CN116064008A - Composite profile control and flooding system, preparation method thereof and deep profile control and flooding method of oil field - Google Patents
Composite profile control and flooding system, preparation method thereof and deep profile control and flooding method of oil field Download PDFInfo
- Publication number
- CN116064008A CN116064008A CN202111284739.6A CN202111284739A CN116064008A CN 116064008 A CN116064008 A CN 116064008A CN 202111284739 A CN202111284739 A CN 202111284739A CN 116064008 A CN116064008 A CN 116064008A
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- Prior art keywords
- alkyl
- profile control
- acrylamide
- solvent
- modified
- 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.)
- Pending
Links
- 238000000034 method Methods 0.000 title claims abstract description 36
- 239000002131 composite material Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title abstract description 44
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 117
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 103
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 80
- 239000002105 nanoparticle Substances 0.000 claims abstract description 77
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 41
- 150000001875 compounds Chemical class 0.000 claims abstract description 38
- 239000003921 oil Substances 0.000 claims abstract description 26
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 22
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 8
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 40
- 239000002904 solvent Substances 0.000 claims description 36
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 24
- 239000000178 monomer Substances 0.000 claims description 23
- 238000006116 polymerization reaction Methods 0.000 claims description 23
- 239000000203 mixture Substances 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 20
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 20
- 238000002156 mixing Methods 0.000 claims description 19
- 239000003607 modifier Substances 0.000 claims description 19
- 229910052757 nitrogen Inorganic materials 0.000 claims description 16
- 239000000126 substance Substances 0.000 claims description 16
- 239000004202 carbamide Substances 0.000 claims description 15
- 239000012966 redox initiator Substances 0.000 claims description 15
- -1 alkyl triethoxysilane Chemical compound 0.000 claims description 14
- 239000002245 particle Substances 0.000 claims description 14
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 12
- 239000008139 complexing agent Substances 0.000 claims description 12
- 239000003999 initiator Substances 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 12
- SCVFZCLFOSHCOH-UHFFFAOYSA-M potassium acetate Chemical compound [K+].CC([O-])=O SCVFZCLFOSHCOH-UHFFFAOYSA-M 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 9
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 8
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 8
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 8
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 8
- 238000000926 separation method Methods 0.000 claims description 8
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 claims description 7
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 claims description 7
- 150000003839 salts Chemical class 0.000 claims description 7
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 6
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 6
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 6
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 6
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 6
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 6
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 claims description 5
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- 229910052700 potassium Inorganic materials 0.000 claims description 5
- 235000011056 potassium acetate Nutrition 0.000 claims description 5
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- PQUCIEFHOVEZAU-UHFFFAOYSA-N Diammonium sulfite Chemical compound [NH4+].[NH4+].[O-]S([O-])=O PQUCIEFHOVEZAU-UHFFFAOYSA-N 0.000 claims description 4
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- 239000005543 nano-size silicon particle Substances 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 4
- 239000003208 petroleum Substances 0.000 claims description 4
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims description 4
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 claims description 3
- 239000005695 Ammonium acetate Substances 0.000 claims description 3
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 3
- 150000001412 amines Chemical class 0.000 claims description 3
- 235000019257 ammonium acetate Nutrition 0.000 claims description 3
- 229940043376 ammonium acetate Drugs 0.000 claims description 3
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 claims description 3
- 239000003129 oil well Substances 0.000 claims description 3
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims description 3
- 229910052939 potassium sulfate Inorganic materials 0.000 claims description 3
- BHZRJJOHZFYXTO-UHFFFAOYSA-L potassium sulfite Chemical compound [K+].[K+].[O-]S([O-])=O BHZRJJOHZFYXTO-UHFFFAOYSA-L 0.000 claims description 3
- 235000011151 potassium sulphates Nutrition 0.000 claims description 3
- 235000019252 potassium sulphite Nutrition 0.000 claims description 3
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 3
- 235000011152 sodium sulphate Nutrition 0.000 claims description 3
- 235000010265 sodium sulphite Nutrition 0.000 claims description 3
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims description 2
- 238000010528 free radical solution polymerization reaction Methods 0.000 claims description 2
- 150000003254 radicals Chemical class 0.000 claims description 2
- DZCAZXAJPZCSCU-UHFFFAOYSA-K sodium nitrilotriacetate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CN(CC([O-])=O)CC([O-])=O DZCAZXAJPZCSCU-UHFFFAOYSA-K 0.000 claims description 2
- 230000000379 polymerizing effect Effects 0.000 claims 1
- 230000014759 maintenance of location Effects 0.000 abstract description 10
- 230000035699 permeability Effects 0.000 abstract description 6
- 238000006073 displacement reaction Methods 0.000 abstract description 2
- 230000008719 thickening Effects 0.000 abstract 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 28
- 239000000243 solution Substances 0.000 description 18
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 13
- 238000001035 drying Methods 0.000 description 13
- 229920000642 polymer Polymers 0.000 description 11
- 229920001577 copolymer Polymers 0.000 description 10
- 230000007062 hydrolysis Effects 0.000 description 9
- 238000006460 hydrolysis reaction Methods 0.000 description 9
- 238000012360 testing method Methods 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 230000033558 biomineral tissue development Effects 0.000 description 8
- 229920000536 2-Acrylamido-2-methylpropane sulfonic acid Polymers 0.000 description 7
- XHZPRMZZQOIPDS-UHFFFAOYSA-N 2-Methyl-2-[(1-oxo-2-propenyl)amino]-1-propanesulfonic acid Chemical compound OS(=O)(=O)CC(C)(C)NC(=O)C=C XHZPRMZZQOIPDS-UHFFFAOYSA-N 0.000 description 7
- 230000032683 aging Effects 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 229910001425 magnesium ion Inorganic materials 0.000 description 6
- 239000012267 brine Substances 0.000 description 5
- ZFXVRMSLJDYJCH-UHFFFAOYSA-N calcium magnesium Chemical compound [Mg].[Ca] ZFXVRMSLJDYJCH-UHFFFAOYSA-N 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 230000002209 hydrophobic effect Effects 0.000 description 5
- GCGQYJSQINRKQL-UHFFFAOYSA-N n-hexylprop-2-enamide Chemical compound CCCCCCNC(=O)C=C GCGQYJSQINRKQL-UHFFFAOYSA-N 0.000 description 5
- 229920002401 polyacrylamide Polymers 0.000 description 5
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 5
- 239000000725 suspension Substances 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 238000011161 development Methods 0.000 description 4
- 230000018109 developmental process Effects 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 4
- 238000000227 grinding Methods 0.000 description 4
- 230000003301 hydrolyzing effect Effects 0.000 description 4
- 239000002954 polymerization reaction product Substances 0.000 description 4
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 229920006322 acrylamide copolymer Polymers 0.000 description 3
- 239000012298 atmosphere Substances 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 3
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 230000001965 increasing effect Effects 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- BKWMQCLROIZNLX-UHFFFAOYSA-N n-hexadecylprop-2-enamide Chemical compound CCCCCCCCCCCCCCCCNC(=O)C=C BKWMQCLROIZNLX-UHFFFAOYSA-N 0.000 description 3
- 125000002347 octyl 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])[H] 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 238000010008 shearing Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000005352 clarification Methods 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 230000001804 emulsifying effect Effects 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 238000004255 ion exchange chromatography Methods 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 239000006249 magnetic particle Substances 0.000 description 2
