CN114479782B - Plugging agent and preparation method and application thereof - Google Patents
Plugging agent and preparation method and application thereof Download PDFInfo
- Publication number
- CN114479782B CN114479782B CN202011166408.8A CN202011166408A CN114479782B CN 114479782 B CN114479782 B CN 114479782B CN 202011166408 A CN202011166408 A CN 202011166408A CN 114479782 B CN114479782 B CN 114479782B
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- China
- Prior art keywords
- starch
- plugging agent
- monomer
- vinyl
- gamma
- Prior art date
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- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- 229920002472 Starch Polymers 0.000 claims abstract description 116
- 239000008107 starch Substances 0.000 claims abstract description 112
- 235000019698 starch Nutrition 0.000 claims abstract description 112
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 106
- 239000000178 monomer Substances 0.000 claims abstract description 53
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 29
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 29
- 239000002734 clay mineral Substances 0.000 claims abstract description 16
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 16
- 238000004519 manufacturing process Methods 0.000 claims abstract description 10
- 229920001577 copolymer Polymers 0.000 claims abstract description 3
- 238000002156 mixing Methods 0.000 claims description 38
- 229920000578 graft copolymer Polymers 0.000 claims description 33
- 238000001035 drying Methods 0.000 claims description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- 238000005553 drilling Methods 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 20
- 239000003960 organic solvent Substances 0.000 claims description 19
- 238000006243 chemical reaction Methods 0.000 claims description 18
- 239000007864 aqueous solution Substances 0.000 claims description 16
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 15
- 239000012530 fluid Substances 0.000 claims description 14
- OXYZDRAJMHGSMW-UHFFFAOYSA-N 3-chloropropyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)CCCCl OXYZDRAJMHGSMW-UHFFFAOYSA-N 0.000 claims description 12
- 229920002261 Corn starch Polymers 0.000 claims description 12
- 239000008120 corn starch Substances 0.000 claims description 12
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 11
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims description 11
- 229910052901 montmorillonite Inorganic materials 0.000 claims description 11
- 229920001592 potato starch Polymers 0.000 claims description 10
- OOXSLJBUMMHDKW-UHFFFAOYSA-N trichloro(3-chloropropyl)silane Chemical compound ClCCC[Si](Cl)(Cl)Cl OOXSLJBUMMHDKW-UHFFFAOYSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 8
- 229910052622 kaolinite Inorganic materials 0.000 claims description 8
- -1 diallyl propane sulfonate Chemical compound 0.000 claims description 7
- 239000003999 initiator Substances 0.000 claims description 7
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims description 6
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 6
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 claims description 6
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 6
- 125000000129 anionic group Chemical group 0.000 claims description 6
- 125000002091 cationic group Chemical group 0.000 claims description 6
- GQOKIYDTHHZSCJ-UHFFFAOYSA-M dimethyl-bis(prop-2-enyl)azanium;chloride Chemical compound [Cl-].C=CC[N+](C)(C)CC=C GQOKIYDTHHZSCJ-UHFFFAOYSA-M 0.000 claims description 6
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 6
- 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 claims description 5
- 244000017020 Ipomoea batatas Species 0.000 claims description 5
- 235000002678 Ipomoea batatas Nutrition 0.000 claims description 5
- 240000002853 Nelumbo nucifera Species 0.000 claims description 5
- 235000006508 Nelumbo nucifera Nutrition 0.000 claims description 5
- 240000004922 Vigna radiata Species 0.000 claims description 5
- 235000010721 Vigna radiata var radiata Nutrition 0.000 claims description 5
- 235000011469 Vigna radiata var sublobata Nutrition 0.000 claims description 5
- 229910052900 illite Inorganic materials 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- VGIBGUSAECPPNB-UHFFFAOYSA-L nonaaluminum;magnesium;tripotassium;1,3-dioxido-2,4,5-trioxa-1,3-disilabicyclo[1.1.1]pentane;iron(2+);oxygen(2-);fluoride;hydroxide Chemical compound [OH-].[O-2].[O-2].[O-2].[O-2].[O-2].[F-].[Mg+2].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[K+].[K+].[K+].[Fe+2].O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2 VGIBGUSAECPPNB-UHFFFAOYSA-L 0.000 claims description 5
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 4
- 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 4
- LVNLBBGBASVLLI-UHFFFAOYSA-N 3-triethoxysilylpropylurea Chemical compound CCO[Si](OCC)(OCC)CCCNC(N)=O LVNLBBGBASVLLI-UHFFFAOYSA-N 0.000 claims description 4
- 240000003183 Manihot esculenta Species 0.000 claims description 4
- 235000016735 Manihot esculenta subsp esculenta Nutrition 0.000 claims description 4
- 235000003283 Pachira macrocarpa Nutrition 0.000 claims description 4
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 claims description 4
- 239000004113 Sepiolite Substances 0.000 claims description 4
- 240000001085 Trapa natans Species 0.000 claims description 4
- 235000014364 Trapa natans Nutrition 0.000 claims description 4
- 229960000892 attapulgite Drugs 0.000 claims description 4
- TZIHFWKZFHZASV-UHFFFAOYSA-N methyl formate Chemical compound COC=O TZIHFWKZFHZASV-UHFFFAOYSA-N 0.000 claims description 4
- 229910052625 palygorskite Inorganic materials 0.000 claims description 4
