CN116426255A - Microcapsule lubricant and preparation method and application thereof - Google Patents
Microcapsule lubricant and preparation method and application thereof Download PDFInfo
- Publication number
- CN116426255A CN116426255A CN202310412458.7A CN202310412458A CN116426255A CN 116426255 A CN116426255 A CN 116426255A CN 202310412458 A CN202310412458 A CN 202310412458A CN 116426255 A CN116426255 A CN 116426255A
- Authority
- CN
- China
- Prior art keywords
- microcapsule
- lubricant
- monomer
- core material
- surfactant
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000003094 microcapsule Substances 0.000 title claims abstract description 114
- 239000000314 lubricant Substances 0.000 title claims abstract description 105
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 127
- 239000000178 monomer Substances 0.000 claims abstract description 67
- 239000011162 core material Substances 0.000 claims abstract description 55
- 239000010687 lubricating oil Substances 0.000 claims abstract description 51
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 43
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 39
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 35
- 238000005553 drilling Methods 0.000 claims abstract description 33
- 239000004094 surface-active agent Substances 0.000 claims abstract description 30
- 238000000034 method Methods 0.000 claims abstract description 25
- 239000003921 oil Substances 0.000 claims abstract description 23
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 19
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 17
- 239000003999 initiator Substances 0.000 claims abstract description 17
- 238000002156 mixing Methods 0.000 claims abstract description 16
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 16
- 238000011065 in-situ storage Methods 0.000 claims abstract description 15
- 239000002608 ionic liquid Substances 0.000 claims abstract description 14
- 239000002135 nanosheet Substances 0.000 claims abstract description 11
- 230000008569 process Effects 0.000 claims abstract description 8
- 239000002245 particle Substances 0.000 claims description 45
- 239000011259 mixed solution Substances 0.000 claims description 41
- 239000000377 silicon dioxide Substances 0.000 claims description 36
- 238000006243 chemical reaction Methods 0.000 claims description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 15
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 14
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 13
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 13
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical group [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 8
- SOGAXMICEFXMKE-UHFFFAOYSA-N Butylmethacrylate Chemical compound CCCCOC(=O)C(C)=C SOGAXMICEFXMKE-UHFFFAOYSA-N 0.000 claims description 6
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 6
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 6
- 239000002612 dispersion medium Substances 0.000 claims description 6
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims description 6
- -1 trihexyl (tetradecyl) phosphine phosphate Chemical compound 0.000 claims description 6
- 239000003638 chemical reducing agent Substances 0.000 claims description 5
- 239000002064 nanoplatelet Substances 0.000 claims description 5
- 239000007800 oxidant agent Substances 0.000 claims description 5
- 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 5
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 claims description 4
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 4
- 230000001590 oxidative effect Effects 0.000 claims description 4
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 4
- 229920000053 polysorbate 80 Polymers 0.000 claims description 4
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 4
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical group [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 4
- LPMBTLLQQJBUOO-KTKRTIGZSA-N (z)-n,n-bis(2-hydroxyethyl)octadec-9-enamide Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)N(CCO)CCO LPMBTLLQQJBUOO-KTKRTIGZSA-N 0.000 claims description 3
- MYWOJODOMFBVCB-UHFFFAOYSA-N 1,2,6-trimethylphenanthrene Chemical compound CC1=CC=C2C3=CC(C)=CC=C3C=CC2=C1C MYWOJODOMFBVCB-UHFFFAOYSA-N 0.000 claims description 3
- OGBWMWKMTUSNKE-UHFFFAOYSA-N 1-(2-methylprop-2-enoyloxy)hexyl 2-methylprop-2-enoate Chemical compound CCCCCC(OC(=O)C(C)=C)OC(=O)C(C)=C OGBWMWKMTUSNKE-UHFFFAOYSA-N 0.000 claims description 3
- SAMJGBVVQUEMGC-UHFFFAOYSA-N 1-ethenoxy-2-(2-ethenoxyethoxy)ethane Chemical compound C=COCCOCCOC=C SAMJGBVVQUEMGC-UHFFFAOYSA-N 0.000 claims description 3
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 3
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 3
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 3
- 150000001412 amines Chemical group 0.000 claims description 3
- DDXLVDQZPFLQMZ-UHFFFAOYSA-M dodecyl(trimethyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCC[N+](C)(C)C DDXLVDQZPFLQMZ-UHFFFAOYSA-M 0.000 claims description 3
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 3
- MBGQQKKTDDNCSG-UHFFFAOYSA-N ethenyl-diethoxy-methylsilane Chemical compound CCO[Si](C)(C=C)OCC MBGQQKKTDDNCSG-UHFFFAOYSA-N 0.000 claims description 3
- WOXXJEVNDJOOLV-UHFFFAOYSA-N ethenyl-tris(2-methoxyethoxy)silane Chemical compound COCCO[Si](OCCOC)(OCCOC)C=C WOXXJEVNDJOOLV-UHFFFAOYSA-N 0.000 claims description 3
- UEZVMMHDMIWARA-UHFFFAOYSA-M phosphonate Chemical compound [O-]P(=O)=O UEZVMMHDMIWARA-UHFFFAOYSA-M 0.000 claims description 3
- FSDNTQSJGHSJBG-UHFFFAOYSA-N piperidine-4-carbonitrile Chemical compound N#CC1CCNCC1 FSDNTQSJGHSJBG-UHFFFAOYSA-N 0.000 claims description 3
- NHARPDSAXCBDDR-UHFFFAOYSA-N propyl 2-methylprop-2-enoate Chemical compound CCCOC(=O)C(C)=C NHARPDSAXCBDDR-UHFFFAOYSA-N 0.000 claims description 3
- 229940083575 sodium dodecyl sulfate Drugs 0.000 claims description 3
- 235000019333 sodium laurylsulphate Nutrition 0.000 claims description 3
- ZORQXIQZAOLNGE-UHFFFAOYSA-N 1,1-difluorocyclohexane Chemical compound FC1(F)CCCCC1 ZORQXIQZAOLNGE-UHFFFAOYSA-N 0.000 claims description 2
- HNSDLXPSAYFUHK-UHFFFAOYSA-N 1,4-bis(2-ethylhexyl) sulfosuccinate Chemical compound CCCCC(CC)COC(=O)CC(S(O)(=O)=O)C(=O)OCC(CC)CCCC HNSDLXPSAYFUHK-UHFFFAOYSA-N 0.000 claims description 2
- ZDQNWDNMNKSMHI-UHFFFAOYSA-N 1-[2-(2-prop-2-enoyloxypropoxy)propoxy]propan-2-yl prop-2-enoate Chemical compound C=CC(=O)OC(C)COC(C)COCC(C)OC(=O)C=C ZDQNWDNMNKSMHI-UHFFFAOYSA-N 0.000 claims description 2
- HWSSEYVMGDIFMH-UHFFFAOYSA-N 2-[2-[2-(2-methylprop-2-enoyloxy)ethoxy]ethoxy]ethyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCCOCCOCCOC(=O)C(C)=C HWSSEYVMGDIFMH-UHFFFAOYSA-N 0.000 claims description 2
- LZMNXXQIQIHFGC-UHFFFAOYSA-N 3-[dimethoxy(methyl)silyl]propyl 2-methylprop-2-enoate Chemical compound CO[Si](C)(OC)CCCOC(=O)C(C)=C LZMNXXQIQIHFGC-UHFFFAOYSA-N 0.000 claims description 2
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 claims description 2
- XOJWAAUYNWGQAU-UHFFFAOYSA-N 4-(2-methylprop-2-enoyloxy)butyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCCCCOC(=O)C(C)=C XOJWAAUYNWGQAU-UHFFFAOYSA-N 0.000 claims description 2
- DBCAQXHNJOFNGC-UHFFFAOYSA-N 4-bromo-1,1,1-trifluorobutane Chemical compound FC(F)(F)CCCBr DBCAQXHNJOFNGC-UHFFFAOYSA-N 0.000 claims description 2
- JHWGFJBTMHEZME-UHFFFAOYSA-N 4-prop-2-enoyloxybutyl prop-2-enoate Chemical compound C=CC(=O)OCCCCOC(=O)C=C JHWGFJBTMHEZME-UHFFFAOYSA-N 0.000 claims description 2
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 2
- IYFATESGLOUGBX-YVNJGZBMSA-N Sorbitan monopalmitate Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O IYFATESGLOUGBX-YVNJGZBMSA-N 0.000 claims description 2
- VBIIFPGSPJYLRR-UHFFFAOYSA-M Stearyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCCC[N+](C)(C)C VBIIFPGSPJYLRR-UHFFFAOYSA-M 0.000 claims description 2
- DAKWPKUUDNSNPN-UHFFFAOYSA-N Trimethylolpropane triacrylate Chemical compound C=CC(=O)OCC(CC)(COC(=O)C=C)COC(=O)C=C DAKWPKUUDNSNPN-UHFFFAOYSA-N 0.000 claims description 2