- 230000005012 migration Effects 0.000 description 2
- 238000013508 migration Methods 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 239000008399 tap water Substances 0.000 description 2
- 235000020679 tap water Nutrition 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 244000078856 Prunus padus Species 0.000 description 1
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 150000007514 bases Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- XGZGKDQVCBHSGI-UHFFFAOYSA-N butyl(triethoxy)silane Chemical compound CCCC[Si](OCC)(OCC)OCC XGZGKDQVCBHSGI-UHFFFAOYSA-N 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000006266 etherification reaction Methods 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N ferric oxide Chemical compound O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 230000005669 field effect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 125000001165 hydrophobic group Chemical group 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- YRVUCYWJQFRCOB-UHFFFAOYSA-N n-butylprop-2-enamide Chemical group CCCCNC(=O)C=C YRVUCYWJQFRCOB-UHFFFAOYSA-N 0.000 description 1
- 125000001280 n-hexyl group Chemical group C(CCCCC)* 0.000 description 1
- CNWVYEGPPMQTKA-UHFFFAOYSA-N n-octadecylprop-2-enamide Chemical group CCCCCCCCCCCCCCCCCCNC(=O)C=C CNWVYEGPPMQTKA-UHFFFAOYSA-N 0.000 description 1
- BPCNEKWROYSOLT-UHFFFAOYSA-N n-phenylprop-2-enamide Chemical compound C=CC(=O)NC1=CC=CC=C1 BPCNEKWROYSOLT-UHFFFAOYSA-N 0.000 description 1
- 125000004123 n-propyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 230000005311 nuclear magnetism Effects 0.000 description 1
- MSRJTTSHWYDFIU-UHFFFAOYSA-N octyltriethoxysilane Chemical compound CCCCCCCC[Si](OCC)(OCC)OCC MSRJTTSHWYDFIU-UHFFFAOYSA-N 0.000 description 1
- 229960003493 octyltriethoxysilane Drugs 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 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 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- DJEHXEMURTVAOE-UHFFFAOYSA-M potassium bisulfite Chemical compound [K+].OS([O-])=O DJEHXEMURTVAOE-UHFFFAOYSA-M 0.000 description 1
- 229940099427 potassium bisulfite Drugs 0.000 description 1
- 235000010259 potassium hydrogen sulphite Nutrition 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000001632 sodium acetate Substances 0.000 description 1
- 235000017281 sodium acetate Nutrition 0.000 description 1
- 229940079827 sodium hydrogen sulfite Drugs 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000005063 solubilization Methods 0.000 description 1
- 230000007928 solubilization Effects 0.000 description 1
- 238000011895 specific detection Methods 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- OYGYKEULCAINCL-UHFFFAOYSA-N triethoxy(hexadecyl)silane Chemical compound CCCCCCCCCCCCCCCC[Si](OCC)(OCC)OCC OYGYKEULCAINCL-UHFFFAOYSA-N 0.000 description 1
- 238000011179 visual inspection Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
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- 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
- C09K8/50—Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls
- C09K8/504—Compositions based on water or polar solvents
- C09K8/506—Compositions based on water or polar solvents containing organic compounds
- C09K8/508—Compositions based on water or polar solvents containing organic compounds macromolecular compounds
-
- 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
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/56—Acrylamide; Methacrylamide
-
- 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
- C09K8/50—Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls
- C09K8/504—Compositions based on water or polar solvents
- C09K8/5045—Compositions based on water or polar solvents containing inorganic compounds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/58—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/58—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids
- C09K8/588—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids characterised by the use of specific polymers
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- 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
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/84—Compositions based on water or polar solvents
- C09K8/845—Compositions based on water or polar solvents containing inorganic compounds
-
- C—CHEMISTRY; METALLURGY
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Abstract
The invention relates to the field of oil displacement agents, and discloses a compound profile control system, a preparation method thereof and a deep profile control method of an oil field. The composite provided by the invention contains the acrylamide multipolymer and the silicon dioxide nano particles with the surfaces modified by the alkyl, has good stability, water solubility, water phase tackifying and viscosity retention rate, thereby playing a role in multiple functions of strong thickening and high-temperature high-shear tackifying, being particularly suitable for deep profile control and flooding of oil reservoirs with medium and high permeability and having good application significance.
Description
Technical Field
The invention relates to the field of oil displacement agents, in particular to a compound profile control system, a preparation method thereof and a deep profile control method of an oil field.
Background
The eastern old oil field of China integrally enters the 'two-special-one-high' development stage of ultra-high water content, ultra-high recoverable reserve production degree and high cost development at present. In combination with the current low-oil-price situation and the complicated oil reservoir heterogeneous conditions of the old oil field, the traditional technology for efficiently improving the recovery ratio faces serious challenges, so that the development difficulty of the benefit of the oil field is increased. For example, the middle layer system well pattern in the old oil field is generally adjusted, and the large-scale adjustment space is not large under the condition of low oil price. For another example, the low-cost separate-layer water injection technology has great difficulty in controlling contradiction between the in-layer and the plane, and can not meet the requirements of improving the recovery ratio and improving the economic efficiency in the 'two-special-one-high' development stage of the old oil field.
The deep profile control technology has the characteristic of controllable deep migration and plugging, and is one of the most important methods for improving the heterogeneity of the medium-high permeability oil reservoir. However, the existing profile control system has insufficient viscosity increasing effect of injection phase, and the aging and shear viscosity retention rate in the deep migration process of the oil reservoir is low, so that the differential control requirements of different levels of water flooding bands cannot be met, and the overall deep profile control mining field effect is difficult to realize. Therefore, a novel compound efficient profile control system is designed and developed according to the characteristics of the prior medium-high permeability reservoir, so that the requirements of plugging, increasing resistance and displacing oil of the medium-high permeability reservoir are met, deep liquid flow steering of a water consumption belt is realized, the water injection wave efficiency is improved, and the quality improvement and synergy effects of old oil field exploitation are achieved.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and provide a compound profile control and flooding system, a preparation method thereof and a deep profile control and flooding method of an oil field.
In order to achieve the above object, in one aspect, the present invention provides a composite having a profile control function, the composite comprising an acrylamide multipolymer and silica nanoparticles having surfaces modified with alkyl groups.
In a second aspect, the invention provides a composite profile control system comprising a composite as described above and a second solvent.
The third aspect of the invention provides a method for preparing a compound profile control system, comprising the following steps:
and in the presence of a second solvent, carrying out second mixing on the silicon dioxide nano particles with the surfaces modified by alkyl groups and the acrylamide multipolymer to obtain the composite profile control and flooding system.
The fourth aspect of the invention provides a method for deep profile control of an oil field, the method comprising applying a profile control agent to an oil well in an oil field well group, wherein the profile control agent is a compound profile control system as described above or a compound profile control system prepared by the method as described above.