- 235000009165 saligot Nutrition 0.000 claims description 4
- 229910052624 sepiolite Inorganic materials 0.000 claims description 4
- 235000019355 sepiolite Nutrition 0.000 claims description 4
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 4
- 229940100445 wheat starch Drugs 0.000 claims description 4
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 3
- JHUFGBSGINLPOW-UHFFFAOYSA-N 3-chloro-4-(trifluoromethoxy)benzoyl cyanide Chemical compound FC(F)(F)OC1=CC=C(C(=O)C#N)C=C1Cl JHUFGBSGINLPOW-UHFFFAOYSA-N 0.000 claims description 3
- KSCAZPYHLGGNPZ-UHFFFAOYSA-N 3-chloropropyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)CCCCl KSCAZPYHLGGNPZ-UHFFFAOYSA-N 0.000 claims description 3
- AERFECJVKFIHED-UHFFFAOYSA-N 4-ethenylpyridin-1-ium;propane-1-sulfonate Chemical compound CCCS([O-])(=O)=O.C=CC1=CC=[NH+]C=C1 AERFECJVKFIHED-UHFFFAOYSA-N 0.000 claims description 3
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 claims description 3
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 claims description 3
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 3
- KRJRKEPWQOASJN-UHFFFAOYSA-N aniline;trimethoxy(methyl)silane Chemical compound NC1=CC=CC=C1.CO[Si](C)(OC)OC KRJRKEPWQOASJN-UHFFFAOYSA-N 0.000 claims description 3
- ZDOBWJOCPDIBRZ-UHFFFAOYSA-N chloromethyl(triethoxy)silane Chemical compound CCO[Si](CCl)(OCC)OCC ZDOBWJOCPDIBRZ-UHFFFAOYSA-N 0.000 claims description 3
- IOMDIVZAGXCCAC-UHFFFAOYSA-M diethyl-bis(prop-2-enyl)azanium;chloride Chemical compound [Cl-].C=CC[N+](CC)(CC)CC=C IOMDIVZAGXCCAC-UHFFFAOYSA-M 0.000 claims description 3
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 3
- KCXFHTAICRTXLI-UHFFFAOYSA-N propane-1-sulfonic acid Chemical compound CCCS(O)(=O)=O KCXFHTAICRTXLI-UHFFFAOYSA-N 0.000 claims description 3
- RRHXZLALVWBDKH-UHFFFAOYSA-M trimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]azanium;chloride Chemical compound [Cl-].CC(=C)C(=O)OCC[N+](C)(C)C RRHXZLALVWBDKH-UHFFFAOYSA-M 0.000 claims description 3
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 2
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 claims description 2
- ZGCZDEVLEULNLJ-UHFFFAOYSA-M benzyl-dimethyl-(2-prop-2-enoyloxyethyl)azanium;chloride Chemical compound [Cl-].C=CC(=O)OCC[N+](C)(C)CC1=CC=CC=C1 ZGCZDEVLEULNLJ-UHFFFAOYSA-M 0.000 claims description 2
- WBJINCZRORDGAQ-UHFFFAOYSA-N formic acid ethyl ester Natural products CCOC=O WBJINCZRORDGAQ-UHFFFAOYSA-N 0.000 claims description 2
- RQAKESSLMFZVMC-UHFFFAOYSA-N n-ethenylacetamide Chemical compound CC(=O)NC=C RQAKESSLMFZVMC-UHFFFAOYSA-N 0.000 claims description 2
- ZQXSMRAEXCEDJD-UHFFFAOYSA-N n-ethenylformamide Chemical compound C=CNC=O ZQXSMRAEXCEDJD-UHFFFAOYSA-N 0.000 claims description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 2
- SKNFSJNMUVGDKH-UHFFFAOYSA-M sodium 3-methyl-2-prop-2-enoyloxybut-1-ene-1-sulfonate Chemical compound C(C=C)(=O)OC(=CS(=O)(=O)[O-])C(C)C.[Na+] SKNFSJNMUVGDKH-UHFFFAOYSA-M 0.000 claims description 2
- 239000000243 solution Substances 0.000 claims description 2
- 239000001530 fumaric acid Substances 0.000 claims 1
- 229920000642 polymer Polymers 0.000 claims 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims 1
- 239000007822 coupling agent Substances 0.000 abstract description 7
- 230000007613 environmental effect Effects 0.000 abstract description 6
- 238000003756 stirring Methods 0.000 description 17
- 239000000463 material Substances 0.000 description 12
- 239000008367 deionised water Substances 0.000 description 8
- 229910021641 deionized water Inorganic materials 0.000 description 8
- 239000000725 suspension Substances 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 239000000843 powder Substances 0.000 description 7
- 239000000835 fiber Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 239000002245 particle Substances 0.000 description 5
- 239000002002 slurry Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 230000002265 prevention Effects 0.000 description 4
- 240000007049 Juglans regia Species 0.000 description 3
- 235000009496 Juglans regia Nutrition 0.000 description 3
- 230000000903 blocking effect Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000006116 polymerization reaction Methods 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 235000020234 walnut Nutrition 0.000 description 3
- 241000609240 Ambelania acida Species 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 150000004645 aluminates Chemical class 0.000 description 2
- 239000010905 bagasse Substances 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000002657 fibrous material Substances 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000010902 straw Substances 0.000 description 2
- IRLPACMLTUPBCL-KQYNXXCUSA-N 5'-adenylyl sulfate Chemical compound C1=NC=2C(N)=NC=NC=2N1[C@@H]1O[C@H](COP(O)(=O)OS(O)(=O)=O)[C@@H](O)[C@H]1O IRLPACMLTUPBCL-KQYNXXCUSA-N 0.000 description 1
- FHVDTGUDJYJELY-UHFFFAOYSA-N 6-{[2-carboxy-4,5-dihydroxy-6-(phosphanyloxy)oxan-3-yl]oxy}-4,5-dihydroxy-3-phosphanyloxane-2-carboxylic acid Chemical compound O1C(C(O)=O)C(P)C(O)C(O)C1OC1C(C(O)=O)OC(OP)C(O)C1O FHVDTGUDJYJELY-UHFFFAOYSA-N 0.000 description 1
- 229910021532 Calcite Inorganic materials 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 229920000881 Modified starch Polymers 0.000 description 1
- 239000004368 Modified starch Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229910002808 Si–O–Si Inorganic materials 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 229940072056 alginate Drugs 0.000 description 1
- 235000010443 alginic acid Nutrition 0.000 description 1
