ℃ under stirring, then slowly adding ammonium persulfate, stirring in a closed manner and keeping the temperature for reaction for 40-50 minutes, and naturally cooling to room temperature to obtain the alpha-phenyl acrylic acid prepolymer;
said C is 3-4 The enol compound is 2-butene-1-ol;
the sulfur modified petroleum resin is prepared by the following method: c is to be 5 Dissolving petroleum resin in n-hexane, adding organic sulfide, heating to 80-100 deg.C under sealed condition, stirring for 30-40 min,after pressure relief, completely volatilizing normal hexane, and naturally cooling to room temperature to obtain the sulfur modified petroleum resin;
the composite cross-linking agent is a mixture of polyethylene glycol diacrylate and N, N '-methylene bisacrylamide, and the mass ratio of the polyethylene glycol diacrylate to the N, N' -methylene bisacrylamide is 10: 1-4.
2. The temporary plugging agent of claim 1, wherein: the reinforcing agent is any one of superfine calcium carbonate with the granularity of 0.02-0.1 mu m, sepiolite wool with the fiber length of 2-5mm or attapulgite powder with the granularity of 200-400 meshes.
3. The temporary plugging agent of claim 2 wherein: the fiber length of the sepiolite wool is 2mm, 3mm, 4mm or 5 mm.
4. The temporary plugging agent of claim 2 wherein: the particle size of the attapulgite powder is 200 meshes, 300 meshes or 400 meshes.
5. The temporary plugging agent of claim 2 wherein: the reinforcing agent is sepiolite wool with the fiber length of 2-5 mm.
6. The temporary plugging agent of any one of claims 1 to 5 wherein: the initiator is a persulfate compound.
7. The temporary plugging agent of claim 6 wherein: the initiator is any one or combination of any more of sodium persulfate, ammonium persulfate or potassium persulfate.
8. A process for the preparation of a temporary plugging agent according to any one of claims 1 to 7, wherein: the preparation method comprises the following steps:
s1: weighing the above components in respective parts by mass, namely weighing acrylamide, alpha-phenyl acrylic acid prepolymer, sulfur modified petroleum resin, polypropylene fiber, inorganic reinforcing agent, composite cross-linking agent, initiator and deionized water in respective parts by mass;
s2: sequentially adding acrylamide, alpha-phenyl acrylic acid prepolymer, 50% of composite cross-linking agent and initiator into deionized water at room temperature, heating to 45-55 ℃ under stirring, stirring for reacting for 20-30 minutes, adding sulfur modified petroleum resin, polypropylene fiber, inorganic reinforcing agent and the remaining 50% of composite cross-linking agent by mass, and continuing stirring for reacting until the reaction system is uniform viscous liquid, thus obtaining the temporary plugging agent.
9. Use of the temporary plugging agent according to any one of claims 1 to 7 or prepared by the preparation method according to claim 8 in oil exploitation.
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| CN114805672B (en) * | 2022-06-24 | 2022-09-13 | 山东科兴化工有限责任公司 | Degradable temporary plugging agent for oil-gas well as synthetic method and application thereof |
| CN115584252B (en) * | 2022-12-09 | 2023-04-07 | 东营盛世石油科技有限责任公司 | Temporary plugging agent for fracturing operation well repair and preparation method thereof |
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