Through the technical scheme, the invention has the following beneficial effects:
(1) The compound profile control system provided by the invention has better temperature resistance and salt resistance, and can meet the requirements of deep profile control of a medium-high permeability reservoir;
(2) The compound profile control system provided by the invention has good water solubility, better water phase tackifying effect and filterability, higher aging and shear viscosity retention rate and good stability, and is suitable for industrial production and application;
(3) The preparation method of the compound profile control system provided by the invention is simple, raw materials are easy to obtain, and the compound profile control system is suitable for large-scale production and application.
(4) The compound profile control system provided by the invention can be used by mixing the solvent (water) with the active components (the multipolymer and the nano particles, namely the compound with the profile control function provided by the invention) before use, namely, the compound can be transported to a required exploitation site and then prepared into the compound profile control system on site for use, so that the compound profile control system provided by the invention is more convenient to transport, store and use.
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.
In the present invention, "first" and "second" in "first solvent", "second solvent", "first mixture" and "second mixture" are used only for descriptive convenience to distinguish between solvents and mixing operations in different steps.
The inventor of the invention skillfully discovers that a mixture obtained by compounding certain acrylamide multipolymer and nano particles with the surfaces modified by alkyl (such as silicon dioxide nano particles with the surfaces modified by alkyl) has better profile control function, particularly has better temperature resistance, salt resistance and water phase tackifying property, and also has higher aging and shear viscosity retention rate, thus being very suitable for deep profile control.
In one aspect, the invention provides a composite with a profile control function, which contains an acrylamide multipolymer and silicon dioxide nano particles with surfaces modified by alkyl groups. The acrylamide multipolymer and the silicon dioxide nanometer particles with the surfaces modified by alkyl interact through hydrophobic association.
According to a preferred embodiment of the present invention, wherein the acrylamide multipolymer contains a first structural unit R provided by acrylamide 1 A second structural unit R provided by a substance of formula I 2 And providing a third structural unit R from a substance of formula II 3 。
In the formula I, M 1 H, K or Na.
In formula II, X is O or NH, preferably NH; r is selected from C 1-18 Alkyl and/or phenyl, preferably C 6-16 Alkyl and/or phenyl.
In order to further increase the adhesion promoting effect of the complex, preferably, in formula II, R is selected from C 6-16 An alkyl group.
According to a preferred embodiment of the invention, wherein the first structural unit R 1 Comprising a structural unit shown in a formula III and a structural unit shown in a formula IV. Specifically, after polymerization of the monomer mixture, the acrylamide multipolymer obtained by polymerization is contacted with an inorganic basic compound under conventional hydrolysis conditions well known to those skilled in the art, the hydrolysis conditions being such that the acrylamide structural units in the multipolymer are partially hydrolyzed to structural units having formula IV.
Wherein M is 2 Preferably Na or K.
According to a preferred embodiment of the present invention, wherein the first structural unit R is based on 100 parts by weight of the acrylamide multipolymer 1 The content of the second structural unit R is 80-96 parts by weight 2 The content of the third structural unit R is 2-10 parts by weight 3 The content of (2-10 parts by weight).
Preferably, in the acrylamide multipolymer, the second structural unit R 2 And a third structural unit R 3 The weight ratio of (2) is 1:4-4:1.
according to a preferred embodiment of the present invention, wherein the viscosity average molecular weight of the acrylamide multipolymer is 1000 to 2000 tens of thousands, more preferably 1000 to 1500 tens of thousands. In particular, the multipolymer is preferably a random multipolymer.
According to a preferred embodiment of the present invention, wherein the molar ratio of silica to alkyl groups in the surface-modified nanoparticle is 1:0.3-0.8.
According to a preferred embodiment of the present invention, in the nanoparticle whose surface is modified with an alkyl group, the substance providing the alkyl group is an alkyl trialkoxysilane.
Preferably, the substance providing the alkyl group is alkyl triethoxysilane and/or alkyl trimethoxysilane. Preferably wherein alkyl is C 1-18 More preferably C 6-14 Normal alkyl of (a). For example, C 1-18 The n-alkyl group may be methyl, ethyl, n-propyl, n-butyl, isobutyl, n-hexyl, n-octyl or even n-octadecyl.
According to a preferred embodiment of the present invention, wherein the number average particle diameter of the surface-alkyl-modified silica nanoparticle is 20 to 200nm.
According to a preferred embodiment of the present invention, wherein the surface-alkyl-modified silica nanoparticle is prepared by the following method:
In a first solvent, firstly mixing the silicon dioxide nano-particles with an alkyl modifier, and then carrying out solid-liquid separation to obtain the silicon dioxide nano-particles with the surfaces modified by alkyl. The alkyl modifier is covalently linked to the silica nanoparticle.
Preferably, the silica nanoparticles have a number average particle diameter of 20-90nm.
Preferably, the first mixing is performed under first stirring conditions, the first stirring speed being 250-720 revolutions per minute.
Preferably, the temperature of the first mixing is 20-80 ℃ and the time is 10-14h.
Preferably, the first solvent is used in an amount of 70-100mL based on 1g of the silica nanoparticle.
Preferably, the first solvent is an organic solvent. Preferably at least one of cyclohexane, n-hexane and petroleum ether.
Preferably, the alkyl modifier is used in an amount of preferably 1 to 10g, more preferably 1.8 to 6g, based on 1g of the nano silica particles.
Preferably, the alkyl modifier is an alkyl trialkoxysilane.
More preferably, the alkyl modifier is alkyl triethoxysilane and/or alkyl trimethoxysilane. Preferably wherein alkyl is C 1-18 More preferably C 6-14 Normal alkyl of (a).
In the present invention, in order to accelerate the dispersion of the nano silica particles, the nano silica particles may be dispersed in a first solvent such as cyclohexane or the like in an ultrasonic condition, and the ultrasonic frequency is preferably 20 to 40kHz.
In the present invention, the mode of solid-liquid separation is not limited, and any mode of solid-liquid separation existing in the art may be used. For example, solid-liquid separation may be achieved by centrifugation.
Preferably, the rotational speed of the centrifugation is 2000-3000 rpm and the time is 20-50 minutes.
In the invention, the method further comprises the following steps: the solid obtained after the solid-liquid separation is washed and dried, and the washing liquid used for washing is preferably at least one of ethanol, methanol and acetone. Preferably 2-5 washes.
In the present invention, the drying may be performed by a method conventional in the art, preferably, the drying is performed in a drying apparatus, and the drying conditions may preferably include a drying temperature of preferably 60 to 80 ℃. The drying time is preferably 22 to 26 hours.
In the present invention, the first mixing is preferably performed under weakly alkaline conditions, preferably at a pH of 7-9. Specifically, the pH of the first mixed system may be adjusted to 7 to 9 by a method known to those skilled in the art, for example, ammonia may be added to the first mixed system to adjust the pH of the first mixed system to 7 to 9.
According to a preferred embodiment of the present invention, wherein the weight ratio of the surface-modified silica nanoparticles to the acrylamide multipolymer in the composite is 1:5-20. Preferably 1:10-15.
In a second aspect, the invention provides a complex flooding system comprising a complex as described above and a second solvent. The compound profile control system has a good profile control function, and is particularly suitable for deep profile control driving.
