CN116355606A - Fracturing auxiliary agent - Google Patents
Fracturing auxiliary agent Download PDFInfo
- Publication number
- CN116355606A CN116355606A CN202310344190.8A CN202310344190A CN116355606A CN 116355606 A CN116355606 A CN 116355606A CN 202310344190 A CN202310344190 A CN 202310344190A CN 116355606 A CN116355606 A CN 116355606A
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- Prior art keywords
- parts
- fracturing
- stirring
- preparing
- heating
- Prior art date
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- Granted
Links
- 239000012752 auxiliary agent Substances 0.000 title claims abstract description 35
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 41
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000003094 microcapsule Substances 0.000 claims abstract description 31
- 239000004927 clay Substances 0.000 claims abstract description 26
- 238000002360 preparation method Methods 0.000 claims abstract description 25
- 230000008961 swelling Effects 0.000 claims abstract description 22
- 239000003112 inhibitor Substances 0.000 claims abstract description 7
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims description 70
- 238000003756 stirring Methods 0.000 claims description 67
- 238000010438 heat treatment Methods 0.000 claims description 42
- 239000003446 ligand Substances 0.000 claims description 42
- 239000007864 aqueous solution Substances 0.000 claims description 41
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 39
- 238000002156 mixing Methods 0.000 claims description 37
- 150000002500 ions Chemical class 0.000 claims description 36
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 27
- 238000000034 method Methods 0.000 claims description 25
- 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
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 23
- 239000000243 solution Substances 0.000 claims description 21
- 238000005406 washing Methods 0.000 claims description 20
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 18
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 14
- 238000001914 filtration Methods 0.000 claims description 13
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 12
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 claims description 12
- OCBHHZMJRVXXQK-UHFFFAOYSA-M benzyl-dimethyl-tetradecylazanium;chloride Chemical compound [Cl-].CCCCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 OCBHHZMJRVXXQK-UHFFFAOYSA-M 0.000 claims description 11
- -1 alkynyl modified ammonium chloride Chemical class 0.000 claims description 10
- 229910021538 borax Inorganic materials 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 239000004328 sodium tetraborate Substances 0.000 claims description 10
- 235000010339 sodium tetraborate Nutrition 0.000 claims description 10
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- IUNMPGNGSSIWFP-UHFFFAOYSA-N dimethylaminopropylamine Chemical compound CN(C)CCCN IUNMPGNGSSIWFP-UHFFFAOYSA-N 0.000 claims description 8
- 229940057995 liquid paraffin Drugs 0.000 claims description 7
- 229940057838 polyethylene glycol 4000 Drugs 0.000 claims description 7
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 7
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 7
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 6
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- SUPCQIBBMFXVTL-UHFFFAOYSA-N ethyl 2-methylprop-2-enoate Chemical compound CCOC(=O)C(C)=C SUPCQIBBMFXVTL-UHFFFAOYSA-N 0.000 claims description 6
- 239000013067 intermediate product Substances 0.000 claims description 6
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims description 6
- LFZJRTMTKGYJRS-UHFFFAOYSA-N 1-chloro-4-ethynylbenzene Chemical compound ClC1=CC=C(C#C)C=C1 LFZJRTMTKGYJRS-UHFFFAOYSA-N 0.000 claims description 5
- 229920000858 Cyclodextrin Polymers 0.000 claims description 5
- 239000001116 FEMA 4028 Substances 0.000 claims description 4
- 229960004853 betadex Drugs 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 3
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 3
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 3
- 239000005642 Oleic acid Substances 0.000 claims description 3
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 3
- JZCCFEFSEZPSOG-UHFFFAOYSA-L copper(II) sulfate pentahydrate Chemical compound O.O.O.O.O.[Cu+2].[O-]S([O-])(=O)=O JZCCFEFSEZPSOG-UHFFFAOYSA-L 0.000 claims description 3
- 238000004821 distillation Methods 0.000 claims description 3
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 3
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 3
- 239000002244 precipitate Substances 0.000 claims description 3
- PPASLZSBLFJQEF-RKJRWTFHSA-M sodium ascorbate Substances [Na+].OC[C@@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RKJRWTFHSA-M 0.000 claims description 3
- 235000010378 sodium ascorbate Nutrition 0.000 claims description 3
- 229960005055 sodium ascorbate Drugs 0.000 claims description 3
- PPASLZSBLFJQEF-RXSVEWSESA-M sodium-L-ascorbate Chemical compound [Na+].OC[C@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RXSVEWSESA-M 0.000 claims description 3
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 3
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 claims description 2
- 239000003002 pH adjusting agent Substances 0.000 claims description 2
- FZGFBJMPSHGTRQ-UHFFFAOYSA-M trimethyl(2-prop-2-enoyloxyethyl)azanium;chloride Chemical compound [Cl-].C[N+](C)(C)CCOC(=O)C=C FZGFBJMPSHGTRQ-UHFFFAOYSA-M 0.000 claims description 2
- 239000012530 fluid Substances 0.000 abstract description 40
- 239000004576 sand Substances 0.000 abstract description 10
- 239000000693 micelle Substances 0.000 abstract description 8
- 230000008719 thickening Effects 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract 1
- VAZSKTXWXKYQJF-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)OOS([O-])=O VAZSKTXWXKYQJF-UHFFFAOYSA-N 0.000 description 22
- 239000003795 chemical substances by application Substances 0.000 description 17
- 238000012360 testing method Methods 0.000 description 17
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 12
- 239000007800 oxidant agent Substances 0.000 description 11
- 238000004132 cross linking Methods 0.000 description 10
- 230000001590 oxidative effect Effects 0.000 description 10
- 239000007788 liquid Substances 0.000 description 9
- 239000002775 capsule Substances 0.000 description 8
- 230000001105 regulatory effect Effects 0.000 description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 7
- 239000001301 oxygen Substances 0.000 description 7
- 229910052760 oxygen Inorganic materials 0.000 description 7
- 150000002978 peroxides Chemical class 0.000 description 7
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 6
- 239000004372 Polyvinyl alcohol Substances 0.000 description 6
- 238000006555 catalytic reaction Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 238000001816 cooling Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 229920002451 polyvinyl alcohol Polymers 0.000 description 6
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 description 5
- 230000018044 dehydration Effects 0.000 description 5
- 238000006297 dehydration reaction Methods 0.000 description 5
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 5
- 239000003921 oil Substances 0.000 description 5
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 5
- 238000000197 pyrolysis Methods 0.000 description 5
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 239000002784 hot electron Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 229910052750 molybdenum Inorganic materials 0.000 description 4
- 239000011733 molybdenum Substances 0.000 description 4
- ZIXQIYLQPUHVBI-UHFFFAOYSA-N 2-[carbamimidoyl(3-hydroxypropyl)amino]acetic acid Chemical compound C(=O)(O)CN(C(=N)N)CCCO ZIXQIYLQPUHVBI-UHFFFAOYSA-N 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 239000006004 Quartz sand Substances 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 238000004220 aggregation Methods 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000006228 supernatant Substances 0.000 description 3
- 230000002195 synergetic effect Effects 0.000 description 3
- 239000002562 thickening agent Substances 0.000 description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- 229920000297 Rayon Polymers 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 239000000084 colloidal system Substances 0.000 description 2
