CN106188403A - A kind of anti-CO of high temperature and high salt oil deposit2has channeling blocking agent and preparation method thereof - Google Patents

A kind of anti-CO of high temperature and high salt oil deposit2has channeling blocking agent and preparation method thereof Download PDF

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CN106188403A
CN106188403A CN201610567724.3A CN201610567724A CN106188403A CN 106188403 A CN106188403 A CN 106188403A CN 201610567724 A CN201610567724 A CN 201610567724A CN 106188403 A CN106188403 A CN 106188403A
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blocking agent
temperature
salt
high temperature
monomer
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CN106188403B (en
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刘锐
蒲万芬
陈博文
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Southwest Petroleum University
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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
    • C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
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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
    • C09K8/58—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids
    • C09K8/588—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids characterised by the use of specific polymers
    • C—CHEMISTRY; METALLURGY
    • 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
    • C09K8/58—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids
    • C09K8/594—Compositions used in combination with injected gas, e.g. CO2 orcarbonated gas
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2351/00—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
    • C08J2351/02—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers grafted on to polysaccharides
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids

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  • Health & Medical Sciences (AREA)
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Abstract

The invention discloses a kind of anti-CO of high temperature and high salt oil deposit2Has channeling blocking agent and preparation method thereof, is reaction monomers by carboxylic first (second) base enclosure polysaccharide, acrylamide, temperature-resistant anti-salt monomer, acrylic acid, with phenol, formaldehyde as cross-linking agent, with azo-bis-isobutyrate hydrochloride, azodiisobutyronitrile or (NH4)2S2O8‑NaHSO3System is initiator, and the polymerization of monomer molecule synchronization carries out being formed in situ gel with crosslinking under formation conditions.This blocking agent energy selectivity enters (micro-) crack, little to matrix damage, and can effectively migrate to the deep on stratum, it is achieved the effective closure to predominant pathway, it is adaptable to reservoir temperature 80 DEG C～140 DEG C, high salinity 10 × 104Mg/L, in or strong acidic environment, efficiently solve existing plugging agent at high temperature and high salt, the low-permeability oil deposit CO to supercriticality2The problems such as sealing characteristics is not enough, possess wide market application foreground.

Description

A kind of anti-CO of high temperature and high salt oil deposit2Has channeling blocking agent and preparation method thereof
Technical field
The present invention relates to one and be applicable to reservoir temperature 80 DEG C～130 DEG C, high salinity 10 × 104Mg/L, in or strong Sour environment, can effectively block CO2Gelling Plugging Agent of has channeling and preparation method thereof, belongs to field of oilfield chemistry.
Background technology
Oil field is at the initial stage of exploitation, and oil reservoir energy enriches, by stratum and the release of the elastic energy of fluid, displacement crude oil To pit shaft, referred to as primary oil recovery.Along with the deficit of oil reservoir elastic energy, crude oil production rate reduction, supplement stratum energy Water filling, air insufflation techiques be improve crude oil recovery percent of reserves inevitable measure [Ye Zhongbin, Pu Wanfen etc. improve oil recovery factor (second Version), petroleum industry publishing house, 2007].CO2Drive not only efficiently solve commercial production, people's lives greenhouse gas emission, The significant problems such as storage, and due to its unique effective displacement mechanism such as principles such as oil gas mixed phase, extracting crude oil, and become gas Drive the key technology improving oil recovery factor.Especially for (surpassing) low-permeability oil pool, conventional water drive injection difficulty, CO2Drive technology particularly important.(surpassing) low-permeability oil pool generally goes through pressure break and forms (micro-) crack, to improve the seepage channel of oil And drainage area, it addition, the natural microcrack of low-permeability oil pool is grown, note CO2(pressure break is split along predominant pathway to need to solve gas Seam, intrinsic fracture) problem such as channelling.But, CO2In oil reservoir generally presented in supercritical, meet water and form middle strong acid, Therefore, CO is carried out2The channelling pre-breakthrough plugging technology task of top priority is to prepare acidproof, resisting high temperature, high salt, and being injected simultaneously into property is good Plugging agent.