Preferably, the concentration of the compound in the compound profile control system is 1200-5000ppm. That is, the total concentration of the surface-modified silica nanoparticles and the acrylamide multipolymer is 1200 to 5000ppm.
Preferably, the second solvent is water. The "water" may be pure water (e.g., tap water, distilled water, deionized water, etc.), or may be an aqueous solution. For example, it may be an aqueous salt solution. For convenience of use on site, water having a certain degree of mineralization (e.g., field water such as victory type II brine) may be used as the second solvent.
More preferably, the second solvent is water with mineralization degree of 10000-20000mg/L and calcium-magnesium ion content of 300-800mg/L at 65-85 ℃. Degree of mineralization "means the total mass of each salt in 1L of saline, as measured by ion chromatography. "Ca/Mg ion content" means 1L of Ca in the brine 2+ And Mg (magnesium) 2+ The mass content of (2) can be stoichiometrically calculated according to the formula during preparation, or can be confirmed by measuring by an ion chromatography method.
In a third aspect, the present invention provides a method of preparing a compound flooding system (as described above), the method comprising:
and in the presence of a second solvent, carrying out second mixing on the silicon dioxide nano particles with the surfaces modified by alkyl groups and the acrylamide multipolymer to obtain the composite profile control and flooding system.
According to a preferred embodiment of the present invention, wherein the surface-alkyl-modified silica nanoparticles are dispersed in the second solvent, and emulsified and sonicated, a mixture a containing the surface-alkyl-modified silica nanoparticles is obtained. And dissolving the acrylamide multipolymer in the mixed solution A under the stirring condition, and standing to obtain the composite profile control system (for deep profile control). In particular, the second solvent is preferably water. In consideration of the site conditions of the oil reservoir, site water (such as victory type II brine meeting the aforementioned conditions) with the mineralization degree of 10000-20000mg/L and the calcium-magnesium ion content of 300-800mg/L is selected as the second solvent. The emulsifying time is 10-20 minutes. The ultrasonic frequency is 25-40kHz and the ultrasonic time is 0.5-1.5h. The dissolution of the acrylamide multipolymer is performed under stirring. The acrylamide multipolymer is contacted with the mixed solution A preferably under stirring conditions of 200-300 revolutions per minute for 25-40 seconds. Then stirring for 1.5-3h at the temperature of 20-40 ℃ and 500-700 rpm. And then continuing stirring for a period of time to obtain the compound profile control system (for deep profile control). Preferably, the stirring is continued for 6-12h at 20-40deg.C without special adjustment of pH.
According to a preferred embodiment of the present invention, wherein the method further comprises the step of preparing an acrylamide multipolymer: the monomer mixture is polymerized in water under free radical aqueous solution polymerization conditions in the presence of an initiator.
Preferably, the monomer mixture contains acrylamide, a substance represented by formula I and a substance represented by formula II.
Wherein in formula I, M 1 H, K or Na.
In formula II, X is O or NH, preferably NH. R is selected from C 1-18 Alkyl and/or phenyl, preferably C 6-16 Alkyl and/or phenyl, more preferably C 6-16 An alkyl group.
According to a preferred embodiment of the present invention, the acrylamide is contained in an amount of 80 to 96 parts by weight, the substance represented by formula I is contained in an amount of 2 to 10 parts by weight, and the substance represented by formula II is contained in an amount of 2 to 10 parts by weight based on 100 parts by weight of the monomer mixture.
According to a preferred embodiment of the invention, the initiator is selected from azo-based initiators and/or redox-based initiators. More preferably a redox initiator.
Preferably, the redox initiator is selected from at least one of sulfate and sulfite redox initiators, persulfate and thiourea redox initiators, persulfate and organic salt redox initiators, persulfate and sulfite redox initiators, and ammonium persulfate and fatty amine redox initiators.
More preferably, the sulfate is selected from at least one of sodium sulfate, potassium sulfate and ammonium sulfate.
More preferably, the sulfite is selected from at least one of sodium sulfite, potassium sulfite, sodium bisulfite, potassium bisulfite, and ammonium sulfite.
More preferably, the persulfate is selected from at least one of sodium persulfate, potassium persulfate, and ammonium persulfate.
More preferably, the organic salt is selected from at least one of thiourea, sodium acetate and potassium acetate.
More preferably, the fatty amine is selected from at least one of ammonium acetate, N-tetramethyl ethylenediamine and diethylamine.
Further preferably, the redox initiator is selected from at least one of sodium sulfate and sodium sulfite, potassium sulfate and potassium sulfite, ammonium sulfate and sodium bisulfite, ammonium sulfate and ammonium sulfite, sodium persulfate and thiourea, potassium persulfate and thiourea, ammonium persulfate and thiourea, sodium persulfate and potassium acetate, potassium persulfate and potassium acetate, ammonium persulfate and ammonium acetate, ammonium persulfate and N, N-tetramethyl ethylenediamine, and ammonium persulfate and diethylamine.
In the present invention, the amount of the initiator is not particularly limited. According to a preferred embodiment of the invention, the initiator is used in an amount of 0.0022 to 0.0035g, based on 50g of the monomer mixture.
According to a preferred embodiment of the invention, the polymerization is carried out in the presence of a complexing agent and urea.
Preferably, the complexing agent is selected from at least one of disodium edetate, sodium nitrilotriacetate, and diethylenetriamine pentacarboxylate. Disodium edetate is preferred.
Preferably urea is used in an amount of 0.01 to 0.1 wt.%, based on the total weight of the monomer mixture.
Preferably, the weight ratio of the urea to the complexing agent is 1-10:1. Specifically, the complexing agent and urea are used for complexing metal ions, improving the conversion rate of the polymerized monomer and performing solubilization. Generally, the complexing agent and urea are used in the form of aqueous solutions thereof, wherein the aqueous complexing agent is preferably 1-3% by weight aqueous complexing agent, and the aqueous urea is preferably 1-3% by weight aqueous urea.
According to a preferred embodiment of the present invention, wherein the polymerization conditions include: the temperature is-10 ℃ to 80 ℃, the time is 2-30 hours, and the pH value is 5-10.
Preferably, the polymerization conditions include: the temperature is 5-60 ℃, the time is 8-20 hours, and the pH value is 6-10.
According to a preferred embodiment of the present invention, wherein the method further comprises the step of preparing the surface-alkyl-modified silica nanoparticle:
In a first solvent, firstly mixing nano silicon dioxide particles with an alkyl modifier, and then carrying out solid-liquid separation to obtain the silicon dioxide nano particles with the surfaces modified by alkyl.
Preferably, the first mixing is performed under first stirring conditions, the first stirring speed being 250-720 revolutions per minute.
Preferably, the temperature of the first mixing is 20-80 ℃ and the time is 10-14h.
In the invention, the alkyl modifier is used in an amount such that the molar ratio of silica to alkyl in the prepared nano-particles with the surfaces modified by alkyl is 1:0.3-0.8. In the present invention, it is considered that the etherification reaction occurring between the alkyl modifier and the nanoparticles is completely reacted, and thus, the molar ratio can be estimated by the feed ratio. Preferably, the alkyl modifier is used in an amount of 1 to 10g, more preferably 1.2 to 5g, based on 1g of the nano silica particles. As previously mentioned, the silica nanoparticles preferably have a number average particle diameter of 20 to 200nm.