- 239000011162 core material Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 239000006166 lysate Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000005979 thermal decomposition reaction Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 241000282326 Felis catus Species 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 239000011609 ammonium molybdate Substances 0.000 description 1
- 230000008485 antagonism Effects 0.000 description 1
- 230000006399 behavior Effects 0.000 description 1
- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000012876 carrier material Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- 230000009920 chelation Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- ICYJJTNLBFMCOZ-UHFFFAOYSA-J molybdenum(4+);disulfate Chemical compound [Mo+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O ICYJJTNLBFMCOZ-UHFFFAOYSA-J 0.000 description 1
- VLAPMBHFAWRUQP-UHFFFAOYSA-L molybdic acid Chemical compound O[Mo](O)(=O)=O VLAPMBHFAWRUQP-UHFFFAOYSA-L 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000003129 oil well Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000000546 pharmaceutical excipient Substances 0.000 description 1
- 229940124531 pharmaceutical excipient Drugs 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 1
- 238000010944 pre-mature reactiony Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/62—Compositions for forming crevices or fractures
- C09K8/66—Compositions based on water or polar solvents
- C09K8/68—Compositions based on water or polar solvents containing organic compounds
- C09K8/685—Compositions based on water or polar solvents containing organic compounds containing cross-linking agents
-
- 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
- C09K8/62—Compositions for forming crevices or fractures
- C09K8/70—Compositions for forming crevices or fractures characterised by their form or by the form of their components, e.g. foams
- C09K8/706—Encapsulated breakers
-
- 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
- C09K8/86—Compositions based on water or polar solvents containing organic compounds
- C09K8/88—Compositions based on water or polar solvents containing organic compounds macromolecular compounds
- C09K8/882—Compositions based on water or polar solvents containing organic compounds macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
-
- 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
- C09K8/86—Compositions based on water or polar solvents containing organic compounds
- C09K8/88—Compositions based on water or polar solvents containing organic compounds macromolecular compounds
- C09K8/887—Compositions based on water or polar solvents containing organic compounds macromolecular compounds containing cross-linking agents
-
- 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
- C09K8/86—Compositions based on water or polar solvents containing organic compounds
- C09K8/88—Compositions based on water or polar solvents containing organic compounds macromolecular compounds
- C09K8/90—Compositions based on water or polar solvents containing organic compounds macromolecular compounds of natural origin, e.g. polysaccharides, cellulose
-
- 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
- C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
- C09K2208/12—Swell inhibition, i.e. using additives to drilling or well treatment fluids for inhibiting clay or shale swelling or disintegrating
-
- 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
- C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
- C09K2208/26—Gel breakers other than bacteria or enzymes
Abstract
The invention provides a fracturing auxiliary and a preparation method thereof. The fracturing aid consists of the following raw materials: novel cross-linking agent, microcapsule gel breaker, water, clay swelling inhibitor, demulsifier, pH regulator and functional assistant. According to the invention, a functional auxiliary agent is introduced, and is prepared in a click chemistry mode, so that the functional auxiliary agent has a lower critical micelle concentration and stronger surface tension reducing and viscosity increasing capabilities, and can be intertwined to form micelle worm shapes when being applied to fracturing fluid, and has good sand suspending and thickening capabilities.
Description
Technical Field
The invention relates to the field of petroleum fracturing fluids, in particular to a fracturing aid.
Background
The fracturing technology is an important means for increasing the production of the oil and gas well, and the fracturing fluid has the functions of carrying propping agent, transmitting pressure and fracturing to form a seam, and the quality of the fracturing fluid directly influences the success and failure of the fracturing operation.
Hydraulic fracturing is a main stimulation and injection measure of oil and gas reservoirs, and has been rapidly developed and widely used since fracturing is performed on a large scale.
At present, most of the fracturing auxiliary agents are single-function type, workers are now matched according to geological conditions, the operation is troublesome, because products of various factories are different, compatibility among different products in the system is poor, a synergistic effect is not ideal, even antagonism can be generated, and each single agent cannot exert the respective optimal effect, so that the comprehensive performance of the whole fracturing fluid system is reduced, stratum is seriously injured, and meanwhile, the production cost of oil gas development is increased. The fracturing auxiliary agent with multiple functions and capable of being effectively applied to most geology is a new development idea, and defects caused by personal configuration are reduced.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention provides a fracturing auxiliary agent and a preparation method thereof.
A method for preparing a fracturing aid, comprising the following steps: and mixing the novel cross-linking agent and the microcapsule gel breaker prepared by the method to obtain the fracturing aid.
Further, a preparation method of the fracturing auxiliary comprises the following steps:
heating 50-75 parts of water to 40-50 ℃ according to parts by mass, stirring at a rotating speed of 80-120r/min, adding 10-20 parts of clay swelling inhibitor into the water, and reacting for 0.5-1h; then adding 8-10 parts of demulsifier and continuously stirring for 0.5-1h; adding 0.5-1 part of pH regulator, and stirring for 20-30min; finally, heating to 50-60 ℃ at a speed of 1-10 ℃/min, adding 10-15 parts of novel cross-linking agent and 5-10 parts of microcapsule gel breaker, and stirring for 0.5-1h at a speed of 80-120r/min to obtain the fracturing aid.
Preferably, the demulsifier is one of an AP-type demulsifier, an AR-type demulsifier and an AE-type demulsifier; further preferably, the demulsifier is an AP-type demulsifier. The AP-type demulsifier is more suitable for liquid with higher water content, and can achieve the effect of rapid demulsification under the low-temperature condition. The SP-type demulsifier has a plurality of chain lengths and branched chains, and has higher hydrophilic capacity than that of a SP-type demulsifier with a single molecular structure. The characteristics of the multiple branched chains determine that the AP-type demulsifier has higher wettability and permeability, and molecules of the AP-type demulsifier can rapidly permeate into an oil-water interface film when a crude oil emulsion is demulsified.
Preferably, the pH regulator is one of citric acid, carbonic acid and acetic acid; further preferably, the pH adjuster is citric acid. Molybdenum trioxide is generated because molybdate ions are not easy to dehydrate under alkaline conditions; the molybdate is easy to be directly dehydrated in the presence of hydrochloric acid and nitric acid to generate molybdenum trioxide; in the presence of sulfuric acid, molybdic acid radicals readily react with sulfuric acid to form molybdenum sulfate, thus providing a suitable pH environment, which is necessary for the fracturing aid made in accordance with the present invention. Thus, three weak acids are preferred in the present invention, of which citric acid is more suitable for adjusting the pH of the fracturing aid made in the present invention due to its high volatile point, stronger acidity.