- OKKRPWIIYQTPQF-UHFFFAOYSA-N Trimethylolpropane trimethacrylate Chemical compound CC(=C)C(=O)OCC(CC)(COC(=O)C(C)=C)COC(=O)C(C)=C OKKRPWIIYQTPQF-UHFFFAOYSA-N 0.000 claims description 2
- 229940018602 docusate Drugs 0.000 claims description 2
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 2
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 2
- ZLNAFSPCNATQPQ-UHFFFAOYSA-N ethenyl-dimethoxy-methylsilane Chemical compound CO[Si](C)(OC)C=C ZLNAFSPCNATQPQ-UHFFFAOYSA-N 0.000 claims description 2
- MABAWBWRUSBLKQ-UHFFFAOYSA-N ethenyl-tri(propan-2-yloxy)silane Chemical compound CC(C)O[Si](OC(C)C)(OC(C)C)C=C MABAWBWRUSBLKQ-UHFFFAOYSA-N 0.000 claims description 2
- SUPCQIBBMFXVTL-UHFFFAOYSA-N ethyl 2-methylprop-2-enoate Chemical compound CCOC(=O)C(C)=C SUPCQIBBMFXVTL-UHFFFAOYSA-N 0.000 claims description 2
- STVZJERGLQHEKB-UHFFFAOYSA-N ethylene glycol dimethacrylate Substances CC(=C)C(=O)OCCOC(=O)C(C)=C STVZJERGLQHEKB-UHFFFAOYSA-N 0.000 claims description 2
- YDKNBNOOCSNPNS-UHFFFAOYSA-N methyl 1,3-benzoxazole-2-carboxylate Chemical compound C1=CC=C2OC(C(=O)OC)=NC2=C1 YDKNBNOOCSNPNS-UHFFFAOYSA-N 0.000 claims description 2
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 2
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 2
- 239000000244 polyoxyethylene sorbitan monooleate Substances 0.000 claims description 2
- FBCQUCJYYPMKRO-UHFFFAOYSA-N prop-2-enyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCC=C FBCQUCJYYPMKRO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 2
- 235000010265 sodium sulphite Nutrition 0.000 claims description 2
- 239000001593 sorbitan monooleate Substances 0.000 claims description 2
- 235000011069 sorbitan monooleate Nutrition 0.000 claims description 2
- 229940035049 sorbitan monooleate Drugs 0.000 claims description 2
- HVUMOYIDDBPOLL-XWVZOOPGSA-N Sorbitan monostearate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O HVUMOYIDDBPOLL-XWVZOOPGSA-N 0.000 claims 1
- 235000011076 sorbitan monostearate Nutrition 0.000 claims 1
- 239000001587 sorbitan monostearate Substances 0.000 claims 1
- 229940035048 sorbitan monostearate Drugs 0.000 claims 1
- 229950003429 sorbitan palmitate Drugs 0.000 claims 1
- 239000012530 fluid Substances 0.000 abstract description 20
- 230000001050 lubricating effect Effects 0.000 abstract description 18
- 238000005461 lubrication Methods 0.000 abstract description 13
- 238000003756 stirring Methods 0.000 description 33
- 239000002002 slurry Substances 0.000 description 24
- 239000000440 bentonite Substances 0.000 description 23
- 229940092782 bentonite Drugs 0.000 description 23
- 229910000278 bentonite Inorganic materials 0.000 description 23
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 23
- 239000000463 material Substances 0.000 description 20
- 238000012360 testing method Methods 0.000 description 19
- 230000000694 effects Effects 0.000 description 18
- 239000008367 deionised water Substances 0.000 description 16
- 229910021641 deionized water Inorganic materials 0.000 description 16
- 238000001035 drying Methods 0.000 description 12
- 238000005406 washing Methods 0.000 description 12
- 230000009471 action Effects 0.000 description 11
- 230000014759 maintenance of location Effects 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 9
- 238000006073 displacement reaction Methods 0.000 description 9
- 239000012065 filter cake Substances 0.000 description 9
- 238000005098 hot rolling Methods 0.000 description 9
- 230000009467 reduction Effects 0.000 description 6
- 238000001914 filtration Methods 0.000 description 5
- 239000007764 o/w emulsion Substances 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 description 4
- 238000004132 cross linking Methods 0.000 description 4
- 239000000839 emulsion Substances 0.000 description 4
- 238000000227 grinding Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 230000001603 reducing effect Effects 0.000 description 4
- 238000010008 shearing Methods 0.000 description 4
- 239000007790 solid phase Substances 0.000 description 4
- 239000000725 suspension Substances 0.000 description 4
- 230000032683 aging Effects 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 239000004289 sodium hydrogen sulphite Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000002195 synergetic effect Effects 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- HVUMOYIDDBPOLL-XGKPLOKHSA-N [2-[(2r,3r,4s)-3,4-dihydroxyoxolan-2-yl]-2-hydroxyethyl] octadecanoate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(O)[C@H]1OC[C@H](O)[C@H]1O HVUMOYIDDBPOLL-XGKPLOKHSA-N 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000013270 controlled release Methods 0.000 description 2
- 229920006037 cross link polymer Polymers 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 229920000426 Microplastic Polymers 0.000 description 1
- IYFATESGLOUGBX-NDUCAMMLSA-N [2-[(2r,3r,4s)-3,4-dihydroxyoxolan-2-yl]-2-hydroxyethyl] hexadecanoate Chemical compound CCCCCCCCCCCCCCCC(=O)OCC(O)[C@H]1OC[C@H](O)[C@H]1O IYFATESGLOUGBX-NDUCAMMLSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- DBLFQTDPPZZDGX-UHFFFAOYSA-N bis(6-methylheptoxy)-oxophosphanium Chemical group CC(C)CCCCCO[P+](=O)OCCCCCC(C)C DBLFQTDPPZZDGX-UHFFFAOYSA-N 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- ONCZQWJXONKSMM-UHFFFAOYSA-N dialuminum;disodium;oxygen(2-);silicon(4+);hydrate Chemical compound O.[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Na+].[Na+].[Al+3].[Al+3].[Si+4].[Si+4].[Si+4].[Si+4] ONCZQWJXONKSMM-UHFFFAOYSA-N 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- NMJORVOYSJLJGU-UHFFFAOYSA-N methane clathrate Chemical compound C.C.C.C.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O NMJORVOYSJLJGU-UHFFFAOYSA-N 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229920006254 polymer film Polymers 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229940080314 sodium bentonite Drugs 0.000 description 1
- 229910000280 sodium bentonite Inorganic materials 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- APSBXTVYXVQYAB-UHFFFAOYSA-M sodium docusate Chemical compound [Na+].CCCCC(CC)COC(=O)CC(S([O-])(=O)=O)C(=O)OCC(CC)CCCC APSBXTVYXVQYAB-UHFFFAOYSA-M 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 239000000230 xanthan gum Substances 0.000 description 1
- 229920001285 xanthan gum Polymers 0.000 description 1
- 229940082509 xanthan gum Drugs 0.000 description 1
- 235000010493 xanthan gum Nutrition 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F292/00—Macromolecular compounds obtained by polymerising monomers on to inorganic materials
-
- 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
- C09K8/04—Aqueous well-drilling compositions
- C09K8/14—Clay-containing compositions
- C09K8/18—Clay-containing compositions characterised by the organic compounds
- C09K8/22—Synthetic organic compounds
- C09K8/24—Polymers
-
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Abstract
The invention relates to the technical field of drilling fluid lubricants, and discloses a microcapsule lubricant, a preparation method and application thereof. The preparation method provided by the invention comprises the following steps: mixing a lubricating oil core material, a first monomer, a second monomer, modified nano silicon dioxide, a first surfactant, a second surfactant, an initiator, a cross-linking agent and water to perform in-situ polymerization reaction to obtain a microcapsule lubricant; the lubricating oil core material comprises No. 5 white oil, oil-soluble ionic liquid and graphene nano sheets. The microcapsule lubricant prepared by the preparation method provided by the invention has good lubricating effect and high temperature resistance. Because the microcapsule lubricant coats the lubricating oil core material, part of the microcapsule lubricant releases the core material to play a high-efficiency lubrication role after being damaged at the high friction and torque position in the drilling process, and part of the undamaged microcapsule lubricant can still be stably dispersed in the drilling fluid and can be recycled, so that the use concentration of the lubricant can be obviously reduced.
Description
Technical Field
The invention relates to the technical field of drilling fluid lubricants, in particular to a microcapsule lubricant, a preparation method and application thereof.
Background
The large-displacement well has the advantages of being capable of controlling the oil-containing area in a large range, improving the oil and gas recovery ratio, reducing the development cost of the oil field and the like, has obvious economic and social benefits, and is one of the most effective means for developing marginal oil fields at present. With the increasing energy demand and the increasing maturity of the large displacement drilling technology, the number of large displacement wells is continuously increased, and the horizontal displacement is also continuously prolonged. In the drilling process of a large-displacement horizontal well, the friction and torque problems of the tubular column determine the maximum extension of the horizontal displacement, and the tubular column is one of key factors for restricting the success of drilling. Currently, reducing downhole friction and torque by improving the lubricity of drilling fluids is one of the most dominant means.
In the drilling process, three friction modes of dry friction without any medium between a drill string and a well wall, boundary friction generated by the drill string and a well wall boundary film and flow friction generated by circulating flow of drilling fluid exist. To reduce friction, the lubricating properties of drilling fluids are currently improved primarily by the preference for high-efficiency lubricants. The current lubricants for drilling fluids mainly comprise solid lubricants and liquid lubricants. After solid lubricants such as graphite, plastic pellets and the like are added into the drilling fluid, the friction state is changed by changing the contact mode of the drill string and the casing or the open hole wall, so that the friction coefficient is effectively reduced. The liquid lubricants are of various types, and some lubricants can form hydrophobic films through adsorption on the surfaces of drill rods and mud cakes, so that direct contact between metal and between metal and rock of a downhole drilling tool and a well wall is converted into contact between the hydrophobic films, and the friction coefficient is remarkably reduced.
However, at present, the traditional lubricant is directly added into the drilling fluid, and after being uniformly dispersed, the lubricant acts along with the circulation of the drilling fluid, and the action mode has two defects: the first is that the lubricant is directly added into the drilling fluid to easily influence the rheological property, the fluid loss property and the like of the drilling fluid, for example, some emulsion lubricants are added into the drilling fluid to easily foam, so that the rheological property, the density and the like of the drilling fluid are obviously changed. The second disadvantage is that the lubricant acts equally well after being added to the drilling fluid and dispersed evenly, both at high friction and low friction. While in practice drilling often requires efficient lubrication at high friction.
In the field of oilfield chemistry, attempts have been made to apply microcapsule technology to acidizing, fracturing, well plugging, natural gas hydrate formation temperature control, and the like. However, the existing microcapsule has poor thermal stability and cannot protect the core material to realize the controlled release, so a technology for obtaining a microcapsule lubricant with good high temperature resistance, difficult decomposition at high temperature and excellent lubrication effect is needed.
Disclosure of Invention
The invention aims to solve the problems that the microcapsule lubricant is easy to degrade and decompose at high temperature and cannot protect a core material to realize controlled release in the prior art, and provides a preparation method and application thereof.
In order to achieve the above object, a first aspect of the present invention provides a method for preparing a microcapsule lubricant, the method comprising: mixing a lubricating oil core material, a first monomer, a second monomer, modified nano silicon dioxide, a first surfactant, a second surfactant, an initiator, a cross-linking agent and water, and carrying out in-situ polymerization reaction to obtain a microcapsule lubricant;
the lubricating oil core material comprises No. 5 white oil, oil-soluble ionic liquid and graphene nano sheets.
The second aspect of the invention provides a microcapsule lubricant prepared by the preparation method, wherein the average particle size of the microcapsule lubricant is 3-50 mu m, and the temperature resistance is above 160 ℃.
The third aspect of the invention provides an application of the microcapsule lubricant provided by the invention in a high-temperature drilling environment.
Through the technical scheme, the invention has the beneficial effects that:
according to the invention, the solid-phase particle modified nano silicon dioxide is introduced, and the cross-linking structure is introduced through the cross-linking agent, so that the thermal stability of the microcapsule wall material is improved through the synergistic effect of the solid-phase particle modified nano silicon dioxide and the cross-linking agent. Compared with the microcapsule lubricant prepared by the preparation method without adding modified nano silicon dioxide, the temperature resistance of the microcapsule lubricant prepared by the preparation method provided by the invention is obviously enhanced.
The microcapsule lubricant provided by the invention has good lubricating property, heat stability and shearing resistance in the downhole circulation process. The microcapsule lubricant disclosed by the invention coats the lubricating oil core material, when high friction resistance is encountered in the downhole circulation drilling process, the microcapsule is extruded at the high friction resistance or the wall material is damaged under the strong shearing action, the lubricating oil core material is released, the local concentration effect is formed, the lubricating effect is effectively exerted, and part of the undamaged microcapsule is still stably dispersed in the drilling fluid and can be recycled, so that the use concentration of the lubricant is obviously reduced. On one hand, the lubricating oil is coated, so that the influence of the lubricating oil on the performances such as drilling fluid rheological property, fluid loss and the like is avoided, more importantly, the problem that the lubricating oil is diluted after being added into the drilling fluid and uniformly dispersed and cannot act on a key high friction part is avoided, and the lubricating oil has great significance in reducing friction resistance and torque extension horizontal displacement of a large-displacement horizontal well.
In the preferred embodiment of the invention, the wall material of the obtained microcapsule lubricant has more excellent flexibility and rigidity by further selecting the types and the proportions of the proper first monomer, the proper second monomer and the modified nano silicon dioxide, the types and the addition amounts of the proper first surfactant, the proper second surfactant, the proper cross-linking agent and the proper initiator and the proper in-situ polymerization reaction conditions, thereby further improving the thermal stability of the microcapsule lubricant. In addition, the invention further improves the lubricating performance of the microcapsule lubricant by selecting proper adding amount of the lubricating oil core material and proportion of each lubricating oil raw material in the lubricating oil core material.
Drawings
Fig. 1 is a view of the morphology of the microcapsule lubricant observed under a polarizing microscope.
Detailed Description
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
The first aspect of the present invention provides a method for preparing a microcapsule lubricant, the method comprising: mixing a lubricating oil core material, a first monomer, a second monomer, modified nano silicon dioxide, a first surfactant, a second surfactant, an initiator, a cross-linking agent and water, and carrying out in-situ polymerization reaction to obtain a microcapsule lubricant;
the lubricating oil core material comprises No. 5 white oil, oil-soluble ionic liquid and graphene nano sheets.
The invention comprises the steps of emulsifying a lubricating oil core material comprising No. 5 white oil, oil-soluble ionic liquid and graphene nano sheets into water through a second surfactant to form an oil-in-water emulsion, wherein the first surfactant and the second surfactant cooperate to form a stable oil-in-water emulsion. And then, under the action of a cross-linking agent and an initiator, the first monomer, the second monomer and the modified nano silicon dioxide carry out cross-linking polymerization reaction on the surface of the emulsion liquid drop, so that the emulsion liquid drop is coated, and a microcapsule structure is formed.
According to the invention, the solid-phase particle modified nano silicon dioxide is introduced, and the cross-linking structure is introduced through the cross-linking agent, so that the thermal stability of the microcapsule wall material is improved through the synergistic effect of the solid-phase particle modified nano silicon dioxide and the cross-linking agent. Compared with the microcapsule lubricant prepared by the preparation method without adding modified nano silicon dioxide, the temperature resistance of the microcapsule lubricant prepared by the preparation method provided by the invention is obviously enhanced.
The microcapsule lubricant prepared by the preparation method provided by the invention has good thermal stability and lubricating property, when encountering high friction resistance in the downhole circulation drilling process, the microcapsule is extruded at the high friction resistance or the wall material with strong shearing action is damaged, the lubricating oil core material is released, the local concentration effect is formed, the lubricating effect is effectively exerted, and part of undamaged microcapsule is still stably dispersed in the drilling fluid.
According to the present invention, preferably, the weight ratio of the first monomer, the second monomer, and the modified nano-silica is (2-5): (2-5): 1. when the weight ratio of the first monomer, the second monomer and the modified nano silica satisfies the above range, the first monomer, the second monomer and the modified nano silica can form a dense polymer film on the surface of the lubricating oil core material liquid drop, preventing the lubricating oil core material from being released rapidly.
According to the present invention, it is preferable that the amount of the lubricant core material added is 2 to 4 parts by weight based on 1 part by weight of the total amount of the first monomer, the second monomer, and the modified nano silica. When the addition amount of the lubricating oil core material meets the range, on one hand, the formed microcapsule can be ensured to have proper core-wall ratio, the wall material with too high core material content is prevented from being difficult to effectively coat the microcapsule, and on the other hand, the lubricating oil core material can effectively play the role of lubrication and drag reduction after being released.
According to the present invention, preferably, the crosslinking agent is added in an amount of 0.01 to 0.05wt% based on the total weight of the first monomer, the second monomer and the modified nano-silica;
according to the present invention, it is preferable that the initiator is added in an amount of 0.1 to 0.5wt% based on the total weight of the first monomer, the second monomer and the modified nano-silica.
According to the present invention, the volume ratio of the lubricating oil core material to water is preferably (20-30): 100.
According to the invention, the weight ratio of the first surfactant to water is preferably (0.1-1): 100. When the addition amount of the first surfactant satisfies the above range, the lubricating oil core material can be assisted in being stably dispersed in water.
According to the invention, the weight ratio of the second surfactant to water is preferably (1.2-3): 100. When the addition amount of the second surfactant satisfies the above range, the lubricating oil core material can be dispersed in water to form stable oil-in-water emulsion droplets.
According to the present invention, preferably, the in-situ polymerization is carried out at a temperature of 55 to 85℃for a time of 4 to 24 hours.
Further, the temperature of the in-situ polymerization reaction is 60-75 ℃ and the time is 6-12h.
In the invention, after the in-situ polymerization reaction is finished, carrying out suction filtration, washing and drying to obtain the microcapsule lubricant;
wherein, the washing is carried out by adopting absolute ethyl alcohol and deionized water.
According to the present invention, preferably, the amount of the 5# white oil, the oil-soluble ionic liquid, and the graphene nanoplatelets added is 70 to 90wt%, 10 to 20wt%, and 5 to 10wt%, respectively, based on the total weight of the lubricating oil core material. When the addition amount of the No. 5 white oil, the oil-soluble ionic liquid and the graphene nano-sheets meets the above range, the three can be synergistic, and the lubrication effect can be exerted to the maximum extent.
According to the present invention, preferably, the oil-soluble ionic liquid is selected from at least one of diisooctyl cetyl trioctyl phosphonate, sodium cetyl trioctyl quaternary amine docusate, diisooctyl trihexyl (tetradecyl) phosphine phosphate and trihexyl tetradecylphosphine bis (2-ethylhexyl) phosphate.
According to the present invention, preferably, the graphene nanoplatelets have a thickness of 4-20nm and a length of 1-10 μm. When the thickness and the length of the graphene nano sheet meet the above ranges, the abrasion resistance of the graphene nano sheet can be improved, and the interface friction force can be reduced.
According to the present invention, preferably, the first surfactant is selected from at least one of sorbitan palmitate (Span-40), sorbitan monostearate (Span-60), sorbitan monooleate (Span-80) and oleic acid diethanolamide.
According to the present invention, preferably, the second surfactant is selected from at least one of polyoxyethylene sorbitan monooleate (Tween-80), octylphenol polyoxyethylene ether (OP-10), sodium dodecylbenzenesulfonate, sodium dodecylsulfate, dodecyltrimethylammonium chloride, cetyltrimethylammonium bromide and octadecyltrimethylammonium chloride.
According to the present invention, preferably, the first monomer is selected from one of methyl methacrylate, ethyl methacrylate, propyl methacrylate, and butyl methacrylate. The use of the above-mentioned substances as the first monomer contributes to the formation of a microcapsule lubricant excellent in temperature resistance.
According to the present invention, preferably, the second monomer is selected from one of acrylic acid, methacrylic acid, acrylamide and styrene. The above-mentioned substances can be used as the second monomer to form a microcapsule lubricant having good temperature resistance and good dispersibility.
According to the present invention, preferably, the crosslinking agent is at least one selected from pentaerythritol tetraacrylate, allyl methacrylate, 1, 4-butanediol diacrylate, hexanediol dimethacrylate, diethylene glycol divinyl ether, trimethylolpropane trimethacrylate, triethylene glycol dimethacrylate, dipropylene glycol diacrylate, tripropylene glycol diacrylate, neopentyl glycol diacrylate, trimethylolpropane triacrylate, divinylbenzene, ethylene glycol dimethacrylate and 1, 4-butanediol dimethacrylate.
Preferably, according to the present invention, the initiator is a redox system initiator.
Preferably, the weight ratio of the oxidant to the reducing agent in the redox system initiator is (1-3): 1. when the weight ratio of the oxidizing agent and the reducing agent satisfies the above range, the reaction of the first monomer, the second monomer, the modified nano-silica, and the crosslinking agent can be effectively initiated.
Preferably, the oxidant is ammonium persulfate and/or potassium persulfate, and the reducing agent is sodium sulfite and/or sodium bisulfite.
According to the present invention, preferably, the modified nanosilica is obtained by modifying nanosilica with a silane coupling agent.
According to the present invention, the nanosilica preferably has an average particle size of 10 to 100nm, preferably 10 to 50nm.
According to the present invention, preferably, the silane coupling agent is selected from at least one of methylvinyldimethoxy silane, methylvinyldiethoxy silane, vinyltrimethoxy silane, vinyltriethoxy silane, vinyltriisopropoxy silane, γ -methacryloxypropyl methyldimethoxy silane, γ -methacryloxypropyl trimethoxy silane, and vinyltris (β -methoxyethoxy) silane.
According to the present invention, preferably, the weight ratio of the nanosilica to the silane coupling agent is 1 (1-2). When the weight ratio of the nano-silica to the silane coupling agent satisfies the above range, a sufficient amount of the silane coupling agent can be grafted on the surface of the nano-silica, facilitating modification.
According to the present invention, preferably, the method of modification comprises: dispersing the nano silicon dioxide in a dispersion medium, and then reacting with the silane coupling agent to obtain the modified nano silicon dioxide.
According to the invention, the reaction is preferably carried out at a temperature of 50-75℃for a period of 4-24 hours.
Further, the reaction temperature is 50-70 ℃ and the reaction time is 6-12h.
According to the present invention, preferably, the dispersion medium is a mixture of absolute ethanol and water in a volume ratio of 1 (1-2).
According to the present invention, preferably, the weight ratio of the nanosilica to the dispersion medium is (1-5): 100.
In the invention, after the nano silicon dioxide reacts with the silane coupling agent, cooling, filtering, washing and drying are carried out to obtain white powder, namely the modified nano silicon dioxide;
wherein the solvent used for washing is chloroform and/or ethanol;
the drying temperature is 60-80 ℃ and the drying time is 12-24h.
According to a preferred embodiment of the present invention, the preparation method comprises the steps of:
(1) Firstly mixing the lubricating oil core material and the first surfactant to obtain a mixed solution 1;
(2) Dissolving the second surfactant in water to obtain a mixed solution 2;
(3) Performing second mixing on the modified nano silicon dioxide and the first monomer to obtain a mixed solution 3;
(4) Thirdly, mixing the mixed solution 1 with the mixed solution 2, and then fourth mixing with the mixed solution 3 to obtain a mixed solution 4;
(5) And fifthly, mixing the second monomer, the cross-linking agent and the initiator with the mixed solution 4, and carrying out in-situ polymerization reaction to obtain the microcapsule lubricant.
Preferably, in step (4), said third mixing and said fourth mixing are carried out under stirring conditions, said stirring being carried out at a speed of 500-2000rpm, preferably 1000-2000rpm.
The second aspect of the invention provides a microcapsule lubricant prepared by the preparation method, wherein the average particle size of the microcapsule lubricant is 3-50 mu m, and the temperature resistance is above 160 ℃.
The wall material of the microcapsule lubricant obtained by the method can be obtained by in-situ polymerization reaction of modified nano silicon dioxide, a first monomer and a second monomer in the presence of an initiator and a crosslinking agent, and the wall material has a chemical composition structure comprising structural units from the first monomer and the second monomer, a crosslinking structure formed under the action of the crosslinking agent, and the wall material also comprises the modified nano silicon dioxide. The wall material has good heat stability and lubricating property, and can be damaged by extrusion or strong shearing action at a high friction part when encountering high friction in the downhole circulation drilling process, so that the lubricating oil core material is released, a local concentration effect is formed, the lubricating effect is effectively exerted, and the microcapsules which are not damaged partially are still stably dispersed in the drilling fluid.
The third aspect of the invention provides an application of the microcapsule lubricant provided by the invention in a high-temperature drilling environment.
The present invention will be described in detail by examples.
In the following examples, the test methods and apparatus involved are as follows:
particle size test of microcapsule lubricants: 0.1g of the microcapsule lubricant was added to 100mL of deionized water, and after stirring at 10000rpm for 10min, the test was performed using a Bettersize2000 laser particle sizer.
And (3) observing the microcosmic appearance of the microcapsule lubricant: to 100mL of deionized water, 0.5g of the microcapsule lubricant was added, and after stirring at 10000rpm for 10 minutes, observation was performed by using a polarizing microscope.
Example 1
This example is intended to illustrate the preparation of a microcapsule lubricant
(1) 100g of deionized water and 100g of absolute ethyl alcohol are added into a three-neck flask, 3g of silicon dioxide with the average particle size of 12nm is slowly added under the condition of the stirring speed of 1000rpm, 3g of silane coupling agent KH570 is dropwise added after stirring for 30min, and the temperature is raised to 50 ℃ after the dropwise addition for 6h of reaction. Filtering after the reaction is finished, washing a filter cake with absolute ethyl alcohol for three times, and drying at 80 ℃ for 24 hours to obtain the modified nano silicon dioxide.
(2) 15g of cetyl trioctyl quaternary diisooctyl phosphonate salt and 5g of graphene nano sheets (with average thickness of 20nm and average length of 2 mu m) are dispersed into 80g of No. 5 white oil, and the mixture is stirred uniformly to obtain the mixed lubricating oil core material.
(3) 40g of mixed lubricating oil core material and 1g of Span-80 are accurately weighed and uniformly stirred to obtain a mixed solution 1. Accurately weighing 8g of methyl methacrylate and 4g of modified nano silicon dioxide, and uniformly stirring to obtain a mixed solution 3.
(4) 200mL of deionized water and 4g of OP-10 are added into a 500mL three-neck flask which is provided with a thermometer, a stirring rod, condensed water and water bath heating, after the mixture is fully dissolved, a mixed solution 2 is obtained, the mixed solution 1 is slowly added under the condition of a stirring speed of 1000rpm, after stirring for 30min, the mixed solution 3 is slowly added, after stirring for 30min, 8g of acrylic acid, 0.01g of pentaerythritol tetraacrylate, 0.04g of ammonium persulfate and 0.02g of sodium bisulphite are sequentially added into the mixed solution within 10 min. Then the temperature is raised to 75 ℃ and the temperature is maintained for stable reaction for 6h. After the reaction, the suspension was suction filtered. And (3) alternately washing the obtained filter cake with absolute ethyl alcohol and deionized water for 3 times, drying at 60 ℃ for 24 hours, and lightly grinding to obtain white powder particles, namely the microcapsule lubricant with the average particle size of 19.32 mu m. As can be seen from fig. 1, the microcapsule lubricant particles are mostly spherical and uniform.
Example 2
This example is intended to illustrate the preparation of a microcapsule lubricant
(1) 100g of deionized water and 50g of absolute ethyl alcohol are added into a three-neck flask, 1.5g of silicon dioxide with the average particle size of 50nm is slowly added under the condition of the stirring speed of 1000rpm, 3g of silane coupling agent methyl vinyl diethoxy silane is dropwise added after stirring for 30min, and the temperature is raised to 70 ℃ after the dropwise addition for 7h of reaction. Filtering after the reaction is finished, washing a filter cake with absolute ethyl alcohol for three times, and drying at 60 ℃ for 24 hours to obtain the modified nano silicon dioxide.
(2) 8.1g of cetyl trioctyl quaternary amine docusate sodium salt and 2.7g of graphene nano sheets (with the average thickness of 4nm and the average length of 1 μm) are dispersed into 43.2g of 5# white oil, and the mixture is stirred uniformly to obtain the mixed lubricating oil core material.
(3) 54g of mixed lubricating oil core material and 1.8g of Span-40 are accurately weighed and uniformly stirred to obtain a mixed solution 1. 11.6g of methyl methacrylate and 3.9g of modified nano silicon dioxide are accurately weighed and uniformly stirred to obtain a mixed solution 3.
(4) 180mL of deionized water and 5.4g of Tween-80 are added into a 500mL three-necked flask which is provided with a thermometer, a stirring rod, condensed water and water bath heating, the mixture is fully dissolved, a mixed solution 2 is obtained, the mixed solution 1 is slowly added under the condition that the stirring speed is 1200rpm, the mixed solution 3 is slowly added after stirring for 30min, and 11.6g of methacrylic acid, 0.0027g of hexanediol dimethacrylate, 0.014g of potassium persulfate and 0.013g of sodium bisulfite are sequentially added into the mixed solution within 10min after stirring for 30 min. Then the temperature is raised to 65 ℃ and the temperature is maintained for stable reaction for 12 hours. After the reaction, the suspension was suction filtered. And (3) alternately washing the obtained filter cake with absolute ethyl alcohol and deionized water for 3 times, drying at 80 ℃ for 24 hours, and lightly grinding to obtain white powder particles, namely the microcapsule lubricant with the average particle size of 14.67 mu m.
Example 3
This example is intended to illustrate the preparation of a microcapsule lubricant
(1) 75g of deionized water and 50g of absolute ethyl alcohol are added into a three-neck flask, 2g of silicon dioxide with the average particle size of 25nm is slowly added under the condition of the stirring speed of 1000rpm, 2.8g of silane coupling agent vinyl triethoxysilane is dropwise added after stirring for 30min, and the temperature is raised to 60 ℃ after the dropwise addition for reaction for 8h. Filtering after the reaction is finished, washing a filter cake with absolute ethyl alcohol for three times, and drying at 70 ℃ for 8 hours to obtain the modified nano silicon dioxide.
(2) 5.63g of diisooctyl tri-hexyl (tetradecyl) phosphine phosphate and 3.74g of graphene nanoplatelets (average thickness of 10nm and average length of 3 μm) are dispersed into 28.13g of 5# white oil, and the mixture is stirred uniformly to obtain the mixed lubricating oil core material.
(3) 37.5g of mixed lubricating oil core material and 0.75g of oleic acid diethanolamide are accurately weighed and uniformly stirred to obtain a mixed solution 1. Accurately weighing 5.47g of propyl methacrylate and 1.5g of modified nano silicon dioxide, and uniformly stirring to obtain a mixed solution 3.
(4) 150mL of deionized water and 3.15g of sodium dodecyl sulfate are added into a 500mL three-necked flask which is provided with a thermometer, a stirring rod, condensed water and water bath heating, after full dissolution, mixed solution 2 is obtained, mixed solution 1 is slowly added under the condition that the stirring speed is 1500rpm, mixed solution 3 is slowly added after stirring for 30min, and after stirring for 30min, 5.47g of acrylamide, 0.0038g of diethylene glycol divinyl ether, 0.02g of potassium persulfate and 0.02g of sodium bisulphite are sequentially added into the mixed solution within 10 min. Then the temperature is raised to 70 ℃ and the temperature is maintained for stable reaction for 8 hours. After the reaction, the suspension was suction filtered. And (3) alternately washing the obtained filter cake with absolute ethyl alcohol and deionized water for 3 times, drying at 70 ℃ for 24 hours, and lightly grinding to obtain white powder particles, namely the microcapsule lubricant with the average particle size of 8.79 mu m.
Example 4
This example is intended to illustrate the preparation of a microcapsule lubricant
(1) 96g of deionized water and 60g of absolute ethyl alcohol are added into a three-neck flask, 6.24g of silicon dioxide with the average particle size of 40nm is slowly added under the condition of the stirring speed of 1000rpm, 6.24g of silane coupling agent vinyltris (beta-methoxyethoxy) silane is dropwise added after stirring for 30min, and the temperature is raised to 55 ℃ after the dropwise addition for reaction for 6h. Filtering after the reaction is finished, washing a filter cake with absolute ethyl alcohol for three times, and drying at 80 ℃ for 12 hours to obtain the modified nano silicon dioxide.
(2) 8g of tri-hexyl tetradecylphosphine bis (2-ethylhexyl) phosphate and 8g of graphene nanoplatelets (average thickness of 5nm, average length of 1 μm) were dispersed in 32g of 5# white oil, and uniformly stirred to obtain a mixed lubricating oil core material.
(3) 40g of the mixed lubricating oil core material and 1.6g of Span60 are accurately weighed and uniformly stirred to obtain a mixed solution 1.8g of butyl methacrylate and 4g of modified nano silicon dioxide are accurately weighed and uniformly stirred to obtain a mixed solution 3.
(4) 150mL of deionized water and 4g of dodecyl trimethyl ammonium chloride are added into a 500mL three-necked flask which is provided with a thermometer, a stirring rod, condensed water and water bath heating, after full dissolution, mixed solution 2 is obtained, mixed solution 1 is slowly added under the condition of a stirring speed of 2000rpm, mixed solution 3 is slowly added after stirring for 30min, and after stirring for 30min, 8g of styrene, 0.008g of dipropylene glycol diacrylate, 0.06g of ammonium persulfate and 0.02g of sodium bisulphite are sequentially added into the mixed solution within 10 min. Then the temperature is raised to 70 ℃ and the temperature is maintained for stable reaction for 8 hours. After the reaction, the suspension was suction filtered. And (3) alternately washing the obtained filter cake with absolute ethyl alcohol and deionized water for 3 times, drying at 70 ℃ for 24 hours, and lightly grinding to obtain white powder particles, namely the microcapsule lubricant with the average particle size of 5.76 mu m.
Example 5
A microcapsule lubricant was prepared according to the method of example 1, except that the amount of methyl methacrylate added was 6.6g, the amount of acrylic acid added was 6.6g, and the amount of modified nano silica added was 6.6g, such that the weight ratio of methyl methacrylate (first monomer), acrylic acid (second monomer) and modified nano silica was 1:1:1, a microcapsule lubricant having an average particle diameter of 51.32 μm was obtained.
Example 6
A microcapsule lubricant was prepared as in example 1, except that the amount of methyl methacrylate added was 9.3g, the amount of acrylic acid added was 9.3g, and the amount of modified nano silica added was 1.4g, such that the weight ratio of methyl methacrylate (first monomer), acrylic acid (second monomer) and modified nano silica was 7:7:1, a microcapsule lubricant having an average particle diameter of 23.65 μm was obtained.
Example 7
Microcapsule lubricants were prepared in the same manner as in example 1, except that the amount of the lubricant core material added was varied. Specifically, in the step (3), 90g of the mixed lubricating oil core material and 1g of Span-80 are accurately weighed and uniformly stirred to obtain a mixed solution 1. The microcapsule lubricant was obtained, and its average particle diameter was 76.3. Mu.m.
Example 8
A microcapsule lubricant was prepared according to the method of example 1, except that the addition amounts of the first surfactant and the second surfactant were different. Specifically, in the step (3), the addition amount of Span-80 is 1g; in the step (4), the addition amount of OP-10 was 1.1g.
Example 9
Microcapsule lubricants were prepared as in example 1, except that the in situ polymerization conditions were different. Specifically, the temperature of the in-situ polymerization reaction was 50℃for 13 hours. The microcapsule lubricant was obtained, and its average particle diameter was 63.2. Mu.m.
Example 10
A microcapsule lubricant was prepared as in example 1, except that silica having an average particle diameter of 150nm was used. The microcapsule lubricant was obtained, and its average particle diameter was 84.5. Mu.m.
Example 11
A microcapsule lubricant was prepared as in example 1, except that the temperature of the reaction was 45℃and the time was 15 hours when preparing the modified nano-silica. The microcapsule lubricant was obtained, and its average particle diameter was 75.5. Mu.m.
Comparative example 1
A microcapsule lubricant was prepared in the same manner as in example 1 except that modified nano silica was not added, to obtain a microcapsule lubricant having an average particle diameter of 17.63. Mu.m.
Comparative example 2
A microcapsule lubricant was prepared in the same manner as in example 1 except that diisooctyl cetyl trioctyl phosphonate (oil-soluble ionic liquid) was not added, to obtain a microcapsule lubricant having an average particle diameter of 15.62. Mu.m.
Test example 1 high temperature resistance test
3g of the microcapsule lubricant of each example is respectively added into 100mL of deionized water, the mixture is transferred into an aging tank after being stirred uniformly, the mixture is rolled for 16 hours at 160 ℃, the mixture is cooled to room temperature after the hot rolling is finished, the mixture is filtered, the filter cake is washed for 3 times by absolute ethyl alcohol, the residual solid mass is weighed after vacuum drying, and the microcapsule mass retention rate is calculated. Table 1 shows the mass retention of the microcapsule lubricants after 16h hot rolling at 160℃in each example.
TABLE 1
As can be seen from the test results in Table 1, the mass retention rate of examples 1-4 after being rolled at 160 ℃ at high temperature is above 75%, and the temperature resistance of the microcapsule after the inorganic nano material is introduced is significantly improved as no nano silicon dioxide is added into the wall material in comparative example 1, and the temperature resistance is poor and the mass retention rate is only 40%.
In addition, example 5 changed the weight ratio of methyl methacrylate (first monomer), acrylic acid (second monomer) and modified nano silica, and the mass retention rate was reduced compared to example 1, because the nano silica was excessively added, and because the rigid structure thereof was difficult to form a dense wall material film with the crosslinked polymer, the permeability of the lubricating oil core material was enhanced, which was unfavorable for the stabilization of the lubricating oil core material; example 6 changed the weight ratio of methyl methacrylate (first monomer), acrylic acid (second monomer) and modified nanosilica, and compared with example 1, the mass retention rate was also lower, indicating that when the nanosilica content was lower, the thermal degradation of the crosslinked polymer could not be effectively delayed, resulting in the microcapsule wall material being easily degraded after high temperature, so the mass retention rate was lower; example 7 varying the weight ratio of lubricating oil core to methyl methacrylate (first monomer), acrylic acid (second monomer) and modified nanosilica makes it difficult to form a stable oil-in-water emulsion, resulting in larger microcapsule lubricant particles and lower mass retention after high temperature action. Example 8 the formation of an oil-in-water emulsion was difficult due to the lower amount of secondary surfactant added, and the mass retention of the formed microcapsule particles after high temperature action was also lower. Example 9 the lower reaction temperature resulted in a larger particle size of the microcapsule lubricant and thus lower mass retention after high temperature. The nano-silica selected in example 10 had a larger particle size, resulting in a larger average particle size of the microcapsule lubricant and lower mass retention after high temperature. In example 11, the temperature is low during modification of the nano silica, and the silica is difficult to be sufficiently modified, so that the reaction degree is low during subsequent reaction with the first monomer and the second monomer, resulting in a decrease in thermal stability of the microcapsule lubricant.
Test example 2 lubricating property test
Preparing bentonite-based slurry: 16g of sodium bentonite and 0.8g of sodium carbonate are added into 400mL of clear water, and after stirring for 30min at 10000rpm, the bentonite slurry is obtained after sealed maintenance for more than 24h.
After adding 0.6g of xanthan gum to 400mL of bentonite-based slurry and stirring at 8000rpm for 10min, respectively adding 12g of microcapsule lubricant or No. 5 white oil of each example, stirring for 10min, and testing lubricity by using a four-ball friction and wear tester (Jinan times gold testing machine Co., ltd.) under the following test conditions: the load is 600N, the temperature is 25 ℃, the time is 1800s, and the rotating speed is 1000rpm. After the test, the surface of the steel ball with the mill spots was observed by a metallographic microscope, and table 2 shows the diameter results of the mill spots on the surface of the steel ball with the mill spots of each example.
TABLE 2
| Test sample | Grind diameter/micron |
| Bentonite slurry +5# white oil | 701 |
| Bentonite slurry + example 1 | 442 |
| Bentonite slurry + example 2 | 430 |
| Bentonite slurry + example 3 | 418 |
| Bentonite slurry + example 4 | 415 |
| Bentonite slurry + example 5 | 518 |
| Bentonite slurry + example 6 | 536 |
| Bentonite slurry + example 7 | 543 |
| Bentonite slurry + example 8 | 512 |
| Bentonite slurry + example 9 | 532 |
| Bentonite slurry + example 10 | 534 |
| Bentonite slurry + example 11 | 526 |
| Bentonite-based slurry + comparative example 1 | 589 |
| Bentonite-based slurry + comparative example 2 | 612 |
From the test results of table 2, it is seen that the plaque diameters of examples 1 to 4 were significantly reduced compared to the 5# white oil, because the microcapsules were crushed and the inner lubricating oil core material was gradually released during frictional wear. Comparative example 1 was not added with modified nanosilica, comparative example 2 was not added with ionic liquid, and the plaque diameters were significantly larger than in example 1, indicating a decrease in the friction reducing effect.
In addition, examples 5 and 6, in which the weight ratio of methyl methacrylate (first monomer), acrylic acid (second monomer) and modified nano-silica was changed, had an increased plaque diameter compared to example 1, indicating that too high or too low content of modified nano-silica resulted in a decrease in the friction-reducing effect of the microcapsule lubricant; example 7 changes the weight ratio of the lubricating oil core material to methyl methacrylate (first monomer), acrylic acid (second monomer) and modified nano-silica, the formed microcapsule lubricant has larger particle size, less lubricant on unit surface, resulting in reduced antiwear and antifriction effects; example 8 the resulting microcapsule lubricant has reduced antiwear and antifriction effects compared to example 1 due to reduced emulsion stability. The microcapsule lubricant obtained in example 9 has a larger particle size and reduced antiwear effect. In the embodiment 10, nano silicon dioxide with larger particle size is added, so that the nano silicon dioxide is easily agglomerated into large particles in the reaction process, and the antiwear effect is weakened; the microcapsule wall material obtained in example 11 has relatively low silica content, and is difficult to effectively exert the silica effect, so that the abrasion resistance effect is relatively weak.
Test example 3 high temperature resistance and lubricity test
To 400mL of bentonite slurry, 12g of the microcapsule lubricant or 5# white oil of each example was added, and the mixture was stirred at 10000rpm for 10 minutes and transferred to an aging tank. The aging tank was thermally rolled at 160℃for 16 hours. The EP-1 extreme pressure lubrication device was used to test the extreme pressure lubrication coefficients before and after the hot rolling of the above experimental slurry, and the test results are shown in Table 3.
TABLE 3 Table 3
As can be seen from the test results in Table 3, after the 5# white oil is added into the bentonite slurry, the lubricating effect is better before and after hot rolling, and the lubricating coefficient reduction rate is more than 50% compared with the bentonite slurry. After the addition of examples 1 to 4, the lubricating oil core material was not released due to the dense coating and sealing effect of the microcapsules before and after the hot rolling, and thus the extreme pressure lubrication coefficient was slightly lowered. After 160 ℃ hot rolling, the compactness of the microcapsule wall material is reduced under the action of heat, the core material is released to exert the efficient lubrication effect, and the reduction rate of the lubrication coefficient is more than 75%. In comparative example 1, nano silicon dioxide is not introduced into the wall material, and the temperature resistance and compactness of the wall material are inferior to those of the examples, so that part of core material is released when the wall material is added into bentonite slurry, and the reduction rate of the extreme pressure lubrication coefficient reaches 26.1% before hot rolling. In comparative example 2, since no ionic liquid is added into the core material, the lubricating effect of the microcapsule lubricant released after hot rolling is inferior to that of example 1, the reduction rate of the lubricating coefficient is 60.4%, but still higher than that of white oil, and the microcapsule lubricant provided by the invention has the effects of high temperature resistance and high efficiency lubrication.
In addition, examples 5 and 6 changed the weight ratio of methyl methacrylate (first monomer), acrylic acid (second monomer) and modified nano silica, and the reduction rate of the lubricating coefficient after high temperature action was reduced compared with example 1, indicating that changing the proportion of the components in the wall material had a significant effect on the release of the microcapsule wall material and the lubricating effect.
From this, it can be seen that the reasonable combination of the # 5 white oil, the lipophilic ionic liquid and the graphene sheets through the proper proportion and the different reaction monomers has remarkable effects of improving the high temperature stability of the microcapsule and improving the friction resistance and the torque of the large-displacement well.
As can be seen from the test results of examples 7 to 11, the microcapsule lubricants of examples 7 to 11 were added to the bentonite slurry, and had a certain lubricating effect before hot rolling, because the microcapsule particles obtained in the above examples had a larger particle size, and the microcapsule particles were easily broken to release the core material after being added to the bentonite slurry, thereby exerting a certain lubricating effect. It can be seen that the microcapsules obtained in examples 7 to 11 do not perform well in targeted release of the microcapsules. Since the core material is easily released at normal temperature, the lubrication effect thereof is reduced after the high temperature action as compared with example 1.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the invention, all falling within the scope of protection of the invention.
Claims (11)
1. A method of preparing a microcapsule lubricant, the method comprising: mixing a lubricating oil core material, a first monomer, a second monomer, modified nano silicon dioxide, a first surfactant, a second surfactant, an initiator, a cross-linking agent and water, and carrying out in-situ polymerization reaction to obtain a microcapsule lubricant;
the lubricating oil core material comprises No. 5 white oil, oil-soluble ionic liquid and graphene nano sheets.
2. The method of claim 1, wherein the weight ratio of the first monomer, the second monomer, and the modified nanosilica is (2-5): (2-5): 1, a step of;
preferably, the lubricating oil core material is added in an amount of 2 to 4 parts by weight based on 1 part by weight of the total amount of the first monomer, the second monomer and the modified nano silica;
preferably, the crosslinking agent is added in an amount of 0.01 to 0.05wt% based on the total weight of the first monomer, the second monomer and the modified nano-silica;
preferably, the initiator is added in an amount of 0.1 to 0.5wt% based on the total weight of the first monomer, the second monomer and the modified nano-silica;
preferably, the volume ratio of the lubricating oil core material to the water is (20-30): 100;
preferably, the weight ratio of the first surfactant to water is (0.1-1): 100;
preferably, the weight ratio of the second surfactant to water is (1.2-3): 100.
3. The method according to claim 1 or 2, wherein the in-situ polymerization is carried out at a temperature of 55-85 ℃ for a period of 4-24 hours;
preferably, the temperature of the in-situ polymerization reaction is 60-75 ℃ and the time is 6-12h.
4. The method according to any one of claims 1 to 3, wherein the amounts of the 5# white oil, the oil-soluble ionic liquid, and the graphene nanoplatelets added are 70 to 90wt%, 10 to 20wt%, and 5 to 10wt%, respectively, based on the total weight of the lubricating oil core material;
preferably, the oil-soluble ionic liquid is selected from at least one of diisooctyl cetyl trioctyl phosphonate, sodium cetyl trioctyl quaternary amine docusate, diisooctyl trihexyl (tetradecyl) phosphine phosphate and trihexyl tetradecylphosphine bis (2-ethylhexyl) phosphate;
preferably, the graphene nano-sheets have a thickness of 4-20nm and a length of 1-10 μm.
5. The method according to any one of claims 1 to 4, wherein the first surfactant is at least one selected from sorbitan palmitate, sorbitan monostearate, sorbitan monooleate and oleic acid diethanolamide;
preferably, the second surfactant is selected from at least one of polyoxyethylene sorbitan monooleate, octylphenol polyoxyethylene ether, sodium dodecylbenzene sulfonate, sodium dodecylsulfate, dodecyltrimethylammonium chloride, cetyltrimethylammonium bromide and octadecyltrimethylammonium chloride;
preferably, the first monomer is selected from one of methyl methacrylate, ethyl methacrylate, propyl methacrylate and butyl methacrylate;
preferably, the second monomer is selected from one of acrylic acid, methacrylic acid, acrylamide and styrene;
preferably, the cross-linking agent is selected from at least one of pentaerythritol tetraacrylate, allyl methacrylate, 1, 4-butanediol diacrylate, hexanediol dimethacrylate, diethylene glycol divinyl ether, trimethylolpropane trimethacrylate, triethylene glycol dimethacrylate, dipropylene glycol diacrylate, tripropylene glycol diacrylate, neopentyl glycol diacrylate, trimethylolpropane triacrylate, divinylbenzene, ethylene glycol dimethacrylate and 1, 4-butanediol dimethacrylate.
6. The process according to any one of claims 1 to 5, wherein the initiator is a redox system initiator;
preferably, the weight ratio of the oxidant to the reducing agent in the redox system initiator is (1-3): 1, a step of;
preferably, the oxidant is ammonium persulfate and/or potassium persulfate, and the reducing agent is sodium sulfite and/or sodium bisulfite.
7. The method according to any one of claims 1 to 6, wherein the modified nanosilica is obtained by modifying nanosilica with a silane coupling agent;
preferably, the average particle size of the nano-silica is 10-100nm, preferably 10-50nm;
preferably, the silane coupling agent is selected from at least one of methylvinyldimethoxysilane, methylvinyldiethoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane, vinyltriisopropoxysilane, γ -methacryloxypropyl methyldimethoxysilane, γ -methacryloxypropyl trimethoxysilane and vinyltris (β -methoxyethoxy) silane;
preferably, the weight ratio of the nano silicon dioxide to the silane coupling agent is 1 (1-2).
8. The method of preparing according to claim 7, wherein the method of modifying comprises: dispersing the nano silicon dioxide in a dispersion medium, and then reacting with the silane coupling agent to obtain the modified nano silicon dioxide;
preferably, the temperature of the reaction is 50-75 ℃ and the time is 4-24 hours;
preferably, the temperature of the reaction is 50-70 ℃ and the time is 6-12h;
preferably, the dispersion medium is a mixture of absolute ethyl alcohol and water, and the volume ratio of the absolute ethyl alcohol to the water is 1 (1-2);
preferably, the weight ratio of the nano-silica to the dispersion medium is (1-5): 100.
9. The preparation method according to any one of claims 1 to 8, characterized in that the preparation method comprises the steps of:
(1) Firstly mixing the lubricating oil core material and the first surfactant to obtain a mixed solution 1;
(2) Dissolving the second surfactant in water to obtain a mixed solution 2;
(3) Performing second mixing on the modified nano silicon dioxide and the first monomer to obtain a mixed solution 3;
(4) Thirdly, mixing the mixed solution 1 with the mixed solution 2, and then fourth mixing with the mixed solution 3 to obtain a mixed solution 4;
(5) And fifthly, mixing the second monomer, the cross-linking agent and the initiator with the mixed solution 4, and carrying out in-situ polymerization reaction to obtain the microcapsule lubricant.
10. A microcapsule lubricant prepared by the preparation method of any one of claims 1 to 9, wherein the microcapsule lubricant has an average particle diameter of 3 to 50 μm and a temperature resistance of 160 ℃ or higher.
11. Use of the microcapsule lubricant of claim 10 in a high temperature drilling environment.
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