- 229920000615 alginic acid Polymers 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000010425 asbestos Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- CADWTSSKOVRVJC-UHFFFAOYSA-N benzyl(dimethyl)azanium;chloride Chemical compound [Cl-].C[NH+](C)CC1=CC=CC=C1 CADWTSSKOVRVJC-UHFFFAOYSA-N 0.000 description 1
- GQVVQDJHRQBZNG-UHFFFAOYSA-N benzyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)CC1=CC=CC=C1 GQVVQDJHRQBZNG-UHFFFAOYSA-N 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 229920002301 cellulose acetate Polymers 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000011487 hemp Substances 0.000 description 1
- NUKZAGXMHTUAFE-UHFFFAOYSA-N hexanoic acid methyl ester Natural products CCCCCC(=O)OC NUKZAGXMHTUAFE-UHFFFAOYSA-N 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000019426 modified starch Nutrition 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920002689 polyvinyl acetate Polymers 0.000 description 1
- 239000011118 polyvinyl acetate Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 229910052895 riebeckite Inorganic materials 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 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 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/02—Well-drilling compositions
- C09K8/03—Specific additives for general use in well-drilling compositions
- C09K8/035—Organic additives
-
- 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
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/42—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
- C09K8/426—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells for plugging
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/42—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells
- C09K8/46—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement
- C09K8/467—Compositions for cementing, e.g. for cementing casings into boreholes; Compositions for plugging, e.g. for killing wells containing inorganic binders, e.g. Portland cement containing additives for specific purposes
-
- E—FIXED CONSTRUCTIONS
- E21—EARTH OR ROCK DRILLING; MINING
- E21B—EARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
- E21B33/00—Sealing or packing boreholes or wells
- E21B33/10—Sealing or packing boreholes or wells in the borehole
- E21B33/13—Methods or devices for cementing, for plugging holes, crevices or the like
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Geology (AREA)
- Mining & Mineral Resources (AREA)
- Geochemistry & Mineralogy (AREA)
- Physics & Mathematics (AREA)
- Fluid Mechanics (AREA)
- Environmental & Geological Engineering (AREA)
- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a plugging agent, a preparation method and application thereof, wherein the plugging agent comprises a structural unit A, a structural unit B and a structural unit C, wherein the structural units A and C form a copolymer through a cross-linking agent; wherein the structural unit A is starch; the structural unit B is a vinyl monomer-containing structural unit; the structural unit C is a clay mineral unit. The preparation method of the plugging agent uses a coupling agent to combine organic starch and inorganic clay minerals. The plugging agent has the advantages of good high temperature resistance, high pressure bearing capacity, environmental protection in production and application and the like.
Description
Technical Field
The invention belongs to the technical field of petroleum exploitation, and particularly relates to a plugging material and a preparation method thereof.
Background
The lost circulation is a technical problem in the drilling, well cementation, well logging and well repairing processes, and can cause the drilling fluid to leak into a leakage channel from a well bore, so that a large amount of slurry and plugging materials are consumed, and serious accidents such as well collapse, drilling sticking, blowout and even well bore scrapping can be caused, thereby causing huge economic loss. The plugging material is indispensable in the process of well drilling leakage prevention, and the success rate of well drilling leakage prevention and plugging is directly dependent on the performance of the plugging material. Therefore, the research of the plugging material has very important significance.
At present, research on the well drilling leakage prevention and leakage blocking technology at home and abroad is fast, various solutions are provided, and a series of novel leakage blocking materials and leakage prevention and blocking systems are developed and developed at the same time. The bridging plugging technology has the characteristics of being the most widely applied plugging technology, and inert materials with different shapes and different sizes are mixed in a drilling fluid system according to a certain proportion, and then are injected into a leakage stratum to perform plugging, so that the requirement on a material matching level is high. The bridge-erecting particles commonly used at present mainly comprise rigid particles such as walnut shells and the like and fiber materials such as sawdust and bagasse, wherein the rigid particles such as walnut shells and the like have the characteristics of higher pressure bearing capacity and difficult deformation, but are easy to carbonize under the high-temperature condition; and fiber materials such as sawdust and bagasse are easy to fail under high pressure conditions, so that an effective plugging layer cannot be formed by conventional plugging materials and well slurry. Other types of plugging materials have the common problems of high price, complex plugging process, small improvement range of the pressure bearing capacity of a plugging layer, poor environmental protection indexes of production and application and the like.