Preferably, the clay swelling preventing agent is one of cetyl trimethyl ammonium bromide, tetradecyl dimethyl benzyl ammonium chloride and polymethyl acryloyloxyethyl trimethyl ammonium chloride; further preferably, the clay swelling inhibitor is tetradecyldimethylbenzyl ammonium chloride. When clay contacts with water, the surface of the flaky structure is negatively charged, and the clay is separated under the action of electrostatic repulsive force, so that expansion is generated. Clay expansion occurs in the water injection stratum, so that the water injection speed is reduced; the oil production stratum undergoes earth boring expansion, and the oil well yield is reduced. The invention prefers tetradecyldimethylbenzyl ammonium chloride, and because of the existence of benzyl, the benzene ring has a large pi bond influence, the capacity of containing electrons is stronger, and the capacity of resolving the negative charge on the clay surface is stronger.
Further preferably, a method for preparing the fracturing aid comprises the following steps: heating 50-75 parts of water to 40-50 ℃ according to parts by mass, stirring at a rotating speed of 80-120r/min, adding 10-20 parts of clay swelling inhibitor into the water, and reacting for 0.5-1h; then adding 8-10 parts of demulsifier and continuously stirring for 0.5-1h; adding 0.5-1 part of pH regulator, and stirring for 20-30min; finally, heating to 50-60 ℃ at a speed of 1-10 ℃/min, adding 10-15 parts of novel cross-linking agent, 5-10 parts of microcapsule gel breaker and 5-8 parts of functional auxiliary agent, and stirring for 0.5-1h at a speed of 80-120r/min to obtain the fracturing auxiliary agent.
The preparation method of the functional auxiliary agent comprises the following steps: the preparation method of the functional auxiliary agent comprises the following steps: adding 25-30 parts of oleic acid into a container, then adding 0.16-0.3 part of p-toluenesulfonic acid, heating to 40-60 ℃, adding 7-10 parts of N, N-dimethyl-1, 3-diaminopropane, heating to 140-160 ℃ for reacting for 6-8 hours under the condition of nitrogen, and distilling under reduced pressure after the reaction is finished to remove the N, N-dimethyl-1, 3-diaminopropane and water to obtain an intermediate product; adding the intermediate product into 120-150 parts of isopropanol, then adding 5-7 parts of 1-chloro-4-ethynyl benzene, heating to 60-80 ℃ for reaction for 10-12 hours, performing reduced pressure distillation after the reaction is finished, and then washing and drying by adopting acetone to obtain alkynyl modified ammonium chloride; adding 5-7 parts of mono-6-azido-beta-cyclodextrin into 50-100 parts of toluene, performing ultrasonic dispersion for 3-10min, wherein the ultrasonic power is 100-500W, the ultrasonic frequency is 20-30kHz, adding 4-5 parts of alkynyl modified ammonium chloride, 0.1-0.2 part of copper sulfate pentahydrate and 0.4-0.5 part of sodium ascorbate, uniformly mixing, heating to 70-90 ℃ for reacting for 5-6h, centrifuging, taking out precipitate, washing and drying to obtain the functional auxiliary agent.
The functional auxiliary agent prepared by the method has lower critical micelle concentration and stronger capability of reducing surface tension and increasing viscosity, can be intertwined with each other to form micelle worm shape when being applied to fracturing fluid, has good sand suspending and thickening capabilities, contains more charged groups and has strong polarity, the aggregation structure among molecules is stronger, the viscosity of the functional auxiliary agent is increased due to the increase of carbon number in the functional auxiliary agent, and sand carrying capability is further improved.
The preparation method of the novel cross-linking agent comprises the following steps:
s1, mixing 8-12 parts of ligand and 85-100 parts of water according to parts by weight, and stirring for 5-10min at a rotating speed of 80-120r/min to obtain a ligand aqueous solution;
s2, mixing 2-5 parts of an ion source and 1-2 parts of a 20-30wt% sodium hydroxide aqueous solution according to parts by mass, and stirring for 3-5min at a rotating speed of 80-120r/min to obtain a mixed ion solution;
and S3, heating the ligand aqueous solution prepared in the step S1 to 70-85 ℃ at a speed of 1-10 ℃/min, dropwise adding the mixed ion solution into the ligand aqueous solution at a speed of 2-5mL/min, regulating the pH value to 7.0 by using a 20-30wt% hydrochloric acid aqueous solution after the dropwise adding is finished, reacting at a constant temperature for 1-3h, cooling to room temperature, filtering, washing and drying at room temperature to obtain the novel cross-linking agent.
Preferably, the ligand is one of triethanolamine, glycerol and citric acid; further preferably, the ligand is triethanolamine.
Preferably, the ion source is formed by mixing one or two of molybdenum trioxide and borax; further preferably, the ion source is prepared from molybdenum trioxide and borax according to the mass ratio of (1-2): (1-2) and mixing.
The invention selects molybdenum trioxide and borax as ion sources, uses sodium hydroxide aqueous solution to dissolve to obtain molybdate and borate, uses triethanolamine as ligand, and synthesizes the novel cross-linking agent by amino chelating molybdate and hydroxyl chelating borate. The formed novel cross-linking agent has two ion centers of boron and molybdenum, can cross-link more thickening agents containing hydroxyl, amino and other active groups, has stronger cross-linking capability than the cross-linking agent with a single ion center, has more compact chelating molecular groups, and improves the concentration of fracturing fluid. The novel crosslinking agent can realize good crosslinking in colloid containing hydroxyl or amino. In addition, under the high temperature condition of 80 ℃ and above, molybdenum trioxide is formed by dehydration of molybdic acid radicals, the crosslinking effect is lost, and the effect of reducing the viscosity of the pyrolysis liquid is achieved. The damage research of the fracturing fluid carried out abroad on the diversion capacity of the propping fracture is considered that the fracturing fluid can be concentrated by 5-7 times due to fluid loss during pumping and closing, so that the propping fracture is greatly damaged; the concentration of the lysate greatly improves the viscosity, which causes great trouble to the flowback of the later-stage lysate. And molybdenum trioxide is formed by dehydration along with the penetration of the pyrolysis liquid, so that the crosslinking capability is gradually lost, the viscosity of the pyrolysis liquid is favorably inhibited from rising, the damage to supporting cracks is reduced, and the time for breaking gel is shortened. Meanwhile, molybdenum trioxide formed by dehydration of molybdic acid radical also has excellent thermocatalytic performance, and the semiconductor material can transfer electrons from valence band to conduction band under thermal excitation to generate hot electrons and holes, further generate superoxide radicals, destroy gel structure and play a role of gel breaker.