The plugging material numerous types of oil reservoir anti-gas channeling, can be divided into inorganic material, organic material and composite etc., performance The most identical (Wang Haijing. acid-resisting and oil-resisting type foam profile control agent experimentation [J]. petroleum geology and engineering, 2011 (01): 131-133).Inorganic material low price with cement, calcium silicates and waterglass as representative, heat and salt resistance (40～200 DEG C) Good, resistance to acids and bases, but this kind of material is poor in low-permeability oil pool injection, construction risk big (Li Qiqing, Song Xianmin, Wu Ming Superfine. the acidproof rigid blocking agent of New-type Sodium Silicate Single-fluid method [J]. oil drilling technology, 2003,25 (1): 60-62).With phenolic aldehyde, urea Urea formaldehyde, solidifying (freezing) glue are typical oil field organic materials.It is that solution, injection be good, heatproof before phenolic aldehyde, Lauxite consolidation Salt-resistance (80～180 DEG C) is good, resistance to alkalescence, and shortcoming shows little point of solution injury substrate risk (Wu Jun, Li Liangchuan, Lu Hai Big etc. the development [J] of Lauxite modification water shutoff agent. oilfield chemistry, 2012,29 (003): 299-301).Solidifying (freezing) glue can divide For cross-linked polymer gel and in-situ polymerization thing gel two class, wherein cross-linked polymer gel is certain density high molecular polymerization The gel rubber system that thing base fluid and cross-linking system are cross-linked to form at the formation temperature, before plastic, base fluid is containing macromolecule polyalcohol, therefore, Certain selectivity is had injecting during stratum, the chemical constitution of polymer gel rubber system with the type decided of cross-linking agent Performance such as heat and salt resistance, long-time stability etc. (Jia H, Pu W F, Zhao J Z, et al.Experimental investigation of the novel phenol-formaldehyde cross-linking HPAM gel system: based on the secondary cross-linking method of organic cross-linkers and its gelation performance study after flowing through porous media[J].Energy& Fuels,2011,25(2):727-736).Certain acidproof (alkali) performance is had after cross-linked polymer gel plastic, but at middle strong acid Property (pH 2-3) condition, plastic or plastic rear stability can be not poor.In-situ polymerization thing gel is that little molecule organic monomer base fluid exists The strong gel rubber system of reservoir media plastic, gel plastic controllability is strong on the spot, heat and salt resistance, weak acid resistant (alkali) after plastic Property, but there is the risk of injury substrate in small molecule solution.Composite is by organic polymer hydridization or intercalated inorganic material system Standby, first such material is synthetically formed Weak gel particle on ground, carries out infusion the most again and enters stratum.Composite is high temperature resistant High salt, also has certain acid resistance, and the tune of predominant pathway is blocked up excellent performance, is widely used in China's oil field profile control, water blockoff work Industry.But the particle shape of composite can not injection or injection difference be to limit composite in hyposmosis in hyposmosis The Main Bottleneck of oil reservoir application.
In sum, the history of the stifled investigation of materials of oil field tune is longer, type is various, and its oil reservoir adapts to phase the most not to the utmost With, show highlightedly: the low price of inorganic material, shut-off capacity are strong, resisting high temperature, high salt, but injection is poor, flow process In solidification opportunity control difficulty, easy blind plugging, it is poor to adapt to low-permeability oil deposit；Organic material abundant species, the molecule of this kind of material Its oil reservoir conformability of structures shape (high temperature resistance, high salt, acidproof etc.), but universal performance to be resistance to acids and bases the strongest；Composite Possessing the characteristic of organic material and inorganic material, it often shows the effect of 1+1 > 2, and its injection falls between, resistance to Soda acid performance needs in-depth study.
Summary of the invention
It is an object of the invention to provide a kind of anti-CO of high temperature and high salt oil deposit2Has channeling blocking agent, this blocking agent has one before plastic Fixed molecular dimension can enter (micro-) crack by selectivity effectively, and the injury to substrate is little, and the viscosity of this blocking agent base fluid is the least In the viscosity of cross linked polymer base fluid, can effectively migrate to the deep on stratum, it is achieved the effective closure to predominant pathway, it is adaptable to Reservoir temperature 80 DEG C～140 DEG C, high salinity 10 × 104Mg/L, in or strong acidic environment, efficiently solve existing plugging agent At high temperature and high salt, the low-permeability oil deposit CO to supercriticality2The problems such as sealing characteristics is not enough.
Another object of the present invention also resides in the offer anti-CO of above-mentioned high temperature and high salt oil deposit2The preparation method of has channeling blocking agent, logical Cross blocking agent gelation time prepared by the method controlled, it is adaptable to high temperature and high salt, (in) strong acidic condition, the closure to (micro-) crack Rate reach 85% and more than, can realize CO2The permanently effective closure of has channeling.The principle of the invention is reliable, and raw material sources is extensive, behaviour Make method easy, possess wide market application foreground.
For reaching above technical purpose, the present invention is by the following technical solutions.
A kind of anti-CO of high temperature and high salt oil deposit2Has channeling blocking agent, is by carboxylic first (second) base enclosure polysaccharide, acrylamide, temperature-resistant anti-salt Monomer, acrylic acid, water soluble phenolic, azo or redox system composition base fluid, be polymerized same with crosslinking under formation conditions Step is carried out, the Gelling Plugging Agent being formed in situ.
A kind of anti-CO of high temperature and high salt oil deposit2Has channeling blocking agent, is resisted by carboxylic first (second) base enclosure polysaccharide, acrylamide (AM), heatproof Salt monomer, acrylic acid (AA) are reaction monomers, with phenol, formaldehyde as cross-linking agent, with azo-bis-isobutyrate hydrochloride (AIBA), occasionally Nitrogen bis-isobutyronitrile or (NH4)2S2O8-NaHSO3System is initiator, and the polymerization of monomer molecule is Tong Bu with crosslinking under formation conditions Carrying out being formed in situ gel, its structural formula is as follows:
N=10 or 12, R are CH3Or C2H5
Wherein: v, w, x, y, z are the mass percent of construction unit, v is 3.5～7.5%, and w is 65～75%, and x is 0.5 ～5%, y is 5～10%, z=1-v-w-x-y.
Described carboxylic first (second) base enclosure polysaccharide is carboxymethyl chitosan or carboxyetbyl chitosan, weight average molecular weight is 2～5 × 104G/mol, deacetylation is 45～87%, and molecular structural formula is as follows:
R is CH3Or C2H5。
Described temperature-resistant anti-salt monomer is 2-alkyl acrylamide dodecyl acid (AMC12Or 2-alkyl acrylamide 14 S) Alkyl acid (AMC14S), molecular structural formula is as follows:
N=10 or 12.
Described temperature-resistant anti-salt monomer can also is that N-vinylpyridine network alkanone, 2-acrylamido-2-methacrylic sulfonic acid Sodium or sodium vinyl sulfonate.
The anti-CO of described high temperature and high salt oil deposit2The preparation method of has channeling blocking agent, comprises the following steps successively:
(1) preparation blocking agent base fluid, blocking agent base fluid is made up of by weight percent following components: carboxylic first (second) base enclosure polysaccharide 1 ～2%, acrylamide 3.5～6.2%, acrylic acid 0.25～1%, temperature-resistant anti-salt monomer 0.02～0.1%, initiator 0.008 ～0.12%, phenol, formaldehyde crosslinking agent (phenol, the mass ratio of formaldehyde are 1:3) 0.5～1.2%, remaining be clear water, saline or Oilfield injection water；
(2) pumping in stratum by described blocking agent base fluid, under formation conditions, the polymerization of monomer is synchronization carried out with crosslinking, It is formed in situ motionless gel.
Compared with prior art, there is advantages that
1. base fluid has relatively low viscosity, easy infusion, can enter high permeability zone by selectivity, and leak-off is low, the injury to substrate Rate is little；
2. carboxylic first (second) base enclosure polysaccharide is in complicated double-spiral structure, and steric effect is relatively big, can effectively extend to become on the spot The glue time, it is achieved the indepth plugging of gel rubber system；
3. heatproof, antiacid carboxylic first (second) base enclosure polysaccharide introduce anti-salt groups, form temperature-resistant anti-salt, acid-proof gel rubber system；
4. reservoir temperature 80 DEG C～130 DEG C, the initial gelation time control of base fluid is formed motionless solidifying after 48-72h, final set Glue；
5. reservoir temperature 130 DEG C, high salinity 10 × 104Mg/L, in or highly acid (pH 2～5) condition, gel is 3 Keep stable in individual month, the sealing ratiod of fracture reach 85% and more than, can realize CO2The permanently effective closure of has channeling.
Accompanying drawing explanation
Fig. 1 is the anti-CO of high temperature and high salt oil deposit of the present invention2The microstructure of has channeling blocking agent.
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing, the present invention will be further described, but is not intended to the present invention.
One, the anti-CO of high temperature and high salt oil deposit2Has channeling blocking agent formula designs
Percentage ratio in case study on implementation is mass percent, and chemical reagent used is technical grade product.In proportion by group The various components becoming gel rubber system are added to the water, and stir, and test in making bottle at 130 DEG C, according to range estimation code method (table 1) gelation time and gelling strength are judged.
Table 1 gel strength range estimation code standard
Embodiment 1
Carboxymethyl chitosan 1%, AM 3.5%～6.2%, AA 0.25%, AMC12S or AMC14S 0.05%, AIBA 0.008%, phenolic crosslinkers 0.8%, remaining is water.Gelation time is 48-84h, and final set is I～J level.
The anti-CO of table 22Alter blocking agent embodiment 1 plastic situation
AM (%) 10h 24h 36h 42h 48h 54h 72h 84h 96h 108h 120h
3.5 A A+ B B C C E E I I I
5.1 A B B C E F I- I I I+ I+
6.2 A+ C C D G H I J J J J
Embodiment 2
Carboxyetbyl chitosan 2%, AM 3.5%～6.2%, AA 1%, N-vinylpyridine network alkanone 0.06%, AIBA 0.01%, phenolic crosslinkers 1.0%, remaining is water.Gelation time is 48-72h, and final set is G～J level.
The anti-CO of table 32Alter blocking agent embodiment 2 plastic situation
AM (%) 10h 24h 36h 42h 48h 54h 72h 84h 96h 108h 120h
3.5 A A+ B C D E E G G G G
5.1 A+ C D E E F G G I I I
6.2 A+ C C D F I I J J J J
Embodiment 3
Carboxyetbyl chitosan 1.5%, AM 4～6%, AA 0.75%, 2-acrylamido-2-methylpropene sodium sulfonate 0.1%, (NH4)2S2O8-NaHSO30.012%, phenolic crosslinkers 1.2%, remaining is water.Gelation time is 48-60h, and final set is G～I level.
The anti-CO of table 42Alter blocking agent embodiment 3 plastic situation
AM (%) 10h 24h 36h 42h 48h 54h 72h 84h 96h 108h 120h
4 A C D F E G G G G G G
5 A D- E G H I I I I I I
6 A D F G H I I I I I I
Embodiment 4
Carboxyetbyl chitosan 1.5%, AM 4～6%, AA 0.75%, sodium vinyl sulfonate 0.08%, (NH4)2S2O8- NaHSO30.012%, phenolic crosslinkers 1.0%, remaining is water.Gelation time is 48-72h, and final set is I～J level.
The anti-CO of table 52Alter blocking agent embodiment 4 plastic situation
AM (%) 10h 24h 36h 42h 48h 54h 72h 84h 96h 108h 120h
4 A C D F H G G G G G G
5 A C D E- I- I I I I I I
6 A D E H G G+ I J J J J
Two, the anti-CO of high temperature and high salt oil deposit2The microstructure (as a example by embodiment 1 gel) of has channeling blocking agent
The border surface sweeping Electronic Speculum of the gel after final set is as it is shown in figure 1, carboxymethyl chitosan is thick cell wall-like, tightly Snarling gel formation is fine and close, more regular network structure；The gel microstructure of another part is the form of one integrated mass. May determine that, the microstructure of this gel uniqueness necessarily gives the performance of its excellence.
Three, the anti-CO of high temperature and high salt oil deposit2The temperature-resistant anti-salt of has channeling blocking agent, acid resistance evaluation (with embodiment 2 gel are Example)
Gel after final set according to mass ratio 1:0.2 amount add acid brine (pH 2～5, total salinity 10%, its In, CaCl2Mass concentration 0.32%, MgCl2Mass concentration 0.16%, NaCl mass concentration 9%, Na2SO40.52%, ackd salt In water, thiourea mass concentration is 0.005%).The long-time stability of 130 DEG C of condition gels are shown in Table 6.90d is dehydrated.
The anti-CO of table 62Alter the blocking agent long-time stability at high temperature and high salt acid condition
Four, high temperature and high salt oil deposit CO2Has channeling blocking agent sealing characteristics evaluates (as a example by embodiment 2 gel)
Constant voltage constant speed pump (model ES-V) with 1ml/min flow velocity displacement acid brine (pH 2.5, total salinity 10%, its In, CaCl2Mass concentration 0.32%, MgCl2Mass concentration 0.16%, NaCl mass concentration 9%, Na2SO40.52%) to artificial Microcrack Sandstone Cores (2.5cm × 7.1cm, matrix permeability 1～5mD), measures permeability (K after pressure stabilityb)；Rock subsequently Inject in the heart the blocking agent base fluid (AM 5.1%, other monomer, initiator and cross-linking agent mass concentration are with embodiment 2) of 1PV, stop Repeating acid brine displacement after pump, 130 DEG C of maintenance 15d, after measuring breakthrough pressure gradient and the pressure stability of blocking agent, rock core oozes Rate (K thoroughlyf), according to η=(1-Kf/Kb) × 100%, calculates blocking agent post-breakthrough sealing ratiod η.Result is as shown in table 7.
The residual resistance factor of the hyperbranched slow swollen property granule of table 7 and sealing ratiod
As known from Table 7, blocking agent base fluid can effectively enter microcrack, and high temperature and high salt, strong acidic environment are to microcrack rock core Sealing ratiod be up to 85% and more than.After pressure breakthrough, the permeability of rock core shows higher than matrix permeability, and blocking agent is to substrate Permeability injury is low.

Claims (4)

1. the anti-CO of high temperature and high salt oil deposit2Has channeling blocking agent, by carboxylic first (second) base enclosure polysaccharide, acrylamide, temperature-resistant anti-salt monomer, Acrylic acid is reaction monomers, with phenol, formaldehyde as cross-linking agent, with azo-bis-isobutyrate hydrochloride, azodiisobutyronitrile or (NH4)2S2O8-NaHSO3System is initiator, and the polymerization of monomer molecule synchronization carries out being formed in situ gel with crosslinking under formation conditions, Its structural formula is as follows:
N=10 or 12, R are CH3Or C2H5
Wherein: v, w, x, y, z are the mass percent of construction unit, v is 3.5～7.5%, and w is 65～75%, x be 0.5～ 5%, y are 5～10%, z=1-v-w-x-y；
Described carboxylic first (second) base enclosure polysaccharide is carboxymethyl chitosan or carboxyetbyl chitosan, and weight average molecular weight is 2～5 × 104g/ Mol, deacetylation is 45～87%, and its structural formula is as follows:
R is CH3Or C2H5；
Described temperature-resistant anti-salt monomer is the acid of 2-alkyl acrylamide dodecyl or the acid of 2-alkyl acrylamide myristyl, its knot Structure formula is as follows:
N=10 or 12.
2. a kind of anti-CO of high temperature and high salt oil deposit as claimed in claim 12Has channeling blocking agent, it is characterised in that described temperature-resistant anti-salt list Body can also is that N-vinylpyridine network alkanone, 2-acrylamido-2-methylpropene sodium sulfonate or sodium vinyl sulfonate.
3. the anti-CO of high temperature and high salt oil deposit as claimed in claim 1 or 22The preparation method of has channeling blocking agent, includes following step successively Rapid:
(1) preparation blocking agent base fluid, blocking agent base fluid is made up of by weight percent following components: carboxylic first (second) base enclosure polysaccharide 1～ 2%, acrylamide 3.5～6.2%, acrylic acid 0.25～1%, temperature-resistant anti-salt monomer 0.02～0.1%, initiator 0.008～ 0.12%, phenol, formaldehyde crosslinking agent 0.5～1.2%, remaining is clear water, saline or oilfield injection water；
(2) pumping in stratum by described blocking agent base fluid, under formation conditions, the polymerization of monomer is synchronization carried out, on the spot with crosslinking Form motionless gel.
4. the anti-CO of high temperature and high salt oil deposit as claimed in claim 32The preparation method of has channeling blocking agent, it is characterised in that described benzene In phenol, formaldehyde crosslinking agent, phenol, the mass ratio of formaldehyde are 1:3.
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CN110872504A (en) * 2019-12-09 2020-03-10 中国石油集团川庆钻探工程有限公司工程技术研究院 Acid-resistant strong gel plugging agent and preparation method thereof
CN110903816A (en) * 2019-12-17 2020-03-24 西南石油大学 Temperature-resistant salt-resistant high-expansion plugging agent for plugging large cracks and preparation method thereof
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