CN 201910933718.9 discloses a rigid plugging agent for drilling fluid and a preparation method thereof, wherein the rigid plugging agent comprises walnut shells, calcite, sawdust, polypropylene fibers and elastic particles. Effectively solves the problems of poor pressure bearing capacity and plugging effect, easy leakage, high production cost and lower cost performance of the plugging agent. CN 201910318778. X discloses an acid-soluble pressure-bearing plugging agent for drilling fluid and a preparation method thereof. Consists of crop straw extracted fiber, polyester fiber, cellulose acetate, glass fiber, asbestos fiber, cotton-hemp plant fiber, rock-making mineral powder, alginate, dimethyl diallyl ammonium chloride, polyvinyl acetate, n-octyl alpha-cyanoacrylate, diatomite and proper amount of clear water. The fiber extracted from crop straws with lower cost can be used as the main raw material of the plugging agent, and the plugging effect and the pressure-bearing effect can be well realized.
Disclosure of Invention
Aiming at the defects of the prior art, the invention mainly aims to provide the plugging agent, and the preparation method and the application thereof, wherein the plugging agent has the advantages of good high temperature resistance, high pressure bearing capacity, environmental protection in production and application and the like.
The first aspect of the present invention provides a plugging agent comprising structural unit a, structural unit B and structural unit D, wherein structural units a and D form a copolymer by a crosslinking agent;
the structural unit A is starch;
the structural unit B is a vinyl monomer-containing structural unit;
the structural unit D is a clay mineral unit;
the plugging agent has the following structural formula:
the structural formula of the structural unit B is
Or->
The method comprises the steps of carrying out a first treatment on the surface of the Wherein R is 1 And R is 3 Is the side chain structure of the vinyl polymer except the vinyl structure, R 2 CH-or N (nitrogen).
R is a methylene chain in the coupling agent, and forms a covalent bond Si-O-Si with HO-Si in the clay mineral through Si; the number of carbon atoms in the methylene chain is an integer of 1 to 5 (specifically 1, 2, 3, 4, 5), preferably an integer of 1 to 3 (specifically 1, 2, 3), in particular-CH 2 -、-CH 2 CH 2 -、-CH 2 CH 2 CH 2 -、-CH 2 CH 2 CH 2 -、-CH 2 CH 2 CH 2 CH 2 -、-CH 2 CH 2 CH 2 CH 2 CH 2 -；
m is the degree of polymerization of the starch building block, x is the degree of polymerization of the vinyl monomer, and m+x=800 to 1600.
In the plugging agent, the total amount of the plugging agent is taken as a reference, the content of the structural unit A is 20-65wt%, the content of the structural unit B is 12-55wt%, the content of the structural unit D is 12-55wt%, and the content of the cross-linking agent is 0.5-10wt%.
In the plugging agent, the pressure bearing capacity of the plugging agent is not lower than 4MPa.
In the plugging agent, the starch can be one or more of mung bean starch, tapioca starch, sweet potato starch, wheat starch, water chestnut starch, lotus root starch and corn starch, preferably corn starch and/or potato starch.
In the plugging agent, the vinyl-containing monomer is a water-soluble vinyl monomer and can be one or more of a cationic monomer, an anionic monomer, a nonionic monomer and a zwitterionic monomer; further, the zwitterionic monomer is one or more of methacryloxyethyl-N, N-dimethyl propane sulfonate (DMAPS), N-dimethyl allyl amine propane sulfonate (DAPS), 4-Vinyl Pyridine Propane Sulfonate (VPPS), N-methyl diallyl propane sulfonate (MAPS) and N-methyl diallyl butane sulfonate (MABS), and is preferably N-methyl diallyl propane sulfonate. The cationic monomer is one or more of methacryloxyethyl trimethyl ammonium chloride (DMC), acryloxyethyl trimethyl ammonium chloride (DAC), acryloxyethyl dimethyl benzyl ammonium chloride (DBC), dimethyl diallyl ammonium chloride (DMDAAC) and diethyl diallyl ammonium chloride (DEDAAC), preferably dimethyl diallyl ammonium chloride. The anionic monomer is one or more of AA (acrylic acid), 2-methyl-2-acrylamidopropane sulfonic Acid (AMPS), fumaric Acid (FA), sodium allylsulfonate (SSS) and sodium 2-acryloyloxyisopentene sulfonate (AOIAS), and preferably 2-methyl-2-acrylamidopropane sulfonic acid. The nonionic monomer is one or more of N-vinyl pyrrolidone (NVP), acrylonitrile (AN), vinyl formamide (NVF) and vinyl acetamide (NVA), preferably N-vinyl pyrrolidone.
Among the plugging agents, the cross-linking agent can be one or more of a silane coupling agent, a titanate coupling agent and an aluminate coupling agent, and is preferably a silane coupling agent. Wherein the silane coupling agent is one or more of gamma-chloropropyl trichlorosilane, gamma-chloropropyl methyl dichlorosilane, gamma-chloropropyl trimethoxysilane, gamma-chloropropyl triethoxysilane, chloromethyl triethoxysilane, gamma-aminopropyl trimethoxysilane, gamma- (beta-aminoethyl) aminopropyl trimethoxysilane, gamma-ureido propyl triethoxysilane and aniline methyl trimethoxysilane, preferably one or more of gamma-chloropropyl trichlorosilane, gamma-chloropropyl trimethoxysilane, gamma-aminopropyl triethoxysilane and gamma-aminopropyl trimethoxysilane, and further preferably gamma-chloropropyl trichlorosilane and/or gamma-chloropropyl trimethoxysilane.
In the plugging agent, the clay mineral is one or more of kaolinite, montmorillonite, illite, sepiolite and attapulgite, preferably kaolinite, montmorillonite and illite, and more preferably montmorillonite.
The second aspect of the invention provides a preparation method of a plugging agent, which comprises the following steps:
(1) Mixing starch with water, and uniformly mixing to obtain gelatinized starch;
(2) Mixing vinyl-containing monomer with water, and uniformly mixing to obtain a vinyl-containing monomer aqueous solution;
(3) Mixing the vinyl monomer-containing aqueous solution obtained in the step (2) with the gelatinized starch obtained in the step (1), adding an initiator after uniformly mixing, and reacting to obtain a starch graft copolymer;
(4) The starch graft copolymer obtained in the step (3) is dried and crushed to obtain powdery starch graft copolymer;
(5) Dispersing the powdery starch graft copolymer obtained in the step (4) into an organic solvent, then adding clay mineral and a cross-linking agent, and separating and drying after the reaction is completed to obtain the plugging agent.
In the preparation method of the plugging agent, the mixing temperature in the step (1) is 50-100 ℃, preferably 80-95 ℃.
In the preparation method of the plugging agent, the mass fraction of starch in the gelatinized starch in the step (1) is 5-20wt%.
In the preparation method of the plugging agent, the starch in the step (1) is one or more of mung bean starch, tapioca starch, sweet potato starch, wheat starch, water chestnut starch, lotus root starch and corn starch, preferably corn starch and/or potato starch.
In the preparation method of the plugging agent, the mass fraction of the vinyl-containing polymerized monomer aqueous solution in the step (2) is 30-60 wt%.
In the preparation method of the plugging agent, the mixing temperature in the step (3) is 40-90 ℃, and the reaction temperature is 50-80 ℃.
In the preparation method of the plugging agent, the initiator in the step (3) is one or more of potassium persulfate, sodium persulfate and ammonium persulfate; the initiator is used in an amount of 0.5 to 1.5wt% based on the total mass of the starch and the vinyl-containing monomer.
In the preparation method of the plugging agent, the dosage ratio of the vinyl monomer-containing aqueous solution obtained in the step (2) to the gelatinized starch obtained in the step (1) in the step (3) is 1: 4-2: 1.
in the preparation method of the plugging agent, the drying condition in the step (4) is that the plugging agent is dried for 8 to 16 hours at the temperature of 60 to 120 ℃.
In the preparation method of the plugging agent, any one of the existing modes capable of breaking the solid-phase materials, such as a pulverizer and the like, can be adopted for breaking in the step (4), and specific conditions for breaking can be selected by a person skilled in the art according to actual needs of products.
In the preparation method of the plugging agent, the organic solvent in the step (5) is an organic solvent which can not dissolve the swelling starch but can dissolve the crosslinking agent, and can be one or more of alcohol, methanol, ethanol, propanol, butanol, methyl formate, ethyl acetate, ethyl formate, methyl acetate, butyl acetate and the like.
In the preparation method of the plugging agent, the dosage of the organic solvent in the step (5) is 2-8 times of the total mass of the starch and the vinyl-containing monomer.
In the preparation method of the plugging agent, the cross-linking agent in the step (5) can be one or more of a silane coupling agent, a titanate coupling agent and an aluminate coupling agent, and is preferably a silane coupling agent. Wherein the silane coupling agent is one or more of gamma-chloropropyl trichlorosilane, gamma-chloropropyl methyl dichlorosilane, gamma-chloropropyl trimethoxysilane, gamma-chloropropyl triethoxysilane, chloromethyl triethoxysilane, gamma-aminopropyl trimethoxysilane, gamma- (beta-aminoethyl) aminopropyl trimethoxysilane, gamma-ureido propyl triethoxysilane and aniline methyl trimethoxysilane, preferably one or more of gamma-chloropropyl trichlorosilane, gamma-chloropropyl trimethoxysilane, gamma-aminopropyl triethoxysilane and gamma-aminopropyl trimethoxysilane, and further preferably gamma-chloropropyl trichlorosilane and/or gamma-chloropropyl trimethoxysilane.
In the preparation method of the plugging agent, in the step (5), the clay mineral is one or more of kaolinite, montmorillonite, illite, sepiolite and attapulgite, preferably kaolinite, montmorillonite and illite, and more preferably montmorillonite. The particle size of the clay mineral is not less than 200 meshes.
In the preparation method of the plugging agent, the reaction temperature of the adding cross-linking agent in the step (5) is 30-70 ℃.
In the preparation method of the plugging agent, the separation in the step (5) can be one or more of standing, layering and filtering, centrifugal separation, spray drying, direct powdering and the like.
In the preparation method of the plugging agent, the drying condition in the step (5) is that the plugging agent is dried for 8 to 16 hours at the temperature of 60 to 120 ℃.
According to a third aspect of the invention, there is provided a drilling fluid comprising the above plugging agent, wherein the plugging agent is present in an amount of from 0.5 to 20wt%, preferably from 2 to 10wt%, more preferably from 3 to 7wt%, based on the total weight of the drilling fluid. The drilling fluid added with the plugging agent has good plugging capability, can effectively plug pores or micro cracks, prevent filtrate from penetrating into stratum in a large amount, reduce filtrate loss and play a good role in plugging. .
A fourth aspect of the present invention provides the use of a plugging agent as described above in a drilling process.
When the plugging agent is used in the drilling process, the addition amount is 0.1-5 wt%, preferably 0.5-5 wt%, and more preferably 1-5 wt%.
Compared with the prior art, the plugging agent and the preparation method thereof have the following advantages:
1. the plugging agent provided by the invention uses the vinyl polymerization monomer grafted modified starch, so that the starch has functionality, and besides ensuring the plugging property of the plugging agent, the temperature resistance, salt resistance and calcium resistance of the plugging agent in drilling fluid are improved, wherein the temperature resistance is not lower than 160 ℃, the salt resistance can reach saturation, and the calcium resistance is not lower than 5wt%.
2. In the preparation method of the plugging agent, the coupling agent is used for combining the organic starch and the inorganic clay mineral, so that on one hand, the structural rigidity of the material is increased, and the pressure bearing capacity of the plugging agent is improved. On the other hand, the grafted starch part in the plugging agent has high viscosity after being dissolved in water, and can tightly connect clay minerals of inert parts with stratum, enhance the interface effect and further improve the bearing capacity. The clay mineral has the same lithology as the stratum, and the structure containing silicon and oxygen is further condensed under high temperature and high pressure to form a bonding structure, so that the plugging and bearing capacity under high temperature and high pressure is greatly improved.
3. The preparation method of the plugging agent belongs to a green pollution-free synthesis method, uses a nontoxic and harmless organic solvent as an interface reaction system, has simple and controllable reaction process, is easy to dry into powder, greatly reduces the production energy consumption and cost, and truly achieves the aims of environmental protection of raw materials, environmental protection of production and environmental protection of application.
Drawings
FIG. 1 is an infrared spectrum of a plugging agent prepared in example 1 of the present invention.
Detailed Description
The plugging agent of the present invention, its preparation method and application are further described below by way of specific examples, but the present invention is not limited thereto.
Example 1
40g of corn starch is weighed and added into deionized water to prepare a starch suspension with the mass fraction of 15%. Stirring at 90deg.C for 60min to obtain gelatinized starch; then, 30g of methacryloyloxyethyl-N, N-dimethylpropanesulfonate was weighed and prepared as a 50% by mass aqueous solution. Adding into gelatinized starch, and mixing at 70deg.C for 30min; adding 0.56g of potassium persulfate, and reacting for 3 hours at 70 ℃ to obtain a viscous starch graft copolymer; drying and dewatering at 110 ℃, and crushing to obtain the powdery starch graft copolymer. Dispersing the powdery starch graft copolymer in 300mL of ethyl acetate, and fully stirring and dispersing for 30min; adding 30g of kaolinite, mixing and re-dispersing for 30min; 5g of gamma-chloropropyl trimethoxysilane are added and reacted for 4h at 45 ℃. After the reaction, separating and removing the organic solvent, drying for 8 hours at 110 ℃, and crushing to obtain the plugging agent. The infrared spectrum of the plugging agent is shown in figure 1, and the analysis of figure 1 shows that the plugging agent is 3434cm -1 2931 is the characteristic peak of OH in starch cm -1 、2846 cm -1 And 1386 cm -1 is-CH-, -CH 2 -、CH 3 Characteristic peak, 1640 cm -1 As c=o characteristic peak in monomer, 1048 cm -1 Is a characteristic peak of Si-O-C.
Example 2
20g of potato starch is weighed and added into deionized water to prepare a starch suspension with the mass fraction of 8%. Stirring at 85deg.C for 80min to obtain gelatinized starch; 35g of 2-methyl-2-acrylamidopropane sulfonic acid was weighed to prepare a 52% by mass aqueous solution. Adding into gelatinized starch, and mixing at 60deg.C for 30min; adding 0.61g of ammonium persulfate, and reacting for 4 hours at 60 ℃ to obtain a viscous starch graft copolymer; drying at 120 deg.c to eliminate water and crushing to obtain powdered starch graft copolymer. Dispersing starch graft copolymer powder in 450mL of methanol, and fully stirring and dispersing for 30min; adding 15g of montmorillonite, mixing and re-dispersing for 30min; 4g of gamma-chloropropyl trichlorosilane are added and reacted for 4 hours at 55 ℃. After the reaction, separating and removing the organic solvent, drying for 12 hours at 90 ℃ and crushing to obtain the plugging agent.
Example 3
33g of sweet potato starch is weighed and added into deionized water to prepare starch suspension with the mass fraction of 20%. Stirring at 80deg.C for 90min to obtain gelatinized starch; 15g of methacryloyloxyethyl trimethyl ammonium chloride was weighed to prepare a 30% by mass aqueous solution. Adding into gelatinized starch, and mixing at 55deg.C for 30min; adding 0.62g of sodium persulfate, and reacting for 4 hours at 55 ℃ to obtain a viscous starch graft copolymer; drying at 90 ℃ to remove water, and crushing to obtain the powdery starch graft copolymer. Dispersing starch graft copolymer powder in 550ml ethanol, and stirring thoroughly for 30min; then adding 27g of montmorillonite, mixing and re-dispersing for 30min; 2.5g of gamma-aminopropyl triethoxysilane was added and reacted at 50℃for 3h. Separating and removing the organic solvent after the reaction, drying for 10 hours at 120 ℃, and crushing to obtain the plugging agent.
Example 4
25g of mung bean starch is weighed and added into deionized water to prepare a starch suspension with the mass fraction of 5%. Stirring at 90deg.C for 70min to obtain gelatinized starch; 40, g N-vinyl pyrrolidone is weighed and prepared into a 60% aqueous solution by mass percent. Adding into gelatinized starch, and mixing at 75deg.C for 30min; adding 0.33g of potassium persulfate, and reacting for 2 hours at 75 ℃ to obtain a viscous starch graft copolymer; drying at 70 ℃ to remove water, and crushing to obtain the powdery starch graft copolymer. Dispersing starch graft copolymer powder in 420ml butyl acetate, and fully stirring and dispersing for 30min; adding 10g of attapulgite, mixing and re-dispersing for 30min; 4.5g of phenylmethyltrimethoxysilane were added and reacted at 60℃for 3 hours. After the reaction, separating and removing the organic solvent, drying for 9 hours at 100 ℃ and crushing to obtain the plugging agent.
Example 5
35g of lotus root starch is weighed and added into deionized water to prepare a starch suspension with the mass fraction of 16%. Stirring at 93 ℃ for 60min to obtain gelatinized starch; then, 10g of sodium allylsulfonate was weighed to prepare a 42% by mass aqueous solution. Adding into gelatinized starch, and mixing at 80deg.C for 30min; adding 0.68g of sodium persulfate, and reacting for 2.5 hours at 80 ℃ to obtain a viscous starch graft copolymer; drying and dewatering at 95 ℃, and crushing to obtain the powdery starch graft copolymer. Dispersing starch graft copolymer powder in 380ml ethanol, and stirring thoroughly for 30min; adding 40g of sepiolite, mixing and re-dispersing for 30min; 1g of gamma-chloropropyl trimethoxysilane was added and reacted at 55℃for 2h. Separating and removing the organic solvent after the reaction, drying for 11 hours at 95 ℃, and crushing to obtain the plugging agent.
Example 6
22g of corn starch is weighed and added into deionized water to prepare a starch suspension with the mass fraction of 10%. Stirring at 88 deg.C for 75min to obtain gelatinized starch; 18g of 4-vinylpyridine propane sulfonate was weighed again and prepared as a 36% by mass aqueous solution. Adding into gelatinized starch, and mixing at 65deg.C for 30min; adding 0.4g of potassium persulfate, and reacting for 3 hours at 65 ℃ to obtain a viscous starch graft copolymer; drying at 105 deg.c to eliminate water and crushing to obtain powdered starch graft copolymer. Dispersing starch graft copolymer powder in 620ml butanol, stirring thoroughly for 30min; adding 36g of montmorillonite, mixing and re-dispersing for 30min; 3g of gamma-ureidopropyltriethoxysilane are added and reacted at 50℃for 3h. After the reaction, separating and removing the organic solvent, drying for 13 hours at 90 ℃ and crushing to obtain the plugging agent.
Comparative example 1
40g of corn starch is weighed and added into deionized water to prepare a starch suspension with the mass fraction of 15%. Stirring at 90deg.C for 60min to obtain gelatinized starch, drying at 110deg.C for removing water, and pulverizing to obtain powdery starch. Dispersing powdery starch in 300mL ethyl acetate, and fully stirring and dispersing for 30min; adding 30g of kaolinite, mixing and re-dispersing for 30min; 5g of gamma-chloropropyl trimethoxysilane are added and reacted for 4h at 45 ℃. After the reaction, separating and removing the organic solvent, drying for 8 hours at 110 ℃, and crushing to obtain the plugging agent.
Comparative example 2
40g of corn starch is weighed and added into deionized water to prepare a starch suspension with the mass fraction of 15%. Stirring at 90deg.C for 60min to obtain gelatinized starch; then, 30g of methacryloyloxyethyl-N, N-dimethylpropanesulfonate was weighed and prepared as a 50% by mass aqueous solution. Adding into gelatinized starch, and mixing at 70deg.C for 30min; adding 0.56g of potassium persulfate, and reacting for 3 hours at 70 ℃ to obtain a viscous starch graft copolymer; drying and dewatering at 110 ℃, and crushing to obtain the powdery starch graft copolymer. Dispersing the powdery starch graft copolymer in 300mL of ethyl acetate, and fully stirring and dispersing for 30min; adding 30g of kaolinite, mixing and re-dispersing for 30min; the reaction was carried out at 45℃for 4h. After the reaction, separating and removing the organic solvent, drying for 8 hours at 110 ℃, and crushing to obtain the plugging agent.
Samples of the examples and the comparative examples were taken, and the pressure bearing capacity test was performed using a QD-2 type plugging device with an addition of 5wt% and using different slit plates. The test results are shown in tables 1 and 2. The experimental slurry is mixed salt water-based slurry, and the preparation method comprises the following steps: 40g of test soil is weighed and added into 1000mL of water, 1.4g of anhydrous sodium carbonate is added, and 100g of NaCl and 50g of CaCl are added after stirring for 20min 2 And (5) sealing and curing for 24 hours at room temperature for standby. Before testing the bearing capacity, 350mL of base slurry is added with 5wt% plugging agent, stirred for 20min, then added into an aging kettle, rolled and aged for 16h at 160 ℃, cooled, taken out and stirred for 20min, and then tested for the bearing capacity.
Table 1 results of test of pressure bearing ability of sample on 1mm slit plate
| Sequence number | Sample of | Pressure bearing capacity/MPa |
| 1 | Example 1 | 5.3 |
| 2 | Example 2 | 5.8 |
| 3 | Example 3 | 4.5 |
| 4 | Example 4 | 5.2 |
| 5 | Example 5 | 4.6 |
| 6 | Example 6 | 4.7 |
| 7 | Comparative example 1 | 2.1 |
| 8 | Comparative example 2 | 0.7 |
Table 2 results of test of the bearing ability of the sample in the 3mm slit plate
| Sequence number | Sample of | Pressure bearing capacity/MPa |
| 1 | Example 1 | 5.1 |
| 2 | Example 2 | 5.6 |
| 3 | Example 3 | 4.2 |
| 4 | Example 4 | 5.0 |
| 5 | Example 5 | 4.3 |
| 6 | Example 6 | 4.5 |
| 7 | Comparative example 1 | 1.7 |
| 8 | Comparative example 2 | 0.5 |
Claims (33)
1. A plugging agent comprising structural unit a, structural unit B and structural unit D, wherein structural units a and D form a copolymer via a cross-linking agent;
the structural unit A is starch;
the structural unit B is a vinyl monomer-containing structural unit;
the structural unit D is a clay mineral unit;
the preparation method of the plugging agent comprises the following steps:
(1) Mixing starch with water, and uniformly mixing to obtain gelatinized starch;
(2) Mixing vinyl-containing monomer with water, and uniformly mixing to obtain a vinyl-containing monomer aqueous solution;
(3) Mixing the vinyl monomer-containing aqueous solution obtained in the step (2) with the gelatinized starch obtained in the step (1), adding an initiator after uniformly mixing, and reacting to obtain a starch graft copolymer;
(4) The starch graft copolymer obtained in the step (3) is dried and crushed to obtain powdery starch graft copolymer;
(5) Dispersing the powdery starch graft copolymer obtained in the step (4) into an organic solvent, then adding clay mineral and a cross-linking agent, and separating and drying after the reaction is completed to obtain a plugging agent;
the vinyl-containing monomer is water-soluble vinyl monomer, and is one or more of cationic monomer, anionic monomer, nonionic monomer and zwitterionic monomer; the zwitterionic monomer is one or more of methacryloxyethyl-N, N-dimethyl propane sulfonate, N-dimethyl allylamine propane sulfonate, 4-vinyl pyridine propane sulfonate, N-methyl diallyl propane sulfonate and N-methyl diallyl butane sulfonate; the cationic monomer is one or more of methacryloyloxyethyl trimethyl ammonium chloride, acryloyloxyethyl dimethylbenzyl ammonium chloride, dimethyl diallyl ammonium chloride and diethyl diallyl ammonium chloride; the anionic monomer is one or more of acrylic acid, 2-methyl-2-acrylamidopropane sulfonic acid, fumaric acid, sodium allylsulfonate and sodium 2-acryloyloxyisopentene sulfonate; the nonionic monomer is one or more of N-vinyl pyrrolidone, acrylonitrile, vinyl formamide and vinyl acetamide; the cross-linking agent is a silane coupling agent, and the silane coupling agent is one or more of gamma-chloropropyl trichlorosilane, gamma-chloropropyl methyl dichlorosilane, gamma-chloropropyl trimethoxysilane, gamma-chloropropyl triethoxysilane, chloromethyl triethoxysilane, gamma-aminopropyl trimethoxysilane, gamma- (beta-aminoethyl) aminopropyl trimethoxysilane, gamma-ureidopropyl triethoxysilane and aniline methyl trimethoxysilane.
2. The plugging agent of claim 1, wherein the structural unit A is present in an amount of 20 to 65wt%, the structural unit B is present in an amount of 12 to 55wt%, the structural unit D is present in an amount of 12 to 55wt%, and the crosslinking agent is present in an amount of 0.5 to 10wt%, based on the total amount of the plugging agent.
3. The plugging agent of claim 1, wherein the plugging agent has a pressure-bearing capacity of not less than 4MPa.
4. The plugging agent according to claim 1, wherein the starch is one or more of mung bean starch, tapioca starch, sweet potato starch, wheat starch, water chestnut starch, lotus root starch, and corn starch.
5. Plugging agent according to claim 1 or 4, wherein the starch is corn starch and/or potato starch.
6. The plugging agent of claim 1, wherein the zwitterionic monomