CN116445138A - Plugging agent and preparation method and application thereof - Google Patents
Plugging agent and preparation method and application thereof Download PDFInfo
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- CN116445138A CN116445138A CN202310428174.7A CN202310428174A CN116445138A CN 116445138 A CN116445138 A CN 116445138A CN 202310428174 A CN202310428174 A CN 202310428174A CN 116445138 A CN116445138 A CN 116445138A
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- China
- Prior art keywords
- lipophilic
- calcium carbonate
- molybdenum disulfide
- silicon dioxide
- plugging agent
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- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 165
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 131
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims abstract description 89
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims abstract description 89
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 86
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 65
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 63
- 238000005553 drilling Methods 0.000 claims abstract description 62
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 62
- 239000003921 oil Substances 0.000 claims abstract description 58
- 239000012530 fluid Substances 0.000 claims abstract description 56
- 230000002209 hydrophobic effect Effects 0.000 claims abstract description 54
- 239000002245 particle Substances 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims description 39
- 238000006243 chemical reaction Methods 0.000 claims description 37
- -1 fatty acid modified calcium carbonate Chemical class 0.000 claims description 35
- 150000003242 quaternary ammonium salts Chemical class 0.000 claims description 30
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 28
- 239000000194 fatty acid Substances 0.000 claims description 28
- 229930195729 fatty acid Natural products 0.000 claims description 28
- 238000002156 mixing Methods 0.000 claims description 24
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 22
- 239000004094 surface-active agent Substances 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 125000000217 alkyl group Chemical group 0.000 claims description 16
- 239000003960 organic solvent Substances 0.000 claims description 16
- 230000008569 process Effects 0.000 claims description 16
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims description 6
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 6
- 150000004665 fatty acids Chemical class 0.000 claims description 5
- 125000003545 alkoxy group Chemical group 0.000 claims description 4
- 125000002572 propoxy group Chemical group [*]OC([H])([H])C(C([H])([H])[H])([H])[H] 0.000 claims description 4
- 125000002889 tridecyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 4
- 239000005909 Kieselgur Substances 0.000 claims description 2
- 239000003093 cationic surfactant Substances 0.000 claims description 2
- 125000001421 myristyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 2
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 2
- 125000002958 pentadecyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 2
- 125000002948 undecyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 2
- 239000000654 additive Substances 0.000 claims 7
- 230000000996 additive effect Effects 0.000 claims 7
- 230000000694 effects Effects 0.000 abstract description 14
- 239000004033 plastic Substances 0.000 abstract description 3
- 239000011148 porous material Substances 0.000 abstract description 3
- 230000002265 prevention Effects 0.000 abstract description 3
- 239000003348 petrochemical agent Substances 0.000 abstract description 2
- 230000009467 reduction Effects 0.000 abstract description 2
- 230000002195 synergetic effect Effects 0.000 abstract description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 101
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 69
- 239000007787 solid Substances 0.000 description 44
- 235000019441 ethanol Nutrition 0.000 description 28
- 230000000052 comparative effect Effects 0.000 description 24
- 238000003756 stirring Methods 0.000 description 24
- SCPWMSBAGXEGPW-UHFFFAOYSA-N dodecyl(trimethoxy)silane Chemical group CCCCCCCCCCCC[Si](OC)(OC)OC SCPWMSBAGXEGPW-UHFFFAOYSA-N 0.000 description 23
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical group [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 21
- 238000001914 filtration Methods 0.000 description 20
- 238000005119 centrifugation Methods 0.000 description 19
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 18
- 239000000203 mixture Substances 0.000 description 18
- 239000003995 emulsifying agent Substances 0.000 description 16
- 238000001291 vacuum drying Methods 0.000 description 15
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 11
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 11
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 11
- 239000005642 Oleic acid Substances 0.000 description 11
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 11
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 11
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 10
- 238000012360 testing method Methods 0.000 description 10
- 238000004821 distillation Methods 0.000 description 9
- 239000003638 chemical reducing agent Substances 0.000 description 6
- 239000000706 filtrate Substances 0.000 description 6
- 239000004576 sand Substances 0.000 description 6
- 239000000377 silicon dioxide Substances 0.000 description 6
- 239000000080 wetting agent Substances 0.000 description 6
- 230000008901 benefit Effects 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
- 239000002283 diesel fuel Substances 0.000 description 5
- 239000006185 dispersion Substances 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 239000002002 slurry Substances 0.000 description 5
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 4
- 230000001050 lubricating effect Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000002689 soil Substances 0.000 description 4
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 238000005098 hot rolling Methods 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical group [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 2
- IGFHQQFPSIBGKE-UHFFFAOYSA-N Nonylphenol Natural products CCCCCCCCCC1=CC=C(O)C=C1 IGFHQQFPSIBGKE-UHFFFAOYSA-N 0.000 description 2
- 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
- 239000001110 calcium chloride Substances 0.000 description 2
- 229910001628 calcium chloride Inorganic materials 0.000 description 2
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical group [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 2
- 239000000292 calcium oxide Substances 0.000 description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 229940051841 polyoxyethylene ether Drugs 0.000 description 2
- 229920000056 polyoxyethylene ether Polymers 0.000 description 2
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- WQPMYSHJKXVTME-UHFFFAOYSA-N 3-hydroxypropane-1-sulfonic acid Chemical compound OCCCS(O)(=O)=O WQPMYSHJKXVTME-UHFFFAOYSA-N 0.000 description 1
- GNSFRPWPOGYVLO-UHFFFAOYSA-N 3-hydroxypropyl 2-methylprop-2-enoate Chemical group CC(=C)C(=O)OCCCO GNSFRPWPOGYVLO-UHFFFAOYSA-N 0.000 description 1
- QGTHRCDTVFFPBQ-UHFFFAOYSA-N C(C(=C)C)(=O)OCCCO.[Na] Chemical group C(C(=C)C)(=O)OCCCO.[Na] QGTHRCDTVFFPBQ-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical group C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 241000276425 Xiphophorus maculatus Species 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 125000005336 allyloxy group Chemical group 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000003079 shale oil Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 230000000007 visual effect 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
- C09K8/02—Well-drilling compositions
- C09K8/03—Specific additives for general use in well-drilling compositions
-
- 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
- C09K8/032—Inorganic additives
-
- 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
- C09K8/32—Non-aqueous well-drilling compositions, e.g. oil-based
-
- 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
- C09K8/42—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
- C09K8/46—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement
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- 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)
- Inorganic Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention relates to a plugging agent, a preparation method and application thereof, and belongs to the technical field of petrochemicals. The plugging agent disclosed by the invention mainly comprises diatomite, hydrophobic nano silicon dioxide, lipophilic flaky molybdenum disulfide and lipophilic calcium carbonate, and has better dispersibility and stability and better plugging effect and antifriction and antiwear properties when being used for oil-based drilling fluid. Diatomite, hydrophobic nano silicon dioxide, lipophilic flaky molybdenum disulfide and lipophilic calcium carbonate can produce a synergistic effect, so that the particle size of the drilling fluid is graded reasonably, particles with different gradations can effectively perform leakage prevention and plugging on all pores, the rheological property of the drilling fluid system can be obviously improved, the dynamic-plastic ratio is improved, the effect of the plugging agent on the leakage reduction rate is greatly improved, and the fluid loss is effectively reduced.
Description
Technical Field
The invention relates to a plugging agent, a preparation method and application thereof, and belongs to the technical field of petrochemicals.
Background
With the increasing global oil demand, oil drilling is gradually shifted from shallow to deep. For oil exploitation of deep wells or ultra-deep wells, oil-based drilling fluids present an increasingly prominent advantage due to increased drilling difficulty, particularly in the drilling construction of shale oil and gas wells. Compared with water-based drilling fluid, the oil-based drilling fluid has the advantages of strong pollution resistance, good lubricating performance, good thermal stability and the like, and can maintain the stability of the well wall and stratum. Compared with the traditional plugging material, the nano particles have obvious advantages in high-density drilling fluid. The application of the nano technology in the drilling fluid is one of research hotspots in the field of oilfield chemistry at present, and is widely focused on the drilling fluid industry at home and abroad. The inorganic nano material can improve the problems of poor temperature resistance, single molecular structure and function and the like commonly existing in the conventional materials in the oil gas drilling development field, and particularly, the multi-scale compound nano composite material is formed, so that the particle size of the drilling fluid is graded reasonably, the plugging and collapse prevention performance of a drilling fluid system can be obviously improved, the rheological property of the drilling fluid system is improved, the dynamic-plastic ratio is improved, and the high-temperature high-pressure fluid loss is reduced.
CaCO with different particle sizes 3 The inorganic plugging agent is a common inorganic plugging agent, has wide sources and larger sizes, is suitable for plugging the leakage channels of large holes with different shapes, and can improve the strength of the plugging agent and the plugging success rate by adding the plugging agent into different plugging agent formulas. But CaCO 3 The dispersion performance of the particles in the oil-based mud is poor, so that the plugging performance is limited. In addition, the existing plugging agent for the oil-based drilling fluid containing the inorganic nano material has the problems of poor stability and poor plugging effect.
Disclosure of Invention
The invention aims to provide a plugging agent, which can solve the problems of poor stability and poor plugging effect of the existing plugging agent for oil-based drilling fluid containing inorganic nano materials.
The second purpose of the invention is to provide a preparation method of the plugging agent.
The third object of the invention is to provide an application of the plugging agent in oil-based drilling fluid.
In order to achieve the above purpose, the plugging agent of the invention adopts the following technical scheme:
the plugging agent mainly comprises the following components in parts by mass: 18-30 parts of diatomite, 3-9 parts of hydrophobic nano silicon dioxide, 3-9 parts of lipophilic flaky molybdenum disulfide and 6-18 parts of lipophilic calcium carbonate; the lipophilic flaky molybdenum disulfide is flaky molybdenum disulfide modified by quaternary ammonium salt surfactant; the lipophilic calcium carbonate is fatty acid modified calcium carbonate.
The plugging agent disclosed by the invention mainly comprises diatomite, hydrophobic nano silicon dioxide, lipophilic flaky molybdenum disulfide and lipophilic calcium carbonate, and has better dispersibility and stability and better plugging effect and antifriction and antiwear properties when being used for oil-based drilling fluid. The diatomite has certain viscosity and can improve the rheological property of a drilling system; diatomite, hydrophobic nano silicon dioxide, lipophilic flaky molybdenum disulfide and lipophilic calcium carbonate can produce synergistic effect, so that the particle size of the drilling fluid is ensuredThe method has reasonable grading, particles with different grading can effectively perform leakage prevention and plugging on all pores, can obviously improve the rheological property of a drilling fluid system, improves the dynamic-plastic ratio, greatly improves the effect of the plugging agent on the leakage reduction rate, and effectively reduces the fluid loss. Hydrophobic nano SiO 2 The bentonite-containing high-heat-stability plugging slurry has the characteristics of no toxicity, no pollution, high heat stability and the like, is matched with bentonite components commonly used in the plugging slurry, and can be used for improving the viscosity of the drilling fluid, thereby effectively reducing the filtration loss of the drilling fluid. In addition, hydrophobic nano SiO 2 The method has the advantages of low cost, easy availability, good environment adaptability with an oil layer and the like, can block nanoscale pores, reduce the permeability of rock stratum, reduce the instability of a shale stratum shaft, reduce the fluid loss, reduce friction and the like. Oleophilic MoS 2 Has a special two-dimensional hierarchical structure, good temperature resistance and oleophilic MoS 2 The introduction of the drilling fluid can effectively reduce the friction resistance of the drilling fluid, improve the lubricity of the drilling fluid, reduce the abrasion of a drill bit and a drilling tool and prolong the service life. At the same time, moS in a sheet-like form 2 Can also more effectively block gaps and cracks of the bottom layer, and can be matched with granular nano SiO 2 And CaCO (CaCO) 3 The combination of the plugging materials can effectively cope with leakage points with various shapes in the stratum, and effectively reduce the fluid loss of drilling fluid.
The plugging agent disclosed by the invention is uniformly dispersed in the oil-based drilling fluid, has stable performance, better high-temperature stability, no aggregation in the oil-based drilling fluid at high temperature, wide particle size distribution range of solid particles in the plugging agent, and is favorable for improving and plugging cracks with different widths, and can improve the rheological property and lubricating property of the drilling fluid, and the plugging agent is nontoxic, pollution-free and environment-friendly.
Preferably, the diatomaceous earth has a mass fraction of 300 mesh screen residue of not more than 2%. The oversized diatomite particles can cause poor plugging effect.
Preferably, the particle size of the hydrophobic nano-silica is 100-500 nm. Too large particle size of the hydrophobic nano silicon dioxide can cause poor plugging effect, too small particle size can cause too large viscosity of plugging slurry.
Preferably, the particle size of the lipophilic flaky molybdenum disulfide is 100-1200 nm. Too large particle size of the lipophilic flaky molybdenum disulfide can cause poor plugging effect, and too small particle size can cause too large viscosity of plugging slurry.
Preferably, the particle size of the lipophilic calcium carbonate is 100-1200 nm. Too large particle size of the lipophilic calcium carbonate can cause poor plugging effect, and too small particle size can cause too large viscosity of plugging slurry.
Preferably, the hydrophobic nanosilica is a silane coupling agent modified nanosilica.
Preferably, the silane coupling agent is an alkyl trialkoxysilane. Preferably, the alkyl group in the alkyl trialkoxysilane is a dodecyl, undecyl, dodecyl or tridecyl group. Preferably, the alkoxy in the alkyl trialkoxysilane is selected from one or any combination of methoxy, ethoxy and propoxy. For example, the silane coupling agent is dodecyl trimethoxy silane.
Preferably, the hydrophobic nanosilica is prepared by a process comprising the steps of: mixing nano silicon dioxide and a silane coupling agent in an organic solvent for reaction, carrying out solid-liquid separation, and drying to obtain the hydrophobic nano silicon dioxide. The reaction process of the nano silica and the silane coupling agent dodecyl trimethoxy silane (DTMS) is shown in figure 1.
Preferably, the volume of silane coupling agent used per 3-9 g of nano-silica is 6-10 mL.
Preferably, the temperature of the mixing reaction performed in preparing the hydrophobic nano-silica is 50-70 ℃ and the time is 2-5 h.
Preferably, the organic solvent used in preparing the hydrophobic nanosilica consists of ethanol and N, N-dimethylformamide. Preferably, the volume ratio of the ethanol to the N, N-dimethylformamide is (90-120): (25-50). Preferably, when preparing the hydrophobic nano-silica, the volume of the organic solvent adopted for each 3-9 g of nano-silica is x-ymL, and the volume of the ethanol used for preparing the organic solvent of x-ymL is 90-120 mL.
Preferably, the quaternary ammonium salt surfactant is a quaternary ammonium salt cationic surfactant. Preferably, the quaternary ammonium salt surfactant is an alkyl alkoxy quaternary ammonium salt. Preferably, the alkyl alkoxy quaternary ammonium salt is an alkyl trialkoxy quaternary ammonium salt. Preferably, the alkyl in the alkyl trialkoxy quaternary ammonium salt is dodecyl, tridecyl, tetradecyl, pentadecyl or hexadecyl. Preferably, the alkoxy in the alkyl trialkoxy quaternary ammonium salt is selected from one or any combination of methoxy, ethoxy and propoxy. For example, the quaternary ammonium salt surfactant is cetyltrimethylammonium bromide.
Preferably, the lipophilic platelet molybdenum disulfide is prepared by a process comprising the steps of: and (3) mixing the flaky molybdenum disulfide and the quaternary ammonium salt surfactant in water for reaction, carrying out solid-liquid separation, and drying to obtain the lipophilic flaky molybdenum disulfide. The reaction process of flaky molybdenum disulfide and cetyltrimethylammonium bromide (CTAB) is shown in fig. 2.
Preferably, the mass ratio of the flaky molybdenum disulfide to the quaternary ammonium salt surfactant used in the preparation of the lipophilic flaky molybdenum disulfide is (3-9) to (0.15-0.45).
Preferably, the temperature of the mixing reaction carried out in the preparation of the lipophilic flaky molybdenum disulfide is 60-80 ℃ and the time is 2-4 hours.
Preferably, the fatty acid modified calcium carbonate is C 15 ～C 18 Fatty acid modified calcium carbonate. For example, the fatty acid modified calcium carbonate is oleic acid modified calcium carbonate.
Preferably, the fatty acid modified calcium carbonate is prepared by a process comprising the steps of: mixing calcium carbonate and fatty acid in an organic solvent for reaction, carrying out solid-liquid separation, and drying to obtain the fatty acid modified calcium carbonate. The reaction process of calcium carbonate and oleic acid is shown in figure 3.
Preferably, the mass ratio of the calcium carbonate to the fatty acid used in the preparation of the fatty acid-modified calcium carbonate is (6-18): 5.4-9.
Preferably, the temperature of the mixing reaction performed in the preparation of the fatty acid modified calcium carbonate is 50-70 ℃ for 2-4 hours.
When the plugging agent is used for oil-based drilling fluid, the quaternary ammonium salt surfactant on the surface of the lipophilic flaky molybdenum disulfide has a bonding effect on silane coupling agent groups on the surface of hydrophobic nano silicon dioxide, a large amount of hydrophobic nano silicon dioxide can be adhered to the lipophilic flaky molybdenum disulfide to form a composite material, as shown in figure 4, and then the composite material can be further compounded with lipophilic calcium carbonate with larger particle size, as shown in figure 5, as the lipophilic calcium carbonate and the lipophilic flaky molybdenum disulfide both have certain particle size distribution, the multiphase-level compound plugging agent can be formed, and meanwhile, the plugging effect and the antifriction and antiwear effects are exerted.
The preparation method of the plugging agent adopts the following technical scheme:
the preparation method of the plugging agent comprises the following steps: and uniformly mixing the components in the formula amount to obtain the plugging agent.
The preparation method of the plugging agent disclosed by the invention is simple to operate, the prepared plugging agent is uniformly dispersed in the oil-based drilling fluid, has stable performance, has better high-temperature stability, does not aggregate in the oil-based drilling fluid at a high temperature, has a wide particle size distribution range of solid particles in the plugging agent, is favorable for improving and plugging cracks with different widths, can improve the rheological property and the lubricating property of the drilling fluid, and is nontoxic, pollution-free and environment-friendly.
The application of the plugging agent in the oil-based drilling fluid adopts the following technical scheme:
the use of a plugging agent as described above in an oil-based drilling fluid.
The plugging agent disclosed by the invention is used in oil-based drilling fluid, has the advantages of uniform dispersion and stable performance, and the prepared oil-based drilling fluid can plug cracks with different widths and has good rheological property and lubricating property.
Preferably, the oil-based drilling fluid mainly comprises plugging agent and oil-based mud, and the oil-based mud mainly comprises oil, an emulsifying agent, a wetting agent, barite powder, organic soil, an alkaline regulator and a filtrate reducer.
Preferably, the emulsifier comprises a primary emulsifier and a secondary emulsifier. Preferably, the mass ratio of the main emulsifier to the auxiliary emulsifier is 2 (2.1-3). For example, the mass ratio of the primary emulsifier to the secondary emulsifier is 2:2.4.
Preferably, in the oil-based mud, the mass fraction of the emulsifier is 4-5%; the mass fraction of the wetting agent is 2-3%; the barite powder 3-6% of the weight percentage; the mass fraction of the organic soil is 2-5%; the mass fraction of the alkaline regulator is 2.5-4.5%; the mass fraction of the filtrate reducer is 2-4%.
For example, in the oil-based mud, the mass fraction of the emulsifier is 4.4%; the mass fraction of the wetting agent is 2%; the weight percentage of the barite powder is 3-6%; the mass fraction of the organic soil is 2.5%; the mass fraction of the alkaline regulator is 3%; the mass fraction of the filtrate reducer is 3%.
Preferably, the primary emulsifier is a hydroxypropyl methacrylate sulfonate; the auxiliary emulsifier is allyloxy nonylphenol polyoxyethylene ether; the wetting agent is allyloxy hydroxypropyl sulfonate; the alkaline regulator is calcium oxide; the filtrate reducer is calcium chloride.
Drawings
FIG. 1 is a schematic diagram showing the reaction process of nanosilica and Dodecyl Trimethoxysilane (DTMS) as a silane coupling agent in the present invention;
FIG. 2 is a schematic illustration of the reaction process of flaky molybdenum disulfide and cetyltrimethylammonium bromide (CTAB) in accordance with the present invention;
FIG. 3 is a schematic illustration of the reaction process of calcium carbonate and oleic acid in the present invention;
FIG. 4 is a schematic diagram of a process for forming a composite material from lipophilic platy molybdenum disulfide and hydrophobic nanosilicon dioxide in the present invention;
FIG. 5 is a schematic diagram of a process for forming a compound plugging agent by lipophilic flaky molybdenum disulfide, hydrophobic nano silicon dioxide and lipophilic calcium carbonate in the invention;
FIG. 6 is a schematic diagram showing the dispersion of the plugging agent of example 1 in 0# diesel in experimental example 1;
FIG. 7 is a graph showing the results of the test of the fluid loss properties of the oil-based mud in Experimental example 2;
fig. 8 is a schematic diagram showing the results of testing the fluid loss properties of the oil-based drilling fluid prepared with the plugging agent of example 3 in experimental example 2.
Detailed Description
The technical scheme of the invention is further described below with reference to specific embodiments.
1. Specific examples of the plugging agent of the invention are as follows:
example 1
The plugging agent of the embodiment comprises the following components in parts by mass: 18 parts of diatomite, 3 parts of hydrophobic nano silicon dioxide, 3 parts of lipophilic flaky molybdenum disulfide and 6 parts of lipophilic calcium carbonate; the lipophilic flaky molybdenum disulfide is flaky molybdenum disulfide modified by quaternary ammonium salt surfactant; the lipophilic calcium carbonate is fatty acid modified calcium carbonate; the mass fraction of 300 mesh screen residue of diatomite in the embodiment is less than or equal to 2%;
the hydrophobic nano silicon dioxide in the embodiment is silane coupling agent modified nano silicon dioxide, and is prepared by a method comprising the following steps: 3g of nano silicon dioxide and 6mL of dodecyl trimethoxy silane (DTMS) are put into an organic solvent (composed of 90mL of absolute ethyl alcohol and 25mL of N, N-dimethylformamide), the mixture is stirred uniformly, the mixture is mixed and reacted for 3 hours at 50 ℃, after the reaction is finished, part of the ethanol and N, N-Dimethylformamide (DMF) are removed by reduced pressure distillation, then filtration is carried out, the solid obtained by filtration is washed by acetone, and then the washed solid is dried in vacuum at 60 ℃ to obtain hydrophobic nano silicon dioxide (granularity is 100-500 nm);
the lipophilic flaky molybdenum disulfide in the embodiment is prepared by a method comprising the following steps: dispersing 3g of flaky molybdenum disulfide into 50mL of water, adding 0.15g of Cetyl Trimethyl Ammonium Bromide (CTAB), magnetically stirring at 60 ℃ for reaction for 4 hours, adding a proper amount of water into a reacted system, centrifuging, mixing the solid obtained by centrifugation with a proper amount of ethanol, centrifuging again, and vacuum drying the solid obtained by centrifugation at 60 ℃ to obtain lipophilic flaky molybdenum disulfide (granularity is 100-1200 nm);
the lipophilic calcium carbonate in this example is prepared by a process comprising the steps of: adding 6g of calcium carbonate and 6mL of oleic acid into 100mL of absolute ethyl alcohol, uniformly stirring, heating to 50 ℃, reacting for 3 hours under the stirring condition, adding a proper amount of ethanol into a reacted system, centrifuging, and vacuum drying the solid obtained by centrifuging at 60 ℃ to obtain the lipophilic calcium carbonate (with the granularity of 100-1200 nm).
Example 2
The plugging agent of the embodiment comprises the following components in parts by mass: 18 parts of diatomite, 6 parts of hydrophobic nano silicon dioxide, 6 parts of lipophilic flaky molybdenum disulfide and 12 parts of lipophilic calcium carbonate; the lipophilic flaky molybdenum disulfide is flaky molybdenum disulfide modified by quaternary ammonium salt surfactant; the lipophilic calcium carbonate is fatty acid modified calcium carbonate; the mass fraction of 300 mesh screen residue of diatomite in the embodiment is less than or equal to 2%;
the hydrophobic nano silicon dioxide in the embodiment is silane coupling agent modified nano silicon dioxide, and is prepared by a method comprising the following steps: adding 6g of nano silicon dioxide and 8mL of dodecyl trimethoxy silane (DTMS) into an organic solvent (composed of 100mL of absolute ethyl alcohol and 40mL of N, N-dimethylformamide), uniformly stirring, mixing and reacting for 4 hours at 50 ℃, removing part of ethanol and N, N-Dimethylformamide (DMF) by reduced pressure distillation after the reaction is finished, filtering, washing the solid obtained by filtering by acetone, and vacuum drying the washed solid at 60 ℃ to obtain hydrophobic nano silicon dioxide (granularity is 100-500 nm);
the lipophilic flaky molybdenum disulfide in the embodiment is prepared by a method comprising the following steps: dispersing 6g of flaky molybdenum disulfide into 60mL of water, adding 0.3g of Cetyl Trimethyl Ammonium Bromide (CTAB), magnetically stirring at 60 ℃ for reaction for 3 hours, adding a proper amount of water into a reacted system, centrifuging, mixing the solid obtained by centrifugation with a proper amount of ethanol, centrifuging again, and vacuum drying the solid obtained by centrifugation at 60 ℃ to obtain lipophilic flaky molybdenum disulfide (granularity is 100-1200 nm);
the lipophilic calcium carbonate in this example is prepared by a process comprising the steps of: adding 12g of calcium carbonate and 8mL of oleic acid into 110mL of absolute ethyl alcohol, uniformly stirring, heating to 50 ℃, reacting for 4 hours under the stirring condition, adding a proper amount of ethanol into a reacted system, centrifuging, and vacuum drying the solid obtained by centrifuging at 60 ℃ to obtain the lipophilic calcium carbonate (the granularity is 100-1200 nm).
Example 3
The plugging agent of the embodiment comprises the following components in parts by mass: 18 parts of diatomite, 9 parts of hydrophobic nano silicon dioxide, 9 parts of lipophilic flaky molybdenum disulfide and 18 parts of lipophilic calcium carbonate; the lipophilic flaky molybdenum disulfide is flaky molybdenum disulfide modified by quaternary ammonium salt surfactant; the lipophilic calcium carbonate is fatty acid modified calcium carbonate; the mass fraction of 300 mesh screen residue of diatomite in the embodiment is less than or equal to 2%;
the hydrophobic nano silicon dioxide in the embodiment is silane coupling agent modified nano silicon dioxide, and is prepared by a method comprising the following steps: 9g of nano silicon dioxide and 10mL of dodecyl trimethoxy silane (DTMS) are put into an organic solvent (composed of 120mL of absolute ethyl alcohol and 50mL of N, N-dimethylformamide), the mixture is stirred uniformly, the mixture is mixed and reacted for 3 hours at 50 ℃, after the reaction is finished, part of the ethanol and N, N-Dimethylformamide (DMF) are removed by reduced pressure distillation, then filtration is carried out, the solid obtained by filtration is washed by acetone, and then the washed solid is dried in vacuum at 60 ℃ to obtain hydrophobic nano silicon dioxide (granularity is 100-500 nm);
the lipophilic flaky molybdenum disulfide in the embodiment is prepared by a method comprising the following steps: dispersing 9g of flaky molybdenum disulfide into 80mL of water, adding 0.45g of Cetyl Trimethyl Ammonium Bromide (CTAB), magnetically stirring at 60 ℃ for reaction for 2 hours, adding a proper amount of water into the reacted system, centrifuging, mixing the solid obtained by centrifugation with a proper amount of ethanol, centrifuging again, and vacuum drying the solid obtained by centrifugation at 60 ℃ to obtain lipophilic flaky molybdenum disulfide (granularity is 100-1200 nm);
the lipophilic calcium carbonate in this example is prepared by a process comprising the steps of: 18g of calcium carbonate and 10mL of oleic acid are added into 120mL of absolute ethyl alcohol, the mixture is stirred uniformly, then the temperature is raised to 50 ℃, the reaction is carried out for 4 hours under the stirring condition, then a proper amount of ethanol is added into the reacted system, the mixture is centrifuged, and then the solid obtained by centrifugation is dried in vacuum at 60 ℃ to obtain the lipophilic calcium carbonate (the granularity is 100-1200 nm).
Example 4
The plugging agent of the embodiment comprises the following components in parts by mass: 24 parts of diatomite, 9 parts of hydrophobic nano silicon dioxide, 6 parts of lipophilic flaky molybdenum disulfide and 6 parts of lipophilic calcium carbonate; the lipophilic flaky molybdenum disulfide is flaky molybdenum disulfide modified by quaternary ammonium salt surfactant; the lipophilic calcium carbonate is fatty acid modified calcium carbonate; the mass fraction of 300 mesh screen residue of diatomite in the embodiment is less than or equal to 2%;
the hydrophobic nano silicon dioxide in the embodiment is silane coupling agent modified nano silicon dioxide, and is prepared by a method comprising the following steps: 9g of nano silicon dioxide and 10mL of dodecyl trimethoxy silane (DTMS) are put into an organic solvent (composed of 120mL of absolute ethyl alcohol and 50mL of N, N-dimethylformamide), the mixture is stirred uniformly, the reaction is carried out for 2 hours at 60 ℃, after the reaction is finished, part of the ethanol and N, N-Dimethylformamide (DMF) are removed by reduced pressure distillation, then filtration is carried out, the solid obtained by filtration is washed by acetone, and then the washed solid is dried in vacuum at 60 ℃ to obtain hydrophobic nano silicon dioxide (100-500 nm);
the lipophilic flaky molybdenum disulfide in the embodiment is prepared by a method comprising the following steps: dispersing 6g of flaky molybdenum disulfide into 60mL of water, adding 0.3g of Cetyl Trimethyl Ammonium Bromide (CTAB), magnetically stirring at 70 ℃ for reaction for 3 hours, adding a proper amount of water into a reacted system, centrifuging, mixing the solid obtained by centrifugation with a proper amount of ethanol, centrifuging again, and vacuum drying the solid obtained by centrifugation at 60 ℃ to obtain lipophilic flaky molybdenum disulfide (granularity is 100-1200 nm);
the lipophilic calcium carbonate in this example is prepared by a process comprising the steps of: adding 6g of calcium carbonate and 6mL of oleic acid into 100mL of absolute ethyl alcohol, uniformly stirring, heating to 60 ℃, reacting for 3 hours under the stirring condition, adding a proper amount of ethanol into a reacted system, centrifuging, and vacuum drying the solid obtained by centrifuging at 60 ℃ to obtain the lipophilic calcium carbonate (the granularity is 100-1200 nm).
Example 5
The plugging agent of the embodiment comprises the following components in parts by mass: 24 parts of diatomite, 3 parts of hydrophobic nano silicon dioxide, 9 parts of lipophilic flaky molybdenum disulfide and 12 parts of lipophilic calcium carbonate; the lipophilic flaky molybdenum disulfide is flaky molybdenum disulfide modified by quaternary ammonium salt surfactant; the lipophilic calcium carbonate is fatty acid modified calcium carbonate; the mass fraction of 300 mesh screen residue of diatomite in the embodiment is less than or equal to 2%;
the hydrophobic nano silicon dioxide in the embodiment is silane coupling agent modified nano silicon dioxide, and is prepared by a method comprising the following steps: 3g of nano silicon dioxide and 6mL of dodecyl trimethoxy silane (DTMS) are put into an organic solvent (composed of 90mL of absolute ethyl alcohol and 25mL of N, N-dimethylformamide), the mixture is stirred uniformly, the mixture is mixed and reacted for 3 hours at 60 ℃, after the reaction is finished, part of the ethanol and N, N-Dimethylformamide (DMF) are removed by reduced pressure distillation, then filtration is carried out, the solid obtained by filtration is washed by acetone, and then the washed solid is dried in vacuum at 60 ℃ to obtain hydrophobic nano silicon dioxide (granularity is 100-500 nm);
the lipophilic flaky molybdenum disulfide in the embodiment is prepared by a method comprising the following steps: dispersing 9g of flaky molybdenum disulfide into 80mL of water, adding 0.45g of Cetyl Trimethyl Ammonium Bromide (CTAB), magnetically stirring at 70 ℃ for reaction for 3 hours, adding a proper amount of water into the reacted system, centrifuging, mixing the solid obtained by centrifugation with a proper amount of ethanol, centrifuging again, and vacuum drying the solid obtained by centrifugation at 60 ℃ to obtain lipophilic flaky molybdenum disulfide (granularity is 100-1200 nm);
the lipophilic calcium carbonate in this example is prepared by a process comprising the steps of: adding 12g of calcium carbonate and 8mL of oleic acid into 110mL of absolute ethyl alcohol, uniformly stirring, heating to 60 ℃, reacting for 3 hours under the stirring condition, adding a proper amount of ethanol into the reacted system, centrifuging, and vacuum drying the solid obtained by centrifuging at 60 ℃ to obtain the lipophilic calcium carbonate (the granularity is 100-1200 nm).
Example 6
The plugging agent of the embodiment comprises the following components in parts by mass: 18 parts of diatomite, 3 parts of hydrophobic nano silicon dioxide, 3 parts of lipophilic flaky molybdenum disulfide and 6 parts of lipophilic calcium carbonate; the lipophilic flaky molybdenum disulfide is flaky molybdenum disulfide modified by quaternary ammonium salt surfactant; the lipophilic calcium carbonate is fatty acid modified calcium carbonate; the mass fraction of 300 mesh screen residue of diatomite in the embodiment is less than or equal to 2%;
the hydrophobic nano silicon dioxide in the embodiment is silane coupling agent modified nano silicon dioxide, and is prepared by a method comprising the following steps: 3g of nano silicon dioxide and 6mL of dodecyl trimethoxy silane (DTMS) are put into an organic solvent (composed of 90mL of absolute ethyl alcohol and 25mL of N, N-dimethylformamide), the mixture is stirred uniformly, the mixture is mixed and reacted for 5 hours at 50 ℃, after the reaction is finished, part of the ethanol and N, N-Dimethylformamide (DMF) are removed by reduced pressure distillation, then filtration is carried out, the solid obtained by filtration is washed by acetone, and then the washed solid is dried in vacuum at 60 ℃ to obtain hydrophobic nano silicon dioxide (granularity is 100-500 nm);
the lipophilic sheet molybdenum disulfide in this example is the same as the lipophilic sheet molybdenum disulfide in example 1;
the lipophilic calcium carbonate in this example was the same as that in example 1.
Example 7
The plugging agent of the embodiment comprises the following components in parts by mass: 30 parts of diatomite, 6 parts of hydrophobic nano silicon dioxide, 3 parts of lipophilic flaky molybdenum disulfide and 18 parts of lipophilic calcium carbonate; the lipophilic flaky molybdenum disulfide is flaky molybdenum disulfide modified by quaternary ammonium salt surfactant; the lipophilic calcium carbonate is fatty acid modified calcium carbonate; the mass fraction of 300 mesh screen residue of diatomite in the embodiment is less than or equal to 2%;
the hydrophobic nano silicon dioxide in the embodiment is silane coupling agent modified nano silicon dioxide, and is prepared by a method comprising the following steps: adding 6g of nano silicon dioxide and 8mL of dodecyl trimethoxy silane (DTMS) into an organic solvent (composed of 110mL of absolute ethyl alcohol and 40mL of N, N-dimethylformamide), uniformly stirring, mixing and reacting for 2 hours at 70 ℃, removing part of the ethanol and the N, N-Dimethylformamide (DMF) by reduced pressure distillation after the reaction is finished, filtering, washing the solid obtained by filtering by acetone, and vacuum drying the washed solid at 60 ℃ to obtain hydrophobic nano silicon dioxide (granularity is 100-500 nm);
the lipophilic flaky molybdenum disulfide in the embodiment is prepared by a method comprising the following steps: dispersing 3g of flaky molybdenum disulfide into 50mL of water, adding 0.15g of Cetyl Trimethyl Ammonium Bromide (CTAB), magnetically stirring at 80 ℃ for 2 hours, adding a proper amount of water into the reacted system, centrifuging, mixing the solid obtained by centrifugation with a proper amount of ethanol, centrifuging again, and vacuum drying the solid obtained by centrifugation at 60 ℃ to obtain lipophilic flaky molybdenum disulfide (granularity is 100-1200 nm);
the lipophilic calcium carbonate in this example is prepared by a process comprising the steps of: 18g of calcium carbonate and 10mL of oleic acid are added into 120mL of absolute ethyl alcohol, the mixture is stirred uniformly, then the temperature is raised to 70 ℃, the reaction is carried out for 2 hours under the stirring condition, then a proper amount of ethanol is added into the reacted system, the mixture is centrifuged, and then the solid obtained by centrifugation is dried in vacuum at 60 ℃ to obtain the lipophilic calcium carbonate (the granularity is 100-1200 nm).
Example 8
The plugging agent of the embodiment comprises the following components in parts by mass: 30 parts of diatomite, 9 parts of hydrophobic nano silicon dioxide, 3 parts of lipophilic flaky molybdenum disulfide and 12 parts of lipophilic calcium carbonate; the lipophilic flaky molybdenum disulfide is flaky molybdenum disulfide modified by quaternary ammonium salt surfactant; the lipophilic calcium carbonate is fatty acid modified calcium carbonate; the mass fraction of 300 mesh screen residue of diatomite in the embodiment is less than or equal to 2%;
the hydrophobic nano silicon dioxide in the embodiment is silane coupling agent modified nano silicon dioxide, and is prepared by a method comprising the following steps: 9g of nano silicon dioxide and 10mL of dodecyl trimethoxy silane (DTMS) are put into an organic solvent (composed of 120mL of absolute ethyl alcohol and 50mL of N, N-dimethylformamide), the mixture is stirred uniformly, the reaction is carried out for 2 hours at 70 ℃, after the reaction is finished, part of the ethanol and N, N-Dimethylformamide (DMF) are removed by reduced pressure distillation, then filtration is carried out, the solid obtained by filtration is washed by acetone, and then the washed solid is dried in vacuum at 60 ℃ to obtain hydrophobic nano silicon dioxide (granularity is 100-500 nm);
the lipophilic flaky molybdenum disulfide in the embodiment is prepared by a method comprising the following steps: dispersing 3g of flaky molybdenum disulfide into 50mL of water, adding 0.15g of Cetyl Trimethyl Ammonium Bromide (CTAB), magnetically stirring at 80 ℃ for 2 hours, adding a proper amount of water into the reacted system, centrifuging, mixing the solid obtained by centrifugation with a proper amount of ethanol, centrifuging again, and vacuum drying the solid obtained by centrifugation at 60 ℃ to obtain lipophilic flaky molybdenum disulfide (granularity is 100-1200 nm);
the lipophilic calcium carbonate in this example is prepared by a process comprising the steps of: adding 12g of calcium carbonate and 8mL of oleic acid into 110mL of absolute ethyl alcohol, uniformly stirring, heating to 70 ℃, reacting for 2 hours under the stirring condition, adding a proper amount of ethanol into a reacted system, centrifuging, and vacuum drying the solid obtained by centrifuging at 60 ℃ to obtain the lipophilic calcium carbonate (with the granularity of 100-1200 nm).
Example 9
The plugging agent of the embodiment comprises the following components in parts by mass: 30 parts of diatomite, 9 parts of hydrophobic nano silicon dioxide, 9 parts of lipophilic flaky molybdenum disulfide and 18 parts of lipophilic calcium carbonate; the lipophilic flaky molybdenum disulfide is flaky molybdenum disulfide modified by quaternary ammonium salt surfactant; the lipophilic calcium carbonate is fatty acid modified calcium carbonate; the mass fraction of 300 mesh screen residue of diatomite in the embodiment is less than or equal to 2%;
the hydrophobic nano silicon dioxide in the embodiment is silane coupling agent modified nano silicon dioxide, and is prepared by a method comprising the following steps: 9g of nano silicon dioxide and 6mL of dodecyl trimethoxy silane (DTMS) are put into an organic solvent (composed of 90mL of absolute ethyl alcohol and 25mL of N, N-dimethylformamide), the mixture is stirred uniformly, the mixture is mixed and reacted for 3 hours at 70 ℃, after the reaction is finished, part of the ethanol and N, N-Dimethylformamide (DMF) are removed by reduced pressure distillation, then filtration is carried out, the solid obtained by filtration is washed by acetone, and then the washed solid is dried in vacuum at 60 ℃ to obtain hydrophobic nano silicon dioxide (granularity is 100-500 nm);
the lipophilic flaky molybdenum disulfide in the embodiment is prepared by a method comprising the following steps: dispersing 9g of flaky molybdenum disulfide into 60mL of water, adding 0.3g of Cetyl Trimethyl Ammonium Bromide (CTAB), magnetically stirring at 80 ℃ for 2 hours, adding a proper amount of water into a reacted system, centrifuging, mixing the solid obtained by centrifugation with a proper amount of ethanol, centrifuging again, and vacuum drying the solid obtained by centrifugation at 60 ℃ to obtain lipophilic flaky molybdenum disulfide (granularity is 100-1200 nm);
the lipophilic calcium carbonate in this example is prepared by a process comprising the steps of: 18g of calcium carbonate and 8mL of oleic acid are added into 110mL of absolute ethyl alcohol, the mixture is stirred uniformly, then the temperature is raised to 70 ℃, the reaction is carried out for 2 hours under the stirring condition, then a proper amount of ethanol is added into the reacted system, the mixture is centrifuged, and then the solid obtained by centrifugation is dried in vacuum at 60 ℃ to obtain the lipophilic calcium carbonate (the granularity is 100-1200 nm).
Comparative example 1
The plugging agent of the present comparative example differs from the plugging agent of example 1 only in that the nanosilica used in the plugging agent of the present comparative example is nanosilica which is not modified by a silane coupling agent, and the flaky molybdenum disulfide is flaky molybdenum disulfide which is not modified by a quaternary ammonium salt surfactant, and the calcium carbonate is calcium carbonate which is not modified by a fatty acid.
Comparative example 2
The plugging agent of this comparative example differs from the plugging agent of example 1 only in that the mass fraction of the hydrophobic nanosilica used in the plugging agent of this comparative example is 2 parts.
Comparative example 3
The plugging agent of this comparative example differs from the plugging agent of example 3 only in that the mass fraction of the hydrophobic nanosilica used in the plugging agent of this comparative example is 10 parts.
Comparative example 4
The plugging agent of this comparative example differs from the plugging agent of example 1 only in that the mass fraction of the lipophilic flaky molybdenum disulfide used in the plugging agent of this comparative example is 2 parts.
Comparative example 5
The plugging agent of this comparative example differs from the plugging agent of example 3 only in that the lipophilic flaky molybdenum disulfide used in the plugging agent of this comparative example is 10 parts by mass.
2. Specific examples of the preparation method of the plugging agent of the invention are as follows:
the preparation method of the plugging agent specifically comprises the following steps: the components of the plugging agent in any one of examples 1-9 are added into a stirrer according to the proportion and are mixed uniformly, thus obtaining the plugging agent.
3. Specific examples of the application of the plugging agent of the present invention in oil-based drilling fluids are as follows:
the plugging agent of any of embodiments 1-9 may be used in an oil-based drilling fluid.
Experimental example 1
In order to evaluate the dispersibility of the plugging agents of examples 1 to 9, the plugging agents of examples 1 to 9 were stirred uniformly in 0# diesel oil and then allowed to stand for 1 hour, and the dispersion of the plugging agent in 0# diesel oil was observed, and the dispersion of the plugging agent of example 1 in 0# diesel oil was shown in fig. 6. The results show that the plugging agents of the examples 1-9 are uniformly dispersed after being stirred uniformly in the 0# diesel oil and kept stand for 1h, and no sedimentation and layering phenomenon occurs, so that the plugging agents of the examples 1-9 have better dispersibility.
Experimental example 2
In order to evaluate the application effect of the plugging agents of examples 1-9 and comparative examples 1-5 in oil-based drilling fluids, adding any one of the plugging agents of examples 1-9 and comparative examples 1-5 into oil-based mud, uniformly stirring to obtain an oil-based drilling fluid, and then testing the fluid loss performance of the oil-based drilling fluid; the mass ratio of the plugging agent to the oil-based mud is 3:100; the oil-based mud consists of the following components in parts by mass: 100 parts of diesel oil and barite powder (used for adjusting the density of oil-based drilling fluid to 1.4g/cm 3 ) 2 parts of main emulsifier, 2.4 parts of auxiliary emulsifier, 2 parts of wetting agent, 2.5 parts of organic soil, 3 parts of alkaline regulator and 3 parts of filtrate reducer, and is mainly used for preparing the water-soluble polymerThe emulsifier is sodium hydroxypropyl methacrylate sulfonate, the auxiliary emulsifier is allyloxy nonylphenol polyoxyethylene ether, the wetting agent is sodium allyloxy hydroxypropyl sulfonate, the alkaline regulator is calcium oxide, and the filtrate reducer is calcium chloride.
The method for testing the fluid loss performance of the oil-based drilling fluid comprises the following steps: adding sand with granularity of 20-100 meshes into a cylinder of a visual sand bed filtration instrument, compacting and paving to form a sand bed, slowly adding 500mL of oil-based drilling fluid into the cylinder, standing for 10min, and measuring the immersion depth (L 1 ) Then gradually pressurizing to 0.7MPa, and measuring the depth (L) of the oil-based drilling fluid immersed in the sand bed after 10min 2 )；
Then the oil-based drilling fluid is thermally rolled for 12 hours at 120 ℃, and the oil-based drilling fluid after being thermally rolled is tested and kept stand for 10 minutes by adopting the method, and then the depth (L) of the oil-based drilling fluid immersed in a sand bed 3 ) And the depth (L) of the oil-based drilling fluid immersed in the sand bed after being pressurized to 0.7MPa and maintained for 10min 4 )；
Meanwhile, testing the fluid loss performance of the oil-based mud according to the method and testing the fluid loss performance of the oil-based mud after a hot rolling experiment; the results of the tests of the fluid loss properties of the oil-based drilling fluids prepared by the plugging agents of the oil-based mud, the examples 1-9 and the comparative examples 1-5 are shown in table 1, and the results of the tests of the fluid loss properties of the oil-based drilling fluids prepared by the plugging agents of the oil-based mud, the examples 1-2, the example 6 and the comparative examples 1-5 after the hot rolling test are shown in table 2; the results of the oil-based mud fluid loss test are shown in fig. 7, and the results of the oil-based drilling fluid prepared with the plugging agent of example 3 are shown in fig. 8.
Table 1 fluid loss properties of oil-based drilling fluids
| Project | L 1 (cm) | L 2 (cm) |
| Oil-based mud | 0.7 | 1.4 |
| Example 1 | 0.1 | 0.5 |
| Example 2 | 0.1 | 0.3 |
| Example 3 | 0.2 | 0.5 |
| Example 4 | 0.2 | 0.6 |
| Example 5 | 0.1 | 0.6 |
| Example 6 | 0.2 | 0.5 |
| Example 7 | 0.2 | 0.6 |
| Example 8 | 0.2 | 0.6 |
| Example 9 | 0.2 | 0.7 |
| Comparative example 1 | 0.2 | 0.8 |
| Comparative example 2 | 0.2 | 0.9 |
| Comparative example 3 | 0.2 | 0.8 |
| Comparative example 4 | 0.2 | 0.7 |
| Comparative example 5 | 0.2 | 0.7 |
Table 2 fluid loss properties of oil-based drilling fluids after hot rolling experiments
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Claims (12)
1. The plugging agent is characterized by mainly comprising the following components in parts by mass: 18-30 parts of diatomite, 3-9 parts of hydrophobic nano silicon dioxide, 3-9 parts of lipophilic flaky molybdenum disulfide and 6-18 parts of lipophilic calcium carbonate; the lipophilic flaky molybdenum disulfide is flaky molybdenum disulfide modified by quaternary ammonium salt surfactant; the lipophilic calcium carbonate is fatty acid modified calcium carbonate.
2. The lost circulation additive of claim 1, wherein the diatomaceous earth has a mass fraction of 300 mesh residue of not greater than 2%.
3. The lost circulation additive of claim 1, wherein the hydrophobic nanosilica is a silane coupling agent modified nanosilica; the granularity of the hydrophobic nano silicon dioxide is 100-500 nm.
4. The lost circulation additive of claim 3, wherein the silane coupling agent is an alkyl trialkoxysilane; the alkyl in the alkyl trialkoxysilane is dodecyl, undecyl, dodecyl or tridecyl; the alkoxy in the alkyl trialkoxysilane is selected from one or any combination of methoxy, ethoxy and propoxy.
5. A lost circulation additive according to claim 3, wherein the hydrophobic nanosilica is prepared by a process comprising the steps of: mixing nano silicon dioxide and a silane coupling agent in an organic solvent for reaction, carrying out solid-liquid separation, and drying to obtain hydrophobic nano silicon dioxide; the volume of the silane coupling agent adopted per 3-9 g of nano silicon dioxide is 6-10 mL; the temperature of the mixing reaction carried out in the preparation of the hydrophobic nano silicon dioxide is 50-70 ℃ and the time is 2-5 h.
6. The plugging agent of claim 1, wherein the quaternary ammonium salt surfactant is a quaternary ammonium salt cationic surfactant; the particle size of the lipophilic flaky molybdenum disulfide is 100-1200 nm.
7. The plugging agent of claim 6, wherein the quaternary ammonium salt surfactant is an alkyl alkoxy quaternary ammonium salt; the alkyl alkoxy quaternary ammonium salt is alkyl trialkoxy quaternary ammonium salt; the alkyl in the alkyl trialkoxy quaternary ammonium salt is dodecyl, tridecyl, tetradecyl, pentadecyl or hexadecyl; the alkoxy in the alkyl trialkoxy quaternary ammonium salt is selected from one or any combination of methoxy, ethoxy and propoxy.
8. The lost circulation additive of claim 1, wherein the lipophilic platelet molybdenum disulfide is prepared by a process comprising the steps of: mixing flaky molybdenum disulfide and quaternary ammonium salt surfactant in water for reaction, carrying out solid-liquid separation, and drying to obtain lipophilic flaky molybdenum disulfide; the mass ratio of the flaky molybdenum disulfide to the quaternary ammonium salt surfactant used in the preparation of the lipophilic flaky molybdenum disulfide is (3-9) (0.15-0.45); the temperature of the mixing reaction carried out in the preparation of the lipophilic flaky molybdenum disulfide is 60-80 ℃ and the time is 2-4 h.
9. The lost circulation additive of claim 1, wherein the fatty acid modified calcium carbonate is C 15 ～C 18 Fatty acid modified calcium carbonate; the granularity of the lipophilic calcium carbonate is 100-1200 nm.
10. The lost circulation additive of claim 1, wherein the fatty acid modified calcium carbonate is prepared by a process comprising the steps of: mixing calcium carbonate and fatty acid in an organic solvent for reaction, carrying out solid-liquid separation, and drying to obtain fatty acid modified calcium carbonate; the mass ratio of the calcium carbonate to the fatty acid used for preparing the fatty acid modified calcium carbonate is (6-18) (5.4-9); the temperature of the mixing reaction carried out in the preparation of the fatty acid modified calcium carbonate is 50-70 ℃ and the time is 2-4 h.
11. A method of preparing a plugging agent according to any one of claims 1-10, comprising the steps of: and uniformly mixing the components in the formula amount to obtain the plugging agent.
12. Use of a plugging agent according to any one of claims 1-10 in an oil-based drilling fluid.
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