Preferably, the first solvent is used in an amount of 70-100mL based on 1g of the nano-silica particles.
Preferably, the first solvent is an organic solvent. Preferably at least one of cyclohexane, n-hexane and petroleum ether.
Preferably, the alkyl modifier is an alkyl trialkoxysilane.
More preferably, the alkyl modifier is alkyl triethoxysilane and/or alkyl trimethoxysilane. Preferably wherein alkyl is C 1-18 More preferably C 6-14 Normal alkyl of (a).
According to a preferred embodiment of the present invention, wherein the amount of the surface-alkyl-modified silica nanoparticles and the acrylamide multipolymer is such that the weight ratio of the surface-alkyl-modified silica nanoparticles to the acrylamide multipolymer is 1:5-20, preferably 1:10-15.
Preferably, the amount of the surface-modified silica nanoparticles and the acrylamide multipolymer is such that the total concentration of the surface-modified silica nanoparticles and the acrylamide multipolymer in the composite profile control system is 1200-5000ppm.
Preferably, the second solvent is water. The "water" may be pure water (e.g., tap water, distilled water, deionized water, etc.), or may be an aqueous solution. For example, it may be an aqueous salt solution. For convenience of use on site, water having a certain degree of mineralization (e.g., field water such as victory type II brine) may be used as the second solvent.
More preferably, water having a mineralization of 10000-20000mg/L and a calcium-magnesium ion content of 300-800mg/L is selected as the second solvent in consideration of the reservoir site conditions.
According to a preferred embodiment of the invention, the polymerization is carried out in the presence of a complexing agent and urea, and the manner and conditions of the polymerization are as follows: dissolving the monomer mixture in a solvent, regulating the pH value of the solution of the obtained monomer mixture to 6-10, adding complexing agent and urea, introducing nitrogen into a reaction system at 5-15 ℃ for 10-30 minutes, adding an initiator, introducing nitrogen for 5-30 minutes until the reaction solution starts to become sticky, stopping introducing nitrogen, carrying out adiabatic polymerization for 4-10 hours, and after the polymerization reaction is finished, cutting, granulating, hydrolyzing, drying and powdering to obtain the acrylamide multipolymer.
The inventors of the present invention have unexpectedly found that the polymer obtained by using the above polymerization method and polymerization conditions has more excellent properties. In particular, in order to overcome oxygen inhibition, polymers with a relatively large molecular weight are obtained, preferably the polymerization is carried out in an inert atmosphere. The inert gas used for maintaining the inert atmosphere may be any of various conventional gases or gas mixtures which do not react with the raw materials and the products, and may be, for example, nitrogen or at least one of gases of the group zero elements of the periodic table, and from the viewpoint of economy, the inert atmosphere is preferably provided by nitrogen. In the invention, hydrolysis refers to the use of stoichiometric (degree of hydrolysis related) concentration of 35-40 wt% NaOH solution, evenly spraying on the particle size of 2-4mm acrylamide polymer colloidal particles, after even dispersion, placing in a water bath at 60-90 ℃, heating for 2-8h, wherein the hydrolysis step is a conventional step for preparing acrylamide polymer, and will not be repeated here.
In the invention, the content of each structural unit in the copolymer can be tested by adopting a conventional method in the prior art, such as infrared spectrum, nuclear magnetism, the feeding amount of monomers in the polymerization process and the like.
In the invention, the monomer feeding amount is adopted to determine the content of each structural unit in the polymer, specifically, the feeding ratio of each monomer actually participating in polymerization is determined by testing the content of unreacted monomers, and then the content of each structural unit in the polymer is determined.
Further, in the present invention, the content of each unreacted (residual) monomer in the polymerization reaction product was 0.02% by weight or less, indicating that substantially all the monomer was involved in the polymerization reaction. Specifically, the content of the residual monomer is determined by liquid chromatography.
The composite profile control system prepared by the method also belongs to the content of the invention.
The fourth aspect of the invention provides a method for deep profile control of an oil field, the method comprising applying a profile control agent to an oil well in an oil field well group, wherein the profile control agent is a compound profile control system as described above or a compound profile control system prepared by the method as described above. The compound profile control system can meet the requirements of deep profile control of a medium-high permeability reservoir.
The present invention will be described in detail by examples. It should be understood that the following examples are illustrative only and are not intended to limit the invention.
In the examples below, all reagents used were commercially available analytical pure reagents. Room temperature refers to 25 ℃. The degree of hydrolysis refers to mole percent. The nano silicon dioxide particles are purchased from Shanghai Michlin Biochemical technology Co., ltd, and the particle size is 20-90nm. The formulation water (i.e., the second solvent of the foregoing) was a type II victory saline with a degree of mineralization of about 19334mg/L and a calcium magnesium ion content of about 514 mg/L. The partially hydrolyzed polyacrylamide was purchased from elsen, france under the trade name 1630s, with a degree of hydrolysis of 33% and a viscosity average molecular weight of 1300 ten thousand. Nanometer ferric oxide magnetic particles are purchased from the company of Enoki, and the particle size is 20-80nm. The alkyltriethoxysilanes used in the examples were all available from enokava, both having a purity of >95% and a density of about 0.996g/mL.
Preparation example 1
This preparation example is used to illustrate the preparation of an acrylamide multipolymer.
In this preparation example, the hydrolysis steps are: adding stoichiometric 40 wt% sodium hydroxide solution (33% in terms of hydrolysis degree), spraying onto 2-4mm diameter colloidal particles, mixing, and heating in 70deg.C water bath for 6 hr.
(one) acrylamide Multi-copolymer P1
45g of acrylamide, 2.5g of 2-acrylamido-2-methylpropanesulfonic acid and 2.5g of N-hexylacrylamide were dissolved in 300g of deionized water and the pH was adjusted to 7 with sodium hydroxide. Then, 0.8g of an aqueous solution (1 wt%) of disodium ethylenediamine tetraacetate and 0.8g of an aqueous urea solution (1 wt%) were added and mixed uniformly. The mixture was cooled to 5℃and then charged into a vessel, nitrogen was introduced for 30 minutes, after which 0.8g of an aqueous ammonium persulfate solution (1 wt%) and 1.6g of an aqueous sodium hydrogensulfite solution (1 wt%) were added, and then nitrogen was introduced for another 10 minutes until the reaction solution began to thicken. The nitrogen drum was then stopped and the polymerization was adiabatic for 8h. The residual monomer content in the polymerization reaction product is below 0.02 wt%. After the polymerization reaction is finished, shearing, granulating, hydrolyzing, drying and powdering are carried out to obtain the acrylamide multipolymer P1, wherein the viscosity average molecular weight of the acrylamide multipolymer P1 is about 1410 ten thousand (refer to GB 17514-2008 standard detection and the same applies).
(di) acrylamide Multi-copolymer P2
45g of acrylamide, 2.5g of 2-acrylamido-2-methylpropanesulfonic acid and 2.5g of N-hexadecylacrylamide were dissolved in 300g of deionized water and the pH was adjusted to 10 with sodium hydroxide. Then, 0.3g of an aqueous solution (3 wt%) of disodium ethylenediamine tetraacetate and 0.3g of an aqueous urea solution (3 wt%) were added and mixed uniformly. The mixture was cooled to 15℃and then charged into a vessel, nitrogen was introduced for 10 minutes, after which 1.8g of an aqueous sodium persulfate solution (1 wt%) and 1.7g of an aqueous thiourea solution (1 wt%) were added, followed by further introduction of nitrogen for 30 minutes until the reaction solution began to thicken. The nitrogen drum was then stopped and the polymerization was adiabatic for 10h. The residual monomer content in the polymerization reaction product is below 0.02 wt%. After the polymerization reaction is finished, shearing, granulating, hydrolyzing, drying and powdering are carried out to obtain the acrylamide multipolymer P2, wherein the viscosity average molecular weight of the multipolymer P2 is about 1210 ten thousand.
(III) acrylamide Multi-copolymer P3
45g of acrylamide, 2.5g of 2-acrylamido-2-methylpropanesulfonic acid and 2.5g of N-phenylacrylamide were dissolved in 300g of deionized water and the pH was adjusted to 5 with sodium hydroxide. Then, 0.5g of an aqueous solution (1 wt%) of disodium ethylenediamine tetraacetate and 0.5g of an aqueous urea solution (1 wt%) were added and mixed uniformly. The mixture was cooled to 10℃and then charged into a vessel, nitrogen was introduced for 20 minutes, after which 1.1g of an aqueous ammonium sulfate solution (1 wt%) and 1.1g of an aqueous ammonium sulfite solution (1 wt%) were added, followed by further introduction of nitrogen for 20 minutes until the reaction solution began to become viscous. The nitrogen drum was then stopped and the polymerization was adiabatic for 4h. The residual monomer content in the polymerization reaction product is below 0.02 wt%. After the polymerization reaction is finished, shearing, granulating, hydrolyzing, drying and powdering are carried out to obtain the acrylamide multipolymer P3, wherein the viscosity average molecular weight of the multipolymer P is about 1610 ten thousand.
(IV) acrylamide Multi-copolymer P4
The process for preparing acrylamide multipolymer P1 was followed, except that N-hexyl acrylamide was replaced with N-N-butyl acrylamide, to obtain acrylamide multipolymer P4 having a viscosity average molecular weight of about 1390 ten thousand.
(fifth) acrylamide Multi-copolymer P5
The process for preparing acrylamide multipolymer P1 was followed, except that N-hexyl acrylamide was replaced with N-octadecyl acrylamide, to obtain acrylamide multipolymer P5 having a viscosity average molecular weight of about 995 ten thousand.
(sixth) acrylamide Multi-copolymer P6
The method for producing the acrylamide multipolymer P1 was conducted except that 40g of acrylamide, 5g of 2-acrylamido-2-methylpropanesulfonic acid and 5g of N-hexadecylacrylamide were added to obtain an acrylamide multipolymer P6 having a viscosity average molecular weight of about 1190 ten thousand.
(seventh) acrylamide Multi-copolymer P7
The method for producing the acrylamide multipolymer P1 was conducted except that 47.5g of acrylamide, 1.25g of 2-acrylamido-2-methylpropanesulfonic acid and 1.25g of N-hexadecylacrylamide were added to obtain an acrylamide multipolymer P7 having a viscosity average molecular weight of about 1820 ten thousand.
(eight) acrylamide Multi-copolymer P8
The process for preparing acrylamide multipolymer P1 was followed, except that 45g of acrylamide, 1g of 2-acrylamido-2-methylpropanesulfonic acid and 4g of N-hexylacrylamide were added, to obtain acrylamide multipolymer P6 having a viscosity average molecular weight of about 1490 Wan.
(nine) acrylamide Multi-copolymer P9
The process for preparing acrylamide multipolymer P1 was followed, except that 45g of acrylamide, 4g of 2-acrylamido-2-methylpropanesulfonic acid and 1g of N-hexylacrylamide were added, to obtain acrylamide multipolymer P6 having a viscosity average molecular weight of about 1200 ten thousand.
Preparation example 2
This preparation example is used to illustrate the preparation of silica nanoparticles with alkyl modified surfaces.
Silicon dioxide nano particle N1 with surface modified by alkyl
1g of the nano-silica particles were dispersed in 80mL of cyclohexane and stably dispersed by ultrasonic (40 kHz) for 1 hour. 3.12mL of octyltriethoxysilane are added and stirred at 25℃for 12 hours (stirring speed 480 rpm). Centrifuging at 2500 rpm for 30 min, washing the obtained precipitate with ethanol for 3 times, and drying at 70deg.C for 24 hr to obtain silica nanoparticle N1 with octyl-modified surface.
(II) surface-alkyl-modified silica nanoparticle N2
1g of the nano-silica particles were dispersed in 100mL of cyclohexane and stably dispersed by ultrasonic (30 kHz) for 1 hour. 2.09mL of butyltriethoxysilane was added and stirred at 25℃for 10 hours (stirring speed 250 rpm). Centrifuging at 2000 rpm for 50 minutes, washing the obtained precipitate with ethanol for 2 times, and drying at 60 ℃ for 26 hours in an oven to obtain the silica nanoparticle N2 with the surface modified by butyl.
(III) surface-alkyl-modified silica nanoparticle N3
1g of the nano-silica particles were dispersed in 70mL of cyclohexane and stably dispersed by ultrasonic (20 kHz) for 1 hour. 3.65mL of hexadecyltriethoxysilane was added and stirred at 25℃for 14 hours (stirring speed 720 rpm). Centrifugation at 3000 rpm for 20 minutes, washing the obtained precipitate with ethanol 5 times, and drying in an oven at 80 ℃ for 22 hours to obtain the silica nanoparticle N3 with the surface modified by hexadecyl.
Example 1
(1) The surface octyl-modified silica nanoparticle N1 obtained in preparation example 2 was weighed, slowly dispersed in formulation water, rapidly emulsified for 15min with an emulsifying machine, and then sonicated for 1 hour (30 kHz) with an ultrasonic cleaner to obtain nanoparticle dispersion.
(2) Filling the nanoparticle dispersion liquid obtained in the step (1) into a beaker, weighing the acrylamide multipolymer P1 obtained in the preparation example 1, starting a constant-speed stirrer, slowly adding the polymer P1 along a vortex wall 30s at a rotating speed of 300 revolutions per minute, then adjusting the stirring speed to 500 revolutions per minute, and stirring for 2 hours to obtain a mixed suspension of the nanoparticles and the acrylamide multipolymer. Wherein the content of the silica nano-particles N1 with the surface modified by octyl groups is 150ppm, the content of the acrylamide multipolymer P1 is 1800ppm, and the balance is the prepared aqueous solution. And then stirring for 8 hours at 25 ℃ and the rotating speed of 400 revolutions per minute, so that the nano silicon dioxide particles in the suspension are uniformly mixed with the multipolymer and fully act.
(3) And standing the suspension for 24 hours at the temperature of 25 ℃ without obvious precipitation and layering phenomena, thus obtaining the composite profile control system.
Example 2
Preparation of a complex flooding system was carried out in the same manner as in example 1, except that the acrylamide multipolymer P2 obtained in preparation example 1 was used instead of the acrylamide multipolymer P1.
Example 3
Preparation of a complex flooding system was carried out in the same manner as in example 1, except that the acrylamide multipolymer P3 obtained in preparation example 1 was used instead of the acrylamide multipolymer P1.
Example 4
Preparation of a complex flooding system was carried out in the same manner as in example 1, except that the acrylamide multipolymer P4 obtained in preparation example 1 was used instead of the acrylamide multipolymer P1.
Example 5
Preparation of a complex flooding system was carried out in the same manner as in example 1, except that the acrylamide multipolymer P5 obtained in preparation example 1 was used instead of the acrylamide multipolymer P1.
Example 6
The preparation of the complex profile control system was performed in the same manner as in example 1, except that the silica nanoparticle N2 having the butyl-modified surface obtained in preparation example 2 was used instead of the silica nanoparticle N1 having the octyl-modified surface.
Example 7
The preparation of the complex profile control system was performed in the same manner as in example 1, except that the silica nanoparticle N3 having the butyl-modified surface obtained in preparation example 2 was used instead of the silica nanoparticle N1 having the octyl-modified surface.
Example 8
Preparation of a complex flooding system was carried out in the same manner as in example 1, except that the acrylamide multipolymer P1 was replaced with the acrylamide multipolymer P6 obtained in preparation example 1.
Example 9
Preparation of a complex flooding system was carried out in the same manner as in example 1, except that the acrylamide multipolymer P7 obtained in preparation example 1 was used instead of the acrylamide multipolymer P1.
Example 10
The preparation of the complex flooding system was carried out in the same manner as in example 1, except that the amounts of the nanoparticles N1 and the acrylamide multipolymer P1 were adjusted so that the concentration of the silica nanoparticles N1 with the surface modified with octyl groups was 90ppm and the concentration of the acrylamide multipolymer P1 was 1800ppm in the complex flooding system.
Example 11
The preparation of the complex flooding system was carried out in the same manner as in example 1, except that the amounts of the nanoparticles N1 and the acrylamide multipolymer P1 were adjusted so that the concentration of the silica nanoparticles N1 with the surface modified with octyl groups was 360ppm and the concentration of the acrylamide multipolymer P1 was 1800ppm in the complex flooding system.
Example 12
Preparation of a complex flooding system was carried out in the same manner as in example 1, except that the acrylamide multipolymer P8 obtained in preparation example 1 was used instead of the acrylamide multipolymer P1.
Example 13
Preparation of a complex flooding system was carried out in the same manner as in example 1, except that the acrylamide multipolymer P9 obtained in preparation example 1 was used instead of the acrylamide multipolymer P1.
Comparative example 1
The preparation of the complex flooding system was carried out in the same manner as in example 1, except that partially hydrolyzed polyacrylamide (trade name 1630 s) was used instead of acrylamide multipolymer P1.
Comparative example 2
The preparation of the complex profile control system was performed as in example 1, except that the silica nanoparticle N1 with the surface modified with an alkyl group was replaced with a surface unmodified silica nanoparticle.
Comparative example 3
The preparation of the complex profile control system was performed as in example 1, except that the alkyl-modified silica nanoparticle N1 was not added.
Comparative example 4
The preparation of the complex flooding system was carried out in the same manner as in example 1, except that the acrylamide multipolymer P1 was not added.
Comparative example 5
The preparation of the composite profile control system was performed as in example 1, except that nano-iron oxide magnetic particles were used instead of the alkyl-modified silica nanoparticles N1.
Test example 1
The apparent viscosity of the acrylamide multipolymer obtained in preparation example 1 was tested. The specific test method comprises the following steps: the acrylamide multipolymer to be tested is added into victory type II formulated brine with the mineralization degree of about 20000mg/L and the calcium-magnesium ion content of about 300mg/L at the temperature of 70 ℃ to prepare a polymer suspension with the concentration of 1800ppm, and the apparent viscosity of the suspension is measured by a Brookfield viscometer. The test results obtained are shown in Table 1.
Test example 2
The apparent viscosities of the composite profile control systems obtained in the above examples and comparative examples were each tested by a Brookfield viscometer at a temperature of 70 ℃. The test results obtained are shown in Table 1.
Test example 3
The ageing and shear viscosity retention rate of the compound profile control system obtained in the examples and the comparative examples above were tested with reference to petrochemical enterprise standard Q/SH3135 438-2017. The liquid to be tested is the compound profile control system obtained in the above examples and comparative examples, and the aging viscosity retention rate is measured after the compound profile control system to be tested is aged in an oven at 70 ℃ for 45 days. The test results obtained are shown in Table 1.
Test example 4
The stability of the compound profile control system obtained in the above examples and comparative examples was tested. The specific detection method comprises the following steps: and (3) standing the composite profile control system to be tested at room temperature, and directly observing the number of days required for clarification by visual inspection. The more days needed for clarification, the better the stability of the system. In the stability test, if the solution is not turbid after 45 days, the observation is stopped, and the system can be put into use. The test results obtained are shown in Table 1.
TABLE 1
As can be seen from Table 1, in the profile control and flooding compound composed of the silicon dioxide nano particles with the surfaces modified by the alkyl groups and the acrylamide multipolymer, the viscosity of the compound is greatly improved compared with that of the original polymer through the hydrophobic association synergistic effect of the silicon dioxide nano particles with the surfaces modified by the alkyl groups and the acrylamide multipolymer, the stability is good, the ageing viscosity retention rate is improved, the shear viscosity retention rate is stable, and the compound is suitable for deep profile control and flooding of oil reservoirs. Specifically, the nano-silica surface is subjected to alkyl hydrophobic modification, and then the nano-silica surface and an acrylamide copolymer molecule containing long-chain alkyl hydrophobic groups strengthen hydrophobic association interaction, so that better performance is shown (example 1 and comparative example 2). Acrylamide copolymers with hydrophobic properties also have higher viscosities and viscosity retention than nanoparticles compared to conventional polyacrylamides (example 1 and comparative example 1). After the nano particles-polymer provided by the invention form a compound, the stability of the nano particles is enhanced, the interaction between the nano particles and the polymer is enhanced, and the crosslinking effect of intermolecular non-bonding effect is formed, so that the viscosity of a polymer system is greatly improved (example 1 and comparative examples 3 and 4). In addition, in comparative example 5, the nano-iron trioxide precipitated with the polymer, and the stability was too poor to evaluate the effect. Therefore, the composite profile control and flooding system prepared by adopting the acrylamide copolymer and the nano particles provided by the invention under the preferable condition of the invention has good temperature resistance, salt resistance, stability, water solubility, water phase tackifying, filterability, aging and shear viscosity retention rate, so that the composite profile control and flooding system has better profile control and flooding effect.
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 (10)
1. The compound with the deep profile control function is characterized by comprising an acrylamide multipolymer and silicon dioxide nano particles with the surfaces modified by alkyl groups.
2. The compound of claim 1, wherein the acrylamide multipolymer contains a first structural unit R provided by acrylamide 1 A second structural unit R provided by a substance of formula I 2 And providing a third structural unit R from a substance of formula II 3 ；
In the formula I, M 1 H, K or Na;
in formula II, X is O or NH, preferably NH; r is selected from C 1-18 Alkyl and/or phenyl, preferably C 6-16 Alkyl and/or phenyl;
preferably, the first structural unit R is based on 100 parts by weight of the acrylamide multipolymer 1 The content of the second structural unit R is 80-96 parts by weight 2 The content of the third structural unit R is 2-10 parts by weight 3 The content of (2-10 parts by weight);
preferably, the viscosity average molecular weight of the acrylamide multipolymer is 1000 ten thousand to 2000 ten thousand, more preferably 1000 ten thousand to 1500 ten thousand.
3. The composite of claim 1, wherein the molar ratio of silica to alkyl in the surface-modified nanoparticle is 1:0.3-0.8;
and/or, in the nanoparticles with the surfaces modified by alkyl groups, the substance providing the alkyl groups is alkyl trialkoxysilane;
and/or the number average particle diameter of the silicon dioxide nano particles with the surfaces modified by alkyl groups is 20-200nm;
preferably, in the nanoparticles whose surfaces are modified with alkyl groups, the substance providing the alkyl groups is alkyl triethoxysilane and/or alkyl trimethoxysilane, preferably wherein alkyl is C 1-18 More preferably C 6-14 Normal alkyl of (a);
preferably, the surface-alkyl-modified silica nanoparticle is prepared by the following method:
in a first solvent, firstly mixing the silicon dioxide nano-particles with an alkyl modifier, and then carrying out solid-liquid separation to obtain the silicon dioxide nano-particles with the surfaces modified by alkyl groups;
More preferably, the first mixing is performed under first stirring conditions, the first stirring being at a speed of 250-720 revolutions per minute;
more preferably, the temperature of the first mixing is 20-80 ℃ for 10-14 hours;
more preferably, the amount of the first solvent is 70-100mL, and the amount of the alkyl modifier is 1-10g, preferably 1.2-5g, based on 1g of the silica nanoparticle;
more preferably, the first solvent is an organic solvent, preferably at least one of cyclohexane, n-hexane and petroleum ether;
more preferably, the alkyl modifier is an alkyl trialkoxysilane, preferably the alkyl modifier is an alkyl triethoxysilane and/or an alkyl trimethoxysilane, preferably wherein alkyl is C 1-18 More preferably C 6-14 Normal alkyl of (a).
4. A composite according to any one of claims 1 to 3, wherein the weight ratio of the surface-alkyl-modified silica nanoparticles to the acrylamide multipolymer is 1:5 to 20, preferably 1:10 to 15.
5. A compound profile control system comprising the compound of any one of claims 1-4 and a second solvent;
Preferably, the concentration of the compound in the compound profile control system is 1200-5000ppm;
preferably, the second solvent is water.
6. A method of preparing a composite profile control system, the method comprising:
and in the presence of a second solvent, carrying out second mixing on the silicon dioxide nano particles with the surfaces modified by alkyl groups and the acrylamide multipolymer to obtain the composite profile control and flooding system.
7. The method of claim 6, wherein the method further comprises the step of preparing an acrylamide multipolymer: polymerizing the monomer mixture in water in the presence of an initiator under free radical aqueous solution polymerization conditions;
preferably, the monomer mixture contains acrylamide, a substance shown in a formula I and a substance shown in a formula II;
in the formula I, M 1 H, K or Na;
in formula II, X is O or NH, preferably NH; r is selected from C 1-18 Alkyl and/or phenyl, preferably C 6-16 Alkyl and/or phenyl;
preferably, the acrylamide is contained in an amount of 80 to 96 parts by weight, the substance represented by the formula I is contained in an amount of 2 to 10 parts by weight, and the substance represented by the formula II is contained in an amount of 2 to 10 parts by weight based on 100 parts by weight of the monomer mixture;
Preferably, the initiator is selected from azo-based initiators and/or redox-based initiators, more preferably redox-based initiators;
preferably, the polymerization is carried out in the presence of a complexing agent and urea;
more preferably, the redox initiator is selected from at least one of sulfate and sulfite redox initiators, persulfate and thiourea redox initiators, persulfate and organic salt redox initiators, persulfate and sulfite redox initiators, and ammonium persulfate and fatty amine redox initiators;
more preferably, the complexing agent is selected from at least one of disodium edetate, sodium nitrilotriacetate and diethylenetriamine pentacarboxylate, preferably disodium edetate;
more preferably, the urea is used in an amount of 0.01 to 0.1 wt.%, based on the total weight of the monomer mixture;
more preferably, the weight ratio of urea to complexing agent is 1-10:1;
more preferably, the polymerization conditions include: the temperature is-10 ℃ to 80 ℃, preferably 5-60 ℃; the time is 2-30 hours, preferably 8-20 hours; pH of 5-10, preferably 6-10
Further preferably, the redox initiator is selected from at least one of sodium sulfate and sodium sulfite, potassium sulfate and potassium sulfite, ammonium sulfate and sodium bisulfite, ammonium sulfate and ammonium sulfite, sodium persulfate and thiourea, potassium persulfate and thiourea, ammonium persulfate and thiourea, sodium persulfate and potassium acetate, potassium persulfate and potassium acetate, ammonium persulfate and ammonium acetate, ammonium persulfate and N, N-tetramethyl ethylenediamine, and ammonium persulfate and diethylamine.
8. The method of claim 6, wherein the method further comprises the step of preparing the surface-alkyl-modified silica nanoparticles:
in a first solvent, firstly mixing nano silicon dioxide particles with an alkyl modifier, and then carrying out solid-liquid separation to obtain silicon dioxide nano particles with the surfaces modified by alkyl;
preferably, the first mixing is performed under first stirring conditions, wherein the rotation speed of the first stirring is 250-720 revolutions per minute;
preferably, the temperature of the first mixing is 20-80 ℃ and the time is 10-14h;
preferably, the alkyl modifier is used in an amount of 1 to 10g, preferably 1.2 to 5g, based on 1g of the nano silica particles;
Preferably, the first solvent is used in an amount of 70-100mL, based on 1g of the nano-silica particles;
preferably, the first solvent is an organic solvent, preferably at least one of cyclohexane, n-hexane and petroleum ether;
preferably, the alkyl modifier is an alkyl trialkoxysilane;
more preferably, the alkyl modifier is an alkyl triethoxysilane and/or an alkyl trimethoxysilane, preferably wherein alkyl is C 1-18 More preferably C 6-14 Normal alkyl of (a).
9. The method according to any one of claims 6-8, wherein the amount of the surface-alkyl-modified silica nanoparticles and the acrylamide multipolymer is such that the weight ratio of the surface-alkyl-modified silica nanoparticles to the acrylamide multipolymer is 1:5-20, preferably 1:10-15;
preferably, the amount of the surface-modified silica nanoparticles and the acrylamide multipolymer is such that the total concentration of the surface-modified silica nanoparticles and the acrylamide multipolymer in the composite profile control system is 1200-5000ppm;
preferably, the second solvent is water.
10. A method of deep profile control in an oil field, the method comprising applying a profile control agent to an oil well in a well group in the oil field, wherein the profile control agent is a composite profile control system according to claim 5 or prepared by the method according to any one of claims 6 to 9.
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