CN112745811B - Plugging agent for drilling fluid and preparation method thereof - Google Patents
Plugging agent for drilling fluid and preparation method thereof Download PDFInfo
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- CN112745811B CN112745811B CN201911040835.9A CN201911040835A CN112745811B CN 112745811 B CN112745811 B CN 112745811B CN 201911040835 A CN201911040835 A CN 201911040835A CN 112745811 B CN112745811 B CN 112745811B
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- microcapsule
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- 238000005553 drilling Methods 0.000 title claims abstract description 42
- 239000012530 fluid Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title abstract description 9
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 75
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000003094 microcapsule Substances 0.000 claims abstract description 27
- 239000003822 epoxy resin Substances 0.000 claims abstract description 24
- 239000003607 modifier Substances 0.000 claims abstract description 24
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 24
- 239000010426 asphalt Substances 0.000 claims abstract description 21
- 239000004568 cement Substances 0.000 claims abstract description 14
- 239000007787 solid Substances 0.000 claims abstract description 14
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 39
- 239000007864 aqueous solution Substances 0.000 claims description 33
- 238000003756 stirring Methods 0.000 claims description 33
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 21
- 239000004593 Epoxy Substances 0.000 claims description 20
- 238000006243 chemical reaction Methods 0.000 claims description 17
- 238000010438 heat treatment Methods 0.000 claims description 17
- 239000002775 capsule Substances 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 14
- 150000001299 aldehydes Chemical class 0.000 claims description 12
- 150000001412 amines Chemical class 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 10
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 9
- 229920000768 polyamine Polymers 0.000 claims description 9
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 9
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 6
- FDLQZKYLHJJBHD-UHFFFAOYSA-N [3-(aminomethyl)phenyl]methanamine Chemical compound NCC1=CC=CC(CN)=C1 FDLQZKYLHJJBHD-UHFFFAOYSA-N 0.000 claims description 6
- 150000002989 phenols Chemical class 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 5
- ZTQSAGDEMFDKMZ-UHFFFAOYSA-N Butyraldehyde Chemical compound CCCC=O ZTQSAGDEMFDKMZ-UHFFFAOYSA-N 0.000 claims description 4
- HUMNYLRZRPPJDN-UHFFFAOYSA-N benzaldehyde Chemical compound O=CC1=CC=CC=C1 HUMNYLRZRPPJDN-UHFFFAOYSA-N 0.000 claims description 4
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 4
- 150000001768 cations Chemical group 0.000 claims description 4
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- QWVGKYWNOKOFNN-UHFFFAOYSA-N o-cresol Chemical compound CC1=CC=CC=C1O QWVGKYWNOKOFNN-UHFFFAOYSA-N 0.000 claims description 4
- 239000003208 petroleum Substances 0.000 claims description 4
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 claims description 4
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 3
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 3
- WZCQRUWWHSTZEM-UHFFFAOYSA-N 1,3-phenylenediamine Chemical compound NC1=CC=CC(N)=C1 WZCQRUWWHSTZEM-UHFFFAOYSA-N 0.000 claims description 2
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims description 2
- 238000009775 high-speed stirring Methods 0.000 claims description 2
- 229940018564 m-phenylenediamine Drugs 0.000 claims description 2
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims description 2
- QNGNSVIICDLXHT-UHFFFAOYSA-N para-ethylbenzaldehyde Natural products CCC1=CC=C(C=O)C=C1 QNGNSVIICDLXHT-UHFFFAOYSA-N 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 238000000967 suction filtration Methods 0.000 claims description 2
- HGBOYTHUEUWSSQ-UHFFFAOYSA-N valeric aldehyde Natural products CCCCC=O HGBOYTHUEUWSSQ-UHFFFAOYSA-N 0.000 claims description 2
- 125000003916 ethylene diamine group Chemical group 0.000 claims 1
- 230000003211 malignant effect Effects 0.000 abstract description 5
- 238000009991 scouring Methods 0.000 abstract description 5
- 239000010410 layer Substances 0.000 description 13
- 239000000463 material Substances 0.000 description 11
- 239000002002 slurry Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 7
- 238000004945 emulsification Methods 0.000 description 6
- 235000019333 sodium laurylsulphate Nutrition 0.000 description 6
- 238000001914 filtration Methods 0.000 description 5
- 230000014759 maintenance of location Effects 0.000 description 5
- 230000035484 reaction time Effects 0.000 description 5
- 238000001291 vacuum drying Methods 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 125000002091 cationic group Chemical group 0.000 description 4
- 239000004848 polyfunctional curative Substances 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- 230000018044 dehydration Effects 0.000 description 3
- 238000006297 dehydration reaction Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000003999 initiator Substances 0.000 description 3
- 239000000178 monomer Substances 0.000 description 3
- 238000006116 polymerization reaction Methods 0.000 description 3
- 239000000440 bentonite Substances 0.000 description 2
- 229910000278 bentonite Inorganic materials 0.000 description 2
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 2
- 235000019994 cava Nutrition 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 239000003431 cross linking reagent Substances 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000839 emulsion Substances 0.000 description 2
- 239000008398 formation water Substances 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229940092782 bentonite Drugs 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000012792 core layer Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229940080314 sodium bentonite Drugs 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
Classifications
-
- 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
- C09K8/42—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
- C09K8/426—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells for plugging
-
- 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
- C09K8/02—Well-drilling compositions
- C09K8/03—Specific additives for general use in well-drilling compositions
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Epoxy Resins (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a plugging agent for drilling fluid and a preparation method thereof. The plugging agent comprises the following components in parts by weight: emulsified asphalt: 100 parts of waterborne epoxy resin: 10-40 parts of microcapsule modifier, 10-40 parts of cement: 1 to 10 portions. The plugging agent can effectively reside at the entrance of a large crack, a karst cave and other malignant leakage stratum to form a solid seal, and particularly, the resident plugging capability and the water scouring resistance are improved under high temperature and high pressure, so that the plugging success rate is improved.
Description
Technical Field
The invention relates to the field of petroleum drilling plugging, in particular to a plugging agent for drilling fluid and a preparation method thereof.
Background
Lost circulation is a common and often encountered complex problem in oil and gas drilling. The well leakage causes underground accidents, has great harm to the well drilling and well completion construction, and is always an urgent problem to be solved in the petroleum engineering field. In the drilling operation, once the well leakage occurs, the time is delayed, the drilling fluid is lost, the hydrocarbon reservoir is damaged, the instability of the well wall can be caused, a series of complex conditions and accidents such as well collapse, drilling sticking and blowout are caused, even the well hole is scrapped, and the great economic loss is caused.
Particularly, in the drilling process of oil and gas deep wells in high mountain areas, the number of complicated lost-circulation strata such as large cracks and karst caves during drilling is increased remarkably, and the method becomes one of the main technical problems which troubles the smooth operation of oil and gas exploration and development. The leakage treatment difficulty is higher because the leakage passage of the leakage stratum has large size, low leakage pressure, water-containing stratum and frequent well leakage. At present, the technologies for treating large-crack and karst-cave type leakage mainly comprise a large-particle and high-concentration bridge plugging leakage-stopping slurry technology, a cement slurry leakage-stopping technology and the like. Because the leakage channel is large, the difficulty of realizing high-strength plugging by only using bridging materials is large. Due to reasons such as formation water outflow and the like, the staying capacity of cement paste in a leaking layer is insufficient, and the cement paste diluted by formation water cannot form an effective sealing layer.
CN102504776A discloses a plugging agent for malignant leakage and a preparation method thereof, in the method, firstly, an organic monomer is dissolved in water, an initiator is added for polymerization reaction, and then, a high molecular copolymer is obtained by precipitation and drying. Then the copolymer is prepared into aqueous solution, and sodium dodecyl benzene sulfonate and bentonite clay are added to prepare the plugging agent. The plugging agent obtained by the scheme can be used for plugging a leaking layer and is suitable for plugging a large crack in the drilling process. However, the plugging material is easily diluted by formation fluid in the formation, and the cementing strength of the diluted plugging material is greatly reduced, so that the retention capacity is reduced and the like.
CN104388066A discloses a preparation method of a plugging agent for drilling fluid, which comprises the steps of adding organic monomers into white oil to form a dispersion phase in water for emulsification, then adding an initiator to carry out polymerization reaction to obtain a polymer emulsion, and then adding a phase inversion agent, a cross-linking agent and an inert bridging material to obtain the plugging agent for drilling. Compared with the scheme of the patent, the principle of the method is basically the same, the method is used for preparing the polymer, but the polymer is not precipitated after the polymerization reaction, and the phase inversion and thickening are carried out quickly after the phase inversion agent is added subsequently to form a viscoelastic gel resident plugging slug to form plugging. The crosslinking agent is utilized to further generate crosslinking reaction in the resident plugging slug, thereby improving the strength of the slug and further improving the leakage pressure. Although the plugging capacity is improved compared with the prior patent, the plugging material has the problems that the plugging material is easily diluted by formation fluid in the formation, the cementing strength of the diluted plugging material is greatly reduced, the retention capacity is reduced and the like.
CN102618230A discloses a controllable cross-linked gel water plugging and leakage stopping material for oil and gas fields, which is prepared by reacting an organic monomer in an aqueous solution through an initiator to prepare water-absorbent resin, then continuously reacting in an oil phase and repeatedly wrapping to obtain particles, adding the particles into an HPAM aqueous solution to perform cross-linking reaction to obtain immobile gel which can plug crack-type and karst cave-type leakage stratums, but the leakage stopping material has a complex manufacturing process and poor fluidity in pipelines and drill strings.
CN110003864A discloses a drilling fluid inner plugging agent and a preparation method thereof, the method uses resin as a main agent, adopts a latent curing agent with a microcapsule structure, a core layer is an amine curing agent, and a wall layer is a high-toughness engineering plastic polymer, and can solve the problem of contradiction between long working period for plugging resin and fast curing speed. In addition, because the main agent adopts resin, the cured product has high hardness, poor viscoelasticity and poor adaptability to different sizes of cracks and holes, and is difficult to achieve a good leaking stoppage effect.
At present, although a large amount of research work on plugging materials is carried out aiming at the leakage of large cracks and karst caves, the problems of poor staying capability of the plugging materials in leakage channels, weak water dilution resistance and scouring resistance, low plugging strength and the like still exist. Particularly, under the condition of high-temperature use, the success rate of large cracks and karst cave type leakage loss plugging is very low, and the loss is serious.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the plugging agent for the drilling fluid and the preparation method thereof, the plugging agent can effectively reside and form a solid seal at the entrance of a malignant leakage stratum such as a large crack, a karst cave and the like, and particularly improves the resident plugging capability and the water scouring resistance under high temperature and high pressure, thereby improving the plugging success rate.
The invention provides a plugging agent for drilling fluid, which comprises the following components in parts by weight:
100 parts of emulsified asphalt (by weight),
10 to 40 parts of water-based epoxy resin
10 to 40 parts of microcapsule modifier,
1 to 10 parts of cement.
The emulsified asphalt is cation emulsified petroleum asphalt with solid content not less than 50%.
The waterborne epoxy resin is bisphenol A waterborne epoxy resin, the epoxy equivalent is 180 to 280 g/equivalent, the solid content is 45 to 65 percent, and the preferred is that: one or more of CYDW-100 type waterborne epoxy resin and E-44 type waterborne epoxy resin.
The microcapsule modifier comprises a capsule wall and a capsule core arranged in the capsule wall, and the particle size is 5-20 mu m.
The capsule wall is polymethyl methacrylate. The capsule core is a mixture of a modified amine waterborne epoxy curing agent and an accelerant.
The weight ratio of the capsule wall to the capsule core is 1 to 1. The weight ratio of the modified amine waterborne epoxy curing agent to the accelerator is 5 to 1.
Wherein the amine value of the modified amine waterborne epoxy curing agent is 80-220 mgKOH/g, and the solid content is 40-80%; the modified amine waterborne epoxy curing agent is one or more of WE-8300, WE-8309 and WE-8325. The accelerator comprises a product obtained by reacting polyamine, phenols and an aldehyde-containing aqueous solution, wherein the weight ratio of the polyamine to the phenols to the aldehyde-containing aqueous solution is as follows: 1 to 3.
The polyamine is one or more of ethylenediamine, hexamethylenediamine, diethylenetriamine, m-xylylenediamine and m-phenylenediamine, and preferably the ethylenediamine and the m-xylylenediamine; the phenols are one or more of phenol, o-cresol and resorcinol, preferably phenol; the aldehyde-containing aqueous solution is an aqueous solution containing one or more of formaldehyde, butyraldehyde and benzaldehyde, and preferably an aqueous solution containing formaldehyde; the mass concentration of the aldehyde-containing aqueous solution is 35-40%.
The invention provides a preparation method of the plugging agent for the drilling fluid, which comprises the following steps:
(1) Preparing a microcapsule modifier;
(2) And (2) uniformly mixing the emulsified asphalt and the water-based epoxy resin according to a certain proportion, adding the cement, continuously stirring, adding the microcapsule modifier prepared in the step (1), and uniformly stirring to obtain the plugging agent for the drilling fluid.
The specific steps for preparing the microcapsule modifier in the step (1) comprise:
i) Mixing polyamine and phenolic substances, heating and dissolving, then adding an aldehyde-containing aqueous solution, reacting, and dehydrating to obtain the accelerator.
ii) dissolving polymethyl methacrylate in dichloromethane, then adding the modified amine waterborne epoxy curing agent and the prepared accelerator, and uniformly stirring to form a dispersed phase; and (2) taking a sodium dodecyl sulfate aqueous solution as a continuous phase, dropwise adding the dispersed phase into the continuous phase, stirring at a high speed, reacting under certain conditions after dropwise adding, stirring at a low speed, and performing suction filtration, washing and drying after the reaction to obtain the microcapsule modifier.
In the step i), the temperature for heating and dissolving is 40-90 ℃; the aldehyde-containing aqueous solution is slowly added dropwise, and the reaction conditions are as follows: reacting for 1.0 to 4.0 hours at the temperature of 50 to 120 ℃, and dehydrating by heating to 150 to 200 ℃ and vacuumizing.
In the step ii), the mass concentration of the sodium dodecyl benzene sulfonate aqueous solution is 1.0-1.5%.
The rotating speed of the high-speed stirring is 1000 to 3000r/min, and the rotating speed of the low-speed stirring is 500 to 800r/min.
The reaction conditions are as follows: and reacting at 35 to 45 ℃ for 3 to 8 hours. The reaction is preferably carried out under the conditions of a thermostatic water bath. Wherein dichloromethane is completely volatilized during the reaction.
The washing is carried out by firstly using ethanol and then using deionized water, and the washing can be repeated for many times.
The drying condition is drying at 50 to 80 ℃ for 10 to 20 hours.
The plugging agent for the drilling fluid can be used for plugging operation in water-based drilling fluid, can be prepared into plugging slurry firstly and then added into the water-based drilling fluid, and is particularly suitable for large cracks and hole type leaking layers.
The plugging agent for the drilling fluid can quickly form a high-softening-point modified asphalt elastomer in a large-crack and karst cave type leaking layer, has strong water dilution resistance and scouring resistance, has strong high-temperature resistance, and can meet the plugging requirement of malignant leakage.
Compared with the prior art, the invention has the following advantages:
(1) The invention adopts the microcapsule to temporarily seal the curing agent and the specific accelerator without contacting with the epoxy resin, so that all components in the plugging agent can uniformly and stably exist. The rheological property of the drilling fluid is not influenced at the initial stage of adding the drilling fluid.
(2) When the plugging agent for the drilling fluid is used as a plugging agent while drilling, the capsule wall is broken under a certain pressure when the plugging agent reaches the underground, so that the curing agent and the accelerator are contacted with other components to react, the modified asphalt with good elasticity and high strength is obtained, and a leaking layer can be effectively plugged.
(3) The invention adopts the waterborne epoxy resin and the emulsified asphalt as main agents, and the emulsified asphalt and the waterborne epoxy resin are both in an emulsion form, so that the emulsified asphalt can be more easily and fully contacted with the subsequent waterborne epoxy curing agent in the water-based drilling fluid and can react with the subsequent waterborne epoxy curing agent to form an organic whole. In addition, when drilling fluid is added, the drilling fluid is easier to flow, can quickly reach a leaking layer, and completes leaking stoppage.
(4) The plugging agent can continue to generate a curing reaction in the plugging section, improves the plugging strength, does not depend on the size of a crack during plugging, and is particularly suitable for plugging large cracks and other malignant leakage stratums.
(5) The specific accelerator added into the plugging agent is beneficial to coordinating the coordination of other components, thereby improving the plugging effect on the whole.
Detailed Description
The following non-limiting examples are presented to enable those of ordinary skill in the art to more fully understand the present invention and are not intended to limit the invention in any way. In addition, the percentages referred to in the present invention, which are not specifically mentioned, are mass percentages.
Example 1
Adding 48g of m-xylene diamine and 31.5g of phenol into a reactor, stirring, heating to dissolve, slowly dropwise adding 35.7g of aqueous solution containing 37wt% of formaldehyde at 80 ℃, completing dripping for 60min, reacting for 3.0h at 90 ℃, heating to 175 ℃, and vacuumizing for dehydration to obtain the accelerator.
25g of polymethyl methacrylate was dissolved in methylene chloride, 73.6g of WE-8325 type aqueous epoxy hardener and 16.4g of the above-prepared accelerator were added thereto, and the mixture was uniformly distributed by a homogenizer for 20 minutes to form a dispersed phase. A 1.0% aqueous solution of sodium lauryl sulfate was added as a continuous phase to a three-necked flask. Dropwise adding the dispersed phase into the continuous phase while stirring at normal temperature, and stirring at a high speed of 2500r/min for emulsification; then placing the three-neck flask in a constant-temperature water bath at 40 ℃, reducing the stirring speed to 550r/min until the dichloromethane is completely volatilized, wherein the reaction time is 3.5h; and (3) after the reaction is finished, pouring out, standing and filtering, washing with ethanol and deionized water for multiple times, putting into a vacuum drying oven, and drying at 75 ℃ for 12 hours to obtain the microcapsule modifier.
200g of cationic emulsified asphalt (solid content is 52 percent) and 66.6g of CYDW-100 aqueous epoxy resin are added into a stirrer to be uniformly mixed, 5.8g of cement is added to be continuously stirred and mixed, and finally 48.8g of the prepared microcapsule modifier is added to be uniformly stirred to obtain the plugging agent for the drilling fluid.
Example 2
Adding 64.2g of ethylenediamine and 37.5g of phenol into a reactor, stirring, heating to dissolve, slowly dropwise adding 49.2g of aqueous solution containing 37wt% of formaldehyde at 55 ℃, completing dropping for 70min, reacting at 85 ℃ for 2.5h, heating to 170 ℃, and vacuumizing to dehydrate to obtain the accelerator.
28g of polymethyl methacrylate was dissolved in methylene chloride, 100g of WE-8300 type aqueous epoxy hardener and 31.3g of the above-prepared accelerator were added, and the mixture was uniformly distributed by a homogenizer for 25 minutes to form a dispersed phase. A 1.0% aqueous solution of sodium lauryl sulfate was added as a continuous phase to a three-necked flask. Dropwise adding the dispersed phase into the continuous phase while stirring at normal temperature, and stirring at a high speed of 2200r/min for emulsification; then placing the three-neck flask in a constant-temperature water bath at 45 ℃, reducing the stirring speed to 650r/min until the dichloromethane is completely volatilized, and ensuring the reaction time to be 5h; and (3) after the reaction is finished, pouring out, standing and filtering, washing with ethanol and deionized water for multiple times, putting into a vacuum drying oven, and drying for 15 hours at 65 ℃ to obtain the microcapsule modifier.
200g of cationic emulsified asphalt (solid content is 55 percent) and 58.5g of CYDW-100 waterborne epoxy resin are added into a stirrer to be uniformly mixed, 8.2g of cement is added to be continuously stirred and mixed, and finally 38.5g of the prepared microcapsule modifier is added to be uniformly stirred to obtain the plugging agent for the drilling fluid.
Example 3
Adding 47.6g of m-xylene diamine and 24.2g of phenol into a reactor, stirring, heating for dissolving, slowly dripping 35.7g of 35wt% of formaldehyde-containing aqueous solution at 75 ℃, finishing dripping for 45min, reacting for 3.5h at 100 ℃, heating to 180 ℃, and vacuumizing for dehydrating to obtain the accelerator.
35g of polymethyl methacrylate was dissolved in methylene chloride, 87.2g of WE-8309 type aqueous epoxy hardener and 24.8g of the above-prepared accelerator were added thereto, and the mixture was uniformly distributed for 30 minutes by a homogenizer to form a dispersed phase. A 1.0% aqueous solution of sodium lauryl sulfate was added as a continuous phase to a three-necked flask. Dropwise adding the dispersed phase into the continuous phase while stirring at normal temperature, and stirring at a high speed of 2600r/min for emulsification; then placing the three-neck flask in a constant temperature water bath at 40 ℃, reducing the stirring speed to 700r/min until the dichloromethane is completely volatilized, wherein the reaction time is 4.5h; and after the reaction is finished, pouring out, standing and filtering, washing with ethanol and deionized water for multiple times, putting into a vacuum drying oven, and drying for 14 hours at 70 ℃ to obtain the microcapsule modifier.
Adding 200g of cation emulsified asphalt (solid content is 50 percent) and 37.4g E-44 aqueous epoxy resin into a stirrer to be uniformly mixed, adding 7.0g of cement to be continuously stirred and mixed, and finally adding 47.6g of the prepared microcapsule modifier to be uniformly stirred to obtain the plugging agent for the drilling fluid.
Example 4
Adding 50.5g of ethylenediamine and 27.2g of phenol into a reactor, stirring, heating to dissolve, slowly dropwise adding 44.2g of aqueous solution containing 37wt% of formaldehyde at 75 ℃, finishing dropping for 50min, reacting for 3.0h at 95 ℃, heating to 170 ℃, and vacuumizing for dehydration to obtain the accelerator.
46g of polymethyl methacrylate was dissolved in methylene chloride, 106.7g of WE-8300 type aqueous epoxy hardener and 26.8g of the above-prepared accelerator were added thereto, and the mixture was uniformly distributed by a homogenizer for 25 minutes to form a dispersed phase. A 1.0% aqueous solution of sodium lauryl sulfate was added as a continuous phase to a three-necked flask. At normal temperature, dropwise adding the dispersed phase into the continuous phase while stirring, and stirring at a high speed of 2500r/min for emulsification; then placing the three-neck flask in a constant-temperature water bath at 45 ℃, reducing the stirring speed to 600r/min until the dichloromethane is completely volatilized, wherein the reaction time is 4.0h; and pouring out, standing and filtering after the reaction is finished, sequentially washing the mixture for multiple times by using ethanol and deionized water, putting the washed mixture into a vacuum drying oven, and drying the mixture for 10 hours at the temperature of 75 ℃ to obtain the microcapsule modifier.
200g of cationic emulsified asphalt (solid content is 55 percent) and 70.5g of CYDW-100 aqueous epoxy resin are added into a stirrer to be uniformly mixed, 6.4g of cement is added to be continuously stirred and mixed, and finally 74.2g of the prepared microcapsule modifier is added to be uniformly stirred to obtain the plugging agent for the drilling fluid.
Comparative example 1
46g of polymethyl methacrylate is dissolved in dichloromethane, 106.7g of WE-8300 type waterborne epoxy curing agent is added, and the mixture is uniformly divided by a homogenizer for 25min to form a dispersed phase. A 1.0% aqueous solution of sodium lauryl sulfate was added as a continuous phase to a three-necked flask. Dropwise adding the dispersed phase into the continuous phase while stirring at normal temperature, and stirring at a high speed of 2500r/min for emulsification; then placing the three-neck flask in a constant-temperature water bath at 45 ℃, reducing the stirring speed to 600r/min until the dichloromethane is completely volatilized, wherein the reaction time is 4.0h; and (3) after the reaction is finished, pouring out, standing and filtering, washing with ethanol and deionized water for multiple times, putting into a vacuum drying oven, and drying for 10 hours at 75 ℃ to obtain the microcapsule modifier.
200g of cationic emulsified asphalt (solid content is 55 percent) and 70.5g of CYDW-100 aqueous epoxy resin are added into a stirrer to be uniformly mixed, 6.4g of cement is added to be continuously stirred and mixed, and finally 74.2g of the prepared microcapsule modifier is added to be uniformly stirred to obtain the plugging agent for the water-based drilling fluid.
Comparative example 2
Adding 50.5g of ethylenediamine and 27.2g of phenol into a reactor, stirring, heating to dissolve, slowly dropwise adding 44.2g of aqueous solution containing 37wt% of formaldehyde at 75 ℃, finishing dropping for 50min, reacting for 3.0h at 95 ℃, heating to 170 ℃, and vacuumizing for dehydration to obtain the accelerator.
200g of cation emulsified asphalt (solid content is 55 percent) and 70.5g of CYDW-100 water-based epoxy resin are added into a stirrer to be uniformly mixed, 6.4g of cement is added to be continuously stirred and mixed, and finally 59.4g of WE-8300 type water-based epoxy curing agent and 14.8g of the prepared accelerating agent are added to be uniformly stirred, so that the plugging agent for the drilling fluid is obtained.
A sand layer made of sand stones of 0.5-2.0 cm is adopted to simulate a large-pore leakage layer so as to simulate the use performance of the plugging agent tested by a leakage layer tester in the water-based drilling fluid.
The plugging agent and the base slurry in example 1~4 and the comparative example are prepared into plugging slurry according to 1:1, wherein 2.75g of anhydrous sodium carbonate and 60g of bentonite are added into the base slurry per 1000mL of water, and the plugging slurry is obtained by stirring at a high speed for 20min and maintaining at room temperature for 24 h.
Then squeezing the plugging slurry into a simulated leakage layer by using a constant flow pump, heating to 120 ℃, gradually pressurizing to 3.5 MPa, curing for 90min, carrying out squeezing test by using clear water 2 times of the plugging slurry, and measuring squeezing pressure, namely representing the retention capacity and the pressure-bearing capacity. The specific test results are shown in table 1.
In the comparative example 2, because the microcapsule structure is not prepared, when the plugging agent is prepared, the water-based epoxy resin is directly contacted with the water-based epoxy curing agent and the accelerator to carry out curing reaction, so that the viscosity of the plugging agent is increased and the plugging agent is cured, and the plugging agent cannot be applied to drilling fluid.
TABLE 1 lost circulation performance of example 1~4 and comparative examples
| Dwell Capacity before curing/MPa | Bearing capacity/MPa after curing | |
| Example 1 | 3.2 | 14.5 |
| Example 2 | 2.8 | 13.8 |
| Example 3 | 2.5 | 13.2 |
| Example 4 | 3.4 | 15 |
| Comparative example 1 | 2.6 | 6.2 |
| Comparative example 2 | - | - |
The test results show that after 2 times of clear water is extruded into the plugging agent, the plugging agent has good retention capacity before curing and pressure-bearing capacity after curing in a simulated leakage layer of sandstone with the thickness of 0.5-2.0 cm, and the plugging agent for the drilling fluid has the advantages of strong water scouring resistance, strong retention capacity and high plugging and pressure-bearing capacity, and can be used for large-hole leakage stratum.
Claims (17)
1. The plugging agent for the drilling fluid comprises the following components in parts by weight:
100 parts of emulsified asphalt, namely 100 parts of emulsified asphalt,
10 to 40 parts of waterborne epoxy resin
10 to 40 parts of a microcapsule modifier,
1 to 10 parts of cement;
the microcapsule modifier comprises a capsule wall and a capsule core arranged in the capsule wall, wherein the capsule wall is made of polymethyl methacrylate; the capsule core is a mixture of a modified amine waterborne epoxy curing agent and an accelerant.
2. A plugging agent according to claim 1, characterized in that: the emulsified asphalt is cation emulsified petroleum asphalt with solid content not less than 50%.
3. A plugging agent according to claim 1, characterized in that: the epoxy resin is bisphenol A type waterborne epoxy resin, the epoxy equivalent is 180-280 g/equivalent, and the solid content is 45-65%.
4. A plugging agent according to claim 3, characterized in that: the epoxy resin is one or more of CYDW-100 type waterborne epoxy resin and E-44 type waterborne epoxy resin.
5. A plugging agent according to claim 1, characterized in that: the particle size of the microcapsule modifier is 5-20 mu m.
6. A plugging agent according to claim 1, characterized in that: the weight ratio of the capsule wall to the capsule core is 1 to 1.
7. A plugging agent according to claim 1, characterized in that: the amine value of the modified amine waterborne epoxy curing agent is 80-220mgKOH/g, and the solid content is 40-80%; the modified amine waterborne epoxy curing agent is one or more of WE-8300, WE-8309 and WE-8325.
8. A plugging agent according to claim 1, characterized in that: the accelerator comprises a product obtained by reacting polyamine, phenols and an aldehyde-containing aqueous solution, wherein the weight ratio of the polyamine to the phenols to the aldehyde-containing aqueous solution is as follows: 1 to 3.
9. A plugging agent according to claim 8, characterized in that: the polyamine is one or more of ethylenediamine, hexamethylenediamine, diethylenetriamine, m-xylylenediamine and m-phenylenediamine; the phenols are one or more of phenol, o-cresol and resorcinol; the aldehyde-containing aqueous solution is an aqueous solution containing one or more of formaldehyde, butyraldehyde and benzaldehyde, and the mass concentration of the aldehyde-containing aqueous solution is 35-40%.
10. A plugging agent according to claim 9, characterized in that: the polyamine is ethylenediamine and/or m-xylylenediamine; the phenol is phenol; the aqueous solution containing aldehyde is an aqueous solution containing formaldehyde.
11. A method for preparing a plugging agent according to any one of claims 1 to 10, comprising the steps of:
(1) Preparing a microcapsule modifier;
(2) And (2) uniformly mixing the emulsified asphalt and the water-based epoxy resin according to a certain proportion, adding the cement, continuously stirring, adding the microcapsule modifier prepared in the step (1), and uniformly stirring to obtain the plugging agent for the drilling fluid.
12. The method of claim 11, wherein: the specific steps for preparing the microcapsule modifier in the step (1) comprise:
i) Mixing polyamine and phenolic substances, heating and dissolving, then adding an aldehyde-containing aqueous solution, reacting, and dehydrating to obtain an accelerator;
ii) dissolving polymethyl methacrylate in dichloromethane, then adding the modified amine waterborne epoxy curing agent and the prepared accelerator, and uniformly stirring to form a dispersed phase; and (2) taking a sodium dodecyl sulfate aqueous solution as a continuous phase, dropwise adding the dispersed phase into the continuous phase, stirring at a high speed, reacting under certain conditions after dropwise adding, stirring at a low speed, and performing suction filtration, washing and drying after the reaction to obtain the microcapsule modifier.
13. The method of claim 12, wherein: in the step i), the temperature for heating and dissolving is 40-90 ℃; the reaction conditions are as follows: reacting for 1.0 to 4.0 hours at the temperature of 50 to 120 ℃, and dehydrating by heating to 150 to 200 ℃ and vacuumizing.
14. The method of claim 12, wherein: in the step ii), the mass concentration of the sodium dodecyl benzene sulfonate aqueous solution is 1.0-1.5%.
15. The method of claim 12, wherein: in the step ii), the rotating speed of the high-speed stirring is 1000 to 3000r/min, and the rotating speed of the low-speed stirring is 500 to 800r/min.
16. The method of claim 12, wherein: in step ii), the reaction conditions are as follows: and reacting at 35 to 45 ℃ for 3 to 8 hours.
17. The method of claim 12, wherein: in the step ii), washing is firstly carried out by using ethanol and then washing is carried out by using deionized water; the drying conditions are drying at 50 to 80 ℃ for 10 to 20 hours.
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Effective date of registration: 20231109 Address after: 100728 No. 22 North Main Street, Chaoyang District, Beijing, Chaoyangmen Patentee after: CHINA PETROLEUM & CHEMICAL Corp. Patentee after: Sinopec (Dalian) Petrochemical Research Institute Co.,Ltd. Address before: 100728 No. 22 North Main Street, Chaoyang District, Beijing, Chaoyangmen Patentee before: CHINA PETROLEUM & CHEMICAL Corp. Patentee before: DALIAN RESEARCH INSTITUTE OF PETROLEUM AND PETROCHEMICALS, SINOPEC Corp. |