Due to the limitation of the material, the molybdenum trioxide has insufficient thermal catalytic gel breaking capacity, so that the traditional gel breaker needs to be supplemented. The traditional gel breakers include three types, namely an oxidant breaker, an enzyme breaker and a capsule breaker. The oxidant breaker is preferably selected because the common potassium persulfate, ammonium persulfate and hydrogen peroxide are peroxides, oxygen can be generated at the same time of oxidation, and the oxygen is a carrier of electrons and holes generated by thermal catalysis of molybdenum trioxide, so that the higher the oxygen content is, the more superoxide radicals and hydrogen peroxide generated by thermal catalysis of the molybdenum trioxide are, and the higher the gel structure is damaged.
However, if the oxidizing agent and the crosslinking agent are directly mixed, molybdenum trioxide is directly dehydrated to form by the oxidizing agent, and thus the crosslinking effect is lost, which is to be avoided in the present invention. Therefore, the microcapsule gel breaker is further selected, the peroxide is wrapped by the capsule wall, so that the peroxide is prevented from contacting with the molybdate, the peroxide is released at high temperature and high pressure after the microcapsule gel breaker penetrates into a stratum, and the microcapsule gel breaker cooperates with molybdenum trioxide formed by dehydrating the molybdate, so that quick gel breaking and the return discharge of the pyrolysis liquid are realized.
The preparation method of the microcapsule gel breaker comprises the following steps: mixing 70-75 parts of chloroform, 10-14 parts of liquid paraffin and 0.1-1 part of polyvinylpyrrolidone, adding 6-8 parts of ammonium persulfate, 0.1-1 part of absolute ethyl alcohol, 0.1-0.5 part of n-amyl alcohol, 0.01-0.2 part of polyethylene glycol 4000, 4-6 parts of ethylenediamine tetraacetic acid and 0.1-1 part of ethyl methacrylate, stirring for 20-40min, and filtering, washing and airing to obtain the microcapsule gel breaker.
The microcapsule gel breaker selected by the invention can be slowly degraded along with the change of temperature and pressure, and the capsule core material is intensively released after the capsule coating material is slowly degraded, so that the concentrated release of ammonium persulfate of the capsule core can be ensured, the rapid reaction with molybdate is realized, and the synergistic gel breaking is realized. Furthermore, the surface property of the capsule wall is regulated and controlled by a plurality of alcohols, so that the microcapsule gel breaker with the particle size below 5 mu m is obtained. The extremely small particle size is beneficial to the dispersion in fracturing fluid, and when the fracturing fluid breaks, the breaker ammonium persulfate and colloid in the fracturing fluid are in full contact and react rapidly.
The invention has the beneficial effects that:
1. the microcapsule gel breaker is selected, the peroxide is wrapped by the capsule wall, so that the peroxide is prevented from contacting with molybdic acid root, and the peroxide is released at high temperature and high pressure after the microcapsule gel breaker penetrates into a stratum; and the property of molybdenum trioxide formed by high-temperature dehydration of molybdate is utilized, so that the molybdenum trioxide and an oxidant cooperate, oxygen is generated by the oxidant while oxidizing, the oxygen is a carrier of electrons and holes generated by thermal catalysis of the molybdenum trioxide, the higher the oxygen content is, the more superoxide radicals and hydrogen peroxide generated by thermal catalysis of the molybdenum trioxide are, the higher the speed of destroying a gel structure is, and therefore, the rapid gel breaking and the reverse drainage of a pyrolysis liquid are realized.
2. The functional auxiliary agent prepared by the method has lower critical micelle concentration and stronger capability of reducing surface tension and increasing viscosity, can be intertwined with each other to form micelle worm shape when being applied to fracturing fluid, has good sand suspending and thickening capabilities, contains more charged groups and has strong polarity, the aggregation structure among molecules is stronger, the viscosity of the functional auxiliary agent is increased due to the increase of carbon number in the functional auxiliary agent, and sand carrying capability is further improved.
Detailed Description
Liquid paraffin, CAS number: 32384-98-8, cat No.: KL816415, shanghai kang biosciences limited.
Polyvinylpyrrolidone, cat No.: s30268 Shanghai Source leaf Biotechnology Co., ltd.
AP demulsifier, cat No.: f-6, nantong Runfeng petrochemical Co., ltd.
Polyethylene glycol 4000, cat: 180-9187-4298 pharmaceutical excipients, inc. of Jinxiang, west An.
The preparation method of the mono-6-azido-beta-cyclodextrin described in the examples is described in reference to the preparation method adopted in section 2.3.1.2 (construction and property study based on three alkylamino cyclodextrin functional carrier materials, korean smile, university of agriculture and forestry science and technology, doctor paper, 2020).
N, N-dimethyl-1, 3-diaminopropane, CAS:109-55-7.
1-chloro-4-ethynylbenzene, CAS:873-73-4.
Example 1
A method for preparing a fracturing aid, comprising the following steps:
heating 60 parts of water to 45 ℃ according to parts by mass, stirring at a rotating speed of 100r/min, adding 15 parts of clay swelling preventing agent into the water, and reacting for 1h; then adding 9 parts of demulsifier and continuing stirring for 0.5h; adding 0.7 part of pH regulator, and continuously stirring for 25min; and finally, heating to 55 ℃ at a speed of 5 ℃/min, adding 15 parts of novel cross-linking agent, and stirring for 0.5h at a speed of 100r/min to obtain the fracturing auxiliary agent.
The demulsifier is an AP-type demulsifier.
The pH regulator is citric acid.
The clay swelling preventing agent is tetradecyl dimethyl benzyl ammonium chloride.
The preparation method of the novel cross-linking agent comprises the following steps:
s1, mixing 10 parts of ligand and 90 parts of water according to parts by mass, and stirring for 8 minutes at a rotating speed of 100r/min to obtain a ligand aqueous solution;
s2, mixing 3 parts of an ion source and 1.5 parts of 24wt% sodium hydroxide aqueous solution according to parts by mass, and stirring for 4min at a rotating speed of 100r/min to obtain a mixed ion solution;
and S3, heating the ligand aqueous solution prepared in the step S1 to 80 ℃ at a speed of 5 ℃/min, dripping the mixed ion solution into the ligand aqueous solution at a speed of 3mL/min, regulating the pH value to 7.0 by using 24wt% hydrochloric acid aqueous solution after the dripping is finished, reacting at constant temperature for 2 hours, cooling to room temperature, filtering, washing and drying at room temperature to obtain the novel cross-linking agent.
The ligand is triethanolamine.
The ion source is prepared from molybdenum trioxide and borax according to the mass ratio of 1:2, mixing.
Example 2
A method for preparing a fracturing aid, comprising the following steps:
heating 60 parts of water to 45 ℃ according to parts by mass, stirring at a rotating speed of 100r/min, adding 15 parts of clay swelling preventing agent into the water, and reacting for 1h; then adding 9 parts of demulsifier and continuing stirring for 0.5h; adding 0.7 part of pH regulator, and continuously stirring for 25min; and finally, heating to 55 ℃ at a speed of 5 ℃/min, adding 15 parts of novel cross-linking agent and 8 parts of oxidant gel breaker, and stirring for 0.5h at a speed of 100r/min to obtain the fracturing aid.
The oxidant breaker is ammonium persulfate.
The demulsifier is an AP-type demulsifier.
The pH regulator is citric acid.
The clay swelling preventing agent is tetradecyl dimethyl benzyl ammonium chloride.
The preparation method of the novel cross-linking agent comprises the following steps:
s1, mixing 10 parts of ligand and 90 parts of water according to parts by mass, and stirring for 8 minutes at a rotating speed of 100r/min to obtain a ligand aqueous solution;
s2, mixing 3 parts of an ion source and 1.5 parts of 24wt% sodium hydroxide aqueous solution according to parts by mass, and stirring for 4min at a rotating speed of 100r/min to obtain a mixed ion solution;
and S3, heating the ligand aqueous solution prepared in the step S1 to 80 ℃ at a speed of 5 ℃/min, dripping the mixed ion solution into the ligand aqueous solution at a speed of 3mL/min, regulating the pH value to 7.0 by using 24wt% hydrochloric acid aqueous solution after the dripping is finished, reacting at constant temperature for 2 hours, cooling to room temperature, filtering, washing and drying at room temperature to obtain the novel cross-linking agent.
The ligand is triethanolamine.
The ion source is prepared from molybdenum trioxide and borax according to the mass ratio of 1:2, mixing.
Example 3
A method for preparing a fracturing aid, comprising the following steps:
heating 60 parts of water to 45 ℃ in parts by mass, stirring at a rotating speed of 100r/min, adding 15 parts of clay swelling preventing agent into the mixture, and reacting for 1h; then adding 9 parts of demulsifier and continuing stirring for 0.5h; adding 0.7 part of pH regulator, and continuously stirring for 25min; and finally, heating to 55 ℃ at a speed of 5 ℃/min, adding 15 parts of novel cross-linking agent and 8 parts of microcapsule gel breaker, and stirring for 0.5h at a speed of 100r/min to obtain the fracturing aid.
The demulsifier is an AP-type demulsifier.
The pH regulator is citric acid.
The clay swelling preventing agent is tetradecyl dimethyl benzyl ammonium chloride.
The preparation method of the microcapsule gel breaker comprises the following steps: according to the mass parts, 73.09 parts of chloroform, 11.73 parts of liquid paraffin and 0.59 part of polyvinylpyrrolidone are mixed, then 7.73 parts of ammonium persulfate, 0.59 part of absolute ethyl alcohol, 0.2 part of n-amyl alcohol, 0.1 part of polyethylene glycol 4000, 5.28 parts of ethylenediamine tetraacetic acid and 0.59 part of ethyl methacrylate are added for mixing, stirring is carried out for 30 minutes, and the microcapsule gel breaker is obtained after filtering, washing and airing.
The preparation method of the novel cross-linking agent comprises the following steps:
s1, mixing 10 parts of ligand and 90 parts of water according to parts by mass, and stirring for 8 minutes at a rotating speed of 100r/min to obtain a ligand aqueous solution;
s2, mixing 3 parts of an ion source and 1.5 parts of 24wt% sodium hydroxide aqueous solution according to parts by mass, and stirring for 4min at a rotating speed of 100r/min to obtain a mixed ion solution;
and S3, heating the ligand aqueous solution prepared in the step S1 to 80 ℃ at a speed of 5 ℃/min, dripping the mixed ion solution into the ligand aqueous solution at a speed of 3mL/min, regulating the pH value to 7.0 by using 24wt% hydrochloric acid aqueous solution after the dripping is finished, reacting at constant temperature for 2 hours, cooling to room temperature, filtering, washing and drying at room temperature to obtain the novel cross-linking agent.
The ligand is triethanolamine.
The ion source is prepared from molybdenum trioxide and borax according to the mass ratio of 1:2, mixing.
Example 4
A method for preparing a fracturing aid, comprising the following steps:
heating 60 parts of water to 45 ℃ in parts by mass, stirring at a rotating speed of 100r/min, adding 15 parts of clay swelling preventing agent into the mixture, and reacting for 1h; then adding 9 parts of demulsifier and continuing stirring for 0.5h; adding 0.7 part of pH regulator, and continuously stirring for 25min; and finally, heating to 55 ℃ at a speed of 5 ℃/min, adding 15 parts of novel cross-linking agent and 8 parts of microcapsule gel breaker, and stirring for 0.5h at a speed of 100r/min to obtain the fracturing aid.
The demulsifier is an AP-type demulsifier.
The pH regulator is citric acid.
The clay swelling preventing agent is tetradecyl dimethyl benzyl ammonium chloride.
The preparation method of the microcapsule gel breaker comprises the following steps: according to the parts by mass, 73.09 parts of chloroform, 11.73 parts of liquid paraffin and 0.59 part of polyvinylpyrrolidone are mixed, then 7.73 parts of ammonium persulfate, 0.59 part of absolute ethyl alcohol, 0.2 part of n-amyl alcohol, 0.1 part of polyethylene glycol 4000, 5.28 parts of ethylenediamine tetraacetic acid and 0.59 part of ethyl methacrylate are added for mixing, and the microcapsule gel breaker is obtained after stirring, washing and airing.
The preparation method of the novel cross-linking agent comprises the following steps:
s1, mixing 10 parts of ligand and 90 parts of water according to parts by mass, and stirring for 8 minutes at a rotating speed of 100r/min to obtain a ligand aqueous solution;
s2, mixing 3 parts of an ion source and 1.5 parts of 24wt% sodium hydroxide aqueous solution according to parts by mass, and stirring for 4min at a rotating speed of 100r/min to obtain a mixed ion solution;
and S3, heating the ligand aqueous solution prepared in the step S1 to 80 ℃ at a speed of 5 ℃/min, dripping the mixed ion solution into the ligand aqueous solution at a speed of 3mL/min, regulating the pH value to 7.0 by using 24wt% hydrochloric acid aqueous solution after the dripping is finished, reacting at constant temperature for 2 hours, cooling to room temperature, filtering, washing and drying at room temperature to obtain the novel cross-linking agent.
The ligand is triethanolamine.
The ion source is borax.
Example 5
A method for preparing a fracturing aid, comprising the following steps:
heating 60 parts of water to 45 ℃ in parts by mass, stirring at a rotating speed of 100r/min, adding 15 parts of clay swelling preventing agent into the mixture, and reacting for 1h; then adding 9 parts of demulsifier and continuing stirring for 0.5h; adding 0.7 part of pH regulator, and continuously stirring for 25min; and finally, heating to 55 ℃ at a speed of 5 ℃/min, adding 15 parts of novel cross-linking agent and 8 parts of microcapsule gel breaker, and stirring for 0.5h at a speed of 100r/min to obtain the fracturing aid.
The demulsifier is an AP-type demulsifier.
The pH regulator is citric acid.
The clay swelling preventing agent is tetradecyl dimethyl benzyl ammonium chloride.
The preparation method of the microcapsule gel breaker comprises the following steps: according to the parts by mass, 73.09 parts of chloroform, 11.73 parts of liquid paraffin and 0.59 part of polyvinylpyrrolidone are mixed, then 7.73 parts of ammonium persulfate, 0.59 part of absolute ethyl alcohol, 0.2 part of n-amyl alcohol, 0.1 part of polyethylene glycol 4000, 5.28 parts of ethylenediamine tetraacetic acid and 0.59 part of ethyl methacrylate are added for mixing, and the microcapsule gel breaker is obtained after stirring, washing and airing.
The preparation method of the novel cross-linking agent comprises the following steps:
s1, mixing 10 parts of ligand and 90 parts of water according to parts by mass, and stirring for 8 minutes at a rotating speed of 100r/min to obtain a ligand aqueous solution;
s2, mixing 3 parts of an ion source and 1.5 parts of 24wt% sodium hydroxide aqueous solution according to parts by mass, and stirring for 4min at a rotating speed of 100r/min to obtain a mixed ion solution;
and S3, heating the ligand aqueous solution prepared in the step S1 to 80 ℃ at a speed of 5 ℃/min, dropwise adding the mixed ion solution into the ligand aqueous solution at a speed of 3mL/min, regulating the pH value to 7.0 by using 24wt% hydrochloric acid aqueous solution after the dropwise adding is finished, reacting at a constant temperature for 2 hours, filtering while the solution is hot to remove insoluble matters, treating the filtrate by using 95wt% ethanol aqueous solution, and crystallizing, filtering, washing and drying to obtain the novel cross-linking agent.
The ligand is triethanolamine.
The ion source is molybdenum trioxide.
Comparative example 1
A method for preparing a fracturing aid, comprising the following steps:
heating 60 parts of water to 45 ℃ according to parts by mass, stirring at a rotating speed of 100r/min, adding 15 parts of clay swelling preventing agent into the water, and reacting for 1h; then adding 9 parts of demulsifier and continuing stirring for 0.5h; adding 0.7 part of pH regulator, and continuously stirring for 25min; and finally, heating to 55 ℃ at a speed of 5 ℃/min, adding 15 parts of cross-linking agent and 8 parts of oxidant gel breaker, and stirring for 0.5h at a speed of 100r/min to obtain the fracturing aid.
The demulsifier is an AP-type demulsifier.
The pH regulator is citric acid.
The clay swelling preventing agent is tetradecyl dimethyl benzyl ammonium chloride.
The cross-linking agent is borax.
The oxidant breaker is ammonium persulfate.
Test example 1
Apparent viscosity test
Apparent viscosity test is carried out by referring to a high-temperature high-pressure coaxial cylinder viscometer in SY/T5107-2016 water-based fracturing fluid evaluation method. After the fracturing fluid is prepared, adding the fracturing fluid into a viscosimeter to a height of 2cm immediately, pressurizing by taking nitrogen with a pressure of 3MPa as a system, and starting 100s after the pressurization is finished -1 After shearing and stabilizing the rotation speed for 40s, the viscosity of the fracturing fluid at 25 ℃ is recorded. The test results are shown in Table 1.
Viscosity calculation formula: μ=kγ (n-1)
μ is viscosity in millipascal seconds (mpa.s);
k is the consistency coefficient independent of the geometrical parameters of the instrument, in millipascal seconds to the power n (mpa.s n );
Gamma is the shear rate in seconds to the negative power (s -1 );
n is the flow behavior index.
The preparation method of the fracturing fluid for the test comprises the following steps: mixing 15 parts of polyvinyl alcohol (PVA), 14 parts of carboxymethyl hydroxypropyl guanidine gum and 1000 parts of deionized water, and stirring at a speed of 800r/min for 15min to obtain a base solution; the fracturing auxiliary agent and the base liquid prepared in the examples and the comparative examples are mixed according to the mass ratio of 1.5:100, and stirring for 15min at a rotation speed of 600r/min to obtain the fracturing fluid for testing.
Table 1: apparent viscosity test results
Apparent viscosity/mPa.s at 25 DEG C | |
Example 1 | 562 |
Example 2 | 482 |
Example 3 | 564 |
Example 4 | 546 |
Example 5 | 536 |
Comparative example 1 | 461 |
As can be seen from table 1, the apparent viscosity of example 3 is highest at 25 ℃, because triethanolamine is used as a ligand, the chelation mode is that amino chelated molybdate and hydroxyl chelated borate in triethanolamine, and triethanolamine links the molybdate and borate, so that a novel cross-linking agent is formed, which has two ion centers of boron and molybdenum, can cross-link more thickening agents containing hydroxyl, amino and other active groups, has stronger cross-linking capability than the cross-linking agent with a single ion center, and has tighter chelated molecular groups, thus leading to the increase of viscosity. Examples 4 and 5 show an apparent viscosity slightly lower than example 3, further demonstrating that triethanolamine is used to link the molybdate and borate, and the novel chelating agent formed has a greater crosslinking capacity. The viscosity of the fracturing fluid corresponding to the embodiment 2 is extremely low, because the ammonium persulfate gel breaker is directly added, and ammonium persulfate and molybdate react, so that molybdenum trioxide is formed by dehydration of molybdate, and meanwhile, the ammonium persulfate also damages the molecular chain structure of the thickener, and antagonizes with the crosslinking agent, so that the viscosity of the fracturing fluid is reduced.
Test example 2
Gel breaking Performance test
The breaking performance of the fracturing fluid for test is tested by referring to the 7.9 th test of SY/T5107-2016 water-based fracturing fluid evaluation method.
The testing method comprises the following steps: the breaking speed and the complete breaking time are two important parameters of the breaking performance of the fracturing fluid. Placing the prepared fracturing fluid in a closed container, heating the fracturing fluid to 90 ℃ from 25 ℃ at a speed of 5 ℃/min, performing gel breaking experiments on the fracturing fluid at the temperature, and measuring the viscosity of supernatant. The viscosity of the supernatant can be measured by an NDJ28S type rotational viscometer, and the time required for the viscosity of the supernatant to reach 10 mPa.s can be measured, including the heating time at a rate of 5 ℃/min.
The preparation method of the fracturing fluid for the test comprises the following steps: mixing 15 parts of polyvinyl alcohol (PVA), 14 parts of carboxymethyl hydroxypropyl guanidine gum and 1000 parts of deionized water, and stirring at a speed of 800r/min for 15min to obtain a base solution; the fracturing auxiliary agent and the base liquid prepared in the examples and the comparative examples are mixed according to the mass ratio of 1.5:100, and stirring for 15min at a rotation speed of 600r/min to obtain the fracturing fluid for testing.
Table 2: gel breaking Property
Gel breaking time/min | |
Example 1 | 60 |
Example 2 | 15 |
Example 3 | 18 |
Example 4 | 80 |
Example 5 | 25 |
Comparative example 1 | 40 |
As can be seen from Table 2, the gel breaking time required in example 3 is shorter, 13min of the heating process at the rate of 5 ℃/min is removed, and after the temperature reaches 90 ℃, the viscosity of the gel solution is reduced to 10 mPa.s only for 5min, because at 85 ℃, the capsule shell of the microcapsule gel breaker begins to melt, ammonium persulfate is released, the triethanolamine-chelated molybdate ions are dehydrated under the action of the oxidant ammonium persulfate to generate molybdenum trioxide, the crosslinking effect of the triethanolamine-chelated molybdenum is reduced, further, as the temperature rises, the molybdenum trioxide is heated to excite to generate hot electrons and holes, and the molybdenum persulfate is synergistic with the ammonium persulfate, a large number of superoxide radicals can be further generated, and the gel structure is rapidly destroyed. Compared with example 3, the gel breaking time and the gel breaking performance shown in example 2 are shorter, but because the ammonium persulfate in example 2 is directly added, molybdenum trioxide is generated by premature reaction with molybdic acid radicals playing a role in crosslinking, the crosslinking capacity of the crosslinking agent is weakened, the viscosity of the fracturing fluid is reduced, meanwhile, the molybdenum trioxide and the ammonium persulfate cooperate, and the gel is broken prematurely, so that the viscosity of the initial fracturing fluid cannot meet the requirement of fracturing work, the performance of the fracturing work is not facilitated, and the fracturing fluid is not suitable for the fracturing work. Comparison of example 1 and example 3 shows that molybdenum trioxide is generated by virtue of thermal decomposition of molybdic acid radicals alone, and then the adhesive structure is destroyed by utilizing the thermal catalysis capability of the molybdenum trioxide, so that the adhesive breaking is performed too slowly. Firstly, molybdenum trioxide generated by thermal decomposition of molybdate is too slow, and the quantity of molybdenum trioxide generated in a short time is too small, so that quick gel breaking is not realized; secondly, the movement distance of hot electrons and holes generated by the thermal catalysis of the independent molybdenum trioxide is too short, and the catalytic degradation range is too small, so that the independent gel breaking speed is low. And ammonium persulfate can oxidize molybdate so as to quickly generate molybdenum trioxide, and meanwhile, oxygen molecules generated when the ammonium persulfate oxidizes and damages the viscose structure can become a transfer carrier of molybdenum trioxide hot electrons so as to generate superoxide radicals with longer service life, expand the catalytic degradation range of the superoxide radicals and realize quick gel breaking. As can be seen from the comparative examples, ammonium persulfate alone is also weak in breaking ability, which is determined by its own properties, and it is slow in breaking the viscose structure by oxidation and is also severely affected by concentration, temperature, etc. Therefore, the novel cross-linking agent synthesized by the invention and the microcapsule gel breaker containing ammonium persulfate cooperate to realize rapid gel breaking at a specific temperature, and the novel cross-linking agent can adapt to the fracturing work of a high-temperature oil layer and has excellent performance.
Example 6
A method for preparing a fracturing aid, comprising the following steps:
heating 60 parts of water to 45 ℃ in parts by mass, stirring at a rotating speed of 100r/min, adding 15 parts of clay swelling preventing agent into the mixture, and reacting for 1h; then adding 9 parts of demulsifier and continuing stirring for 0.5h; adding 0.7 part of pH regulator, and continuously stirring for 25min; and finally, heating to 55 ℃ at a speed of 5 ℃/min, adding 15 parts of novel cross-linking agent, 8 parts of microcapsule gel breaker and 5 parts of functional auxiliary agent, and stirring for 0.5h at a speed of 100r/min to obtain the fracturing auxiliary agent.
The demulsifier is an AP-type demulsifier.
The pH regulator is citric acid.
The clay swelling preventing agent is tetradecyl dimethyl benzyl ammonium chloride.
The preparation method of the microcapsule gel breaker comprises the following steps: according to the mass parts, 73.09 parts of chloroform, 11.73 parts of liquid paraffin and 0.59 part of polyvinylpyrrolidone are mixed, then 7.73 parts of ammonium persulfate, 0.59 part of absolute ethyl alcohol, 0.2 part of n-amyl alcohol, 0.1 part of polyethylene glycol 4000, 5.28 parts of ethylenediamine tetraacetic acid and 0.59 part of ethyl methacrylate are added for mixing, stirring is carried out for 30 minutes, and the microcapsule gel breaker is obtained after filtering, washing and airing.
The preparation method of the novel cross-linking agent comprises the following steps:
s1, mixing 10 parts of ligand and 90 parts of water according to parts by mass, and stirring for 8 minutes at a rotating speed of 100r/min to obtain a ligand aqueous solution;
s2, mixing 3 parts of an ion source and 1.5 parts of 24wt% sodium hydroxide aqueous solution according to parts by mass, and stirring for 4min at a rotating speed of 100r/min to obtain a mixed ion solution;
and S3, heating the ligand aqueous solution prepared in the step S1 to 80 ℃ at a speed of 5 ℃/min, dripping the mixed ion solution into the ligand aqueous solution at a speed of 3mL/min, regulating the pH value to 7.0 by using 24wt% hydrochloric acid aqueous solution after the dripping is finished, reacting at constant temperature for 2 hours, cooling to room temperature, filtering, washing and drying at room temperature to obtain the novel cross-linking agent.
The ligand is triethanolamine.
The ion source is prepared from molybdenum trioxide and borax according to the mass ratio of 1:2, mixing.
The preparation method of the functional auxiliary agent comprises the following steps: adding 25 parts of oleic acid into a container, adding 0.16 part of p-toluenesulfonic acid, heating to 50 ℃, adding 7 parts of N, N-dimethyl-1, 3-diaminopropane, heating to 160 ℃ and reacting for 8 hours under the condition of nitrogen, and distilling under reduced pressure after the reaction is finished to remove the N, N-dimethyl-1, 3-diaminopropane and water to obtain an intermediate product; adding the intermediate product into 150 parts of isopropanol, then adding 5 parts of 1-chloro-4-ethynyl benzene, heating to 80 ℃ for reaction for 12 hours, performing reduced pressure distillation after the reaction is finished, and then washing and drying by adopting acetone to obtain alkynyl modified ammonium chloride; adding 5 parts of mono-6-azido-beta-cyclodextrin into 60 parts of toluene, performing ultrasonic dispersion for 5min, wherein the ultrasonic power is 200W, the ultrasonic frequency is 20kHz, adding 4 parts of alkynyl modified ammonium chloride, 0.1 part of copper sulfate pentahydrate and 0.4 part of sodium ascorbate, uniformly mixing, heating to 70-90 ℃ for reacting for 5-6h, centrifuging, taking precipitate, washing and drying to obtain the functional auxiliary agent.
Test example 3
Sand carrying capability test:
the preparation method of the fracturing fluid for the test comprises the following steps: mixing 15 parts of polyvinyl alcohol (PVA), 14 parts of carboxymethyl hydroxypropyl guanidine gum and 1000 parts of deionized water, and stirring at a speed of 800r/min for 15min to obtain a base solution; the fracturing auxiliary agent and the base liquid prepared in the example 3 and the example 6 are respectively prepared according to the mass ratio of 1.5:100, and stirring for 15min at a rotation speed of 600r/min to obtain the fracturing fluid for testing.
Taking 250mL of the fracturing fluid obtained in the previous step in a 500mL beaker, taking three parts of the fracturing fluid in each embodiment, then respectively adding 20/40 mesh quartz sand into the three parts of the fracturing fluid in each embodiment, respectively adding 30 weight percent of the quartz sand in the three parts of the fracturing fluid, uniformly stirring, and observing the dropping speed of the quartz sand.
TABLE 3 sand carrying capacity
Sedimentation velocity/cm.h -1 | |
Example 3 | 0.36 |
Example 6 | 0.15 |
From the table, the fracturing auxiliary prepared by the invention has excellent sand carrying capacity in fracturing fluid. The functional auxiliary agent prepared by the method has lower critical micelle concentration and stronger capability of reducing surface tension and increasing viscosity, can be intertwined with each other to form micelle worm shape when being applied to fracturing fluid, has good sand suspending and thickening capabilities, contains more charged groups and has strong polarity, the aggregation structure among molecules is stronger, the viscosity of the functional auxiliary agent is increased due to the increase of carbon number in the functional auxiliary agent, and sand carrying capability is further improved.
Claims (10)
1. The preparation method of the fracturing auxiliary is characterized by comprising the following steps of: and mixing the novel cross-linking agent, the microcapsule gel breaker, water, the clay swelling inhibitor, the AP-type demulsifier, the pH regulator and the functional auxiliary agent to obtain the fracturing auxiliary agent.
2. The method of preparing a fracturing aid of claim 1, comprising the steps of:
heating 50-75 parts of water to 40-50 ℃ according to parts by mass, stirring at a rotating speed of 80-120r/min, adding 10-20 parts of clay swelling inhibitor into the water, and reacting for 0.5-1h; then adding 8-10 parts of AP-type demulsifier, and continuously stirring for 0.5-1h; adding 0.5-1 part of pH regulator, and stirring for 20-30min; finally, heating to 50-60 ℃ at a speed of 1-10 ℃/min, adding 10-15 parts of novel cross-linking agent, 5-10 parts of microcapsule gel breaker and 5-8 parts of functional auxiliary agent, and stirring for 0.5-1h at a speed of 80-120r/min to obtain the fracturing auxiliary agent.
3. The method for preparing the fracturing aid according to claim 1 or 2, wherein the method for preparing the functional aid comprises the following steps: the preparation method of the functional auxiliary agent comprises the following steps: adding 25-30 parts of oleic acid into a container, then adding 0.16-0.3 part of p-toluenesulfonic acid, heating to 40-60 ℃, adding 7-10 parts of N, N-dimethyl-1, 3-diaminopropane, heating to 140-160 ℃ for reacting for 6-8 hours under the condition of nitrogen, and distilling under reduced pressure after the reaction is finished to remove the N, N-dimethyl-1, 3-diaminopropane and water to obtain an intermediate product; adding the intermediate product into 120-150 parts of isopropanol, then adding 5-7 parts of 1-chloro-4-ethynyl benzene, heating to 60-80 ℃ for reaction for 10-12 hours, performing reduced pressure distillation after the reaction is finished, and then washing and drying by adopting acetone to obtain alkynyl modified ammonium chloride; adding 5-7 parts of mono-6-azido-beta-cyclodextrin into 50-100 parts of toluene, performing ultrasonic dispersion for 3-10min, wherein the ultrasonic power is 100-500W, the ultrasonic frequency is 20-30kHz, adding 4-5 parts of alkynyl modified ammonium chloride, 0.1-0.2 part of copper sulfate pentahydrate and 0.4-0.5 part of sodium ascorbate, uniformly mixing, heating to 70-90 ℃ for reacting for 5-6h, centrifuging, taking out precipitate, washing and drying to obtain the functional auxiliary agent.
4. The method of preparing a fracturing aid according to claim 1 or 2, wherein the pH adjuster is one of citric acid, carbonic acid and acetic acid.
5. The method for preparing the fracturing aid according to claim 1 or 2, wherein the clay swelling inhibitor is one of cetyl trimethyl ammonium bromide, tetradecyl dimethyl benzyl ammonium chloride and polymethyl acryloyloxyethyl trimethyl ammonium chloride.
6. The method for preparing the fracturing aid according to claim 1 or 2, wherein the method for preparing the novel cross-linking agent comprises the following steps:
s1, mixing a ligand and water to obtain a ligand aqueous solution;
s2, mixing an ion source and a sodium hydroxide aqueous solution to obtain a mixed ion solution;
s3, dripping the mixed ion solution into the ligand aqueous solution, adding the hydrochloric acid aqueous solution, filtering, washing and drying to obtain the novel cross-linking agent.
7. The method for preparing the fracturing aid according to claim 6, wherein the ligand is one of triethanolamine, glycerol and citric acid.
8. The method for preparing the fracturing aid according to claim 6, wherein the ion source is formed by mixing one or two of molybdenum trioxide and borax.
9. The method of preparing a fracturing aid according to claim 1 or 2, wherein the method of preparing a microcapsule breaker comprises the steps of: mixing 70-75 parts of chloroform, 10-14 parts of liquid paraffin and 0.1-1 part of polyvinylpyrrolidone, adding 6-8 parts of ammonium persulfate, 0.1-1 part of absolute ethyl alcohol, 0.1-0.5 part of n-amyl alcohol, 0.01-0.2 part of polyethylene glycol 4000, 4-6 parts of ethylenediamine tetraacetic acid and 0.1-1 part of ethyl methacrylate, stirring for 20-40min, and filtering, washing and airing to obtain the microcapsule gel breaker.
10. A fracturing aid prepared by the method of any one of claims 1 to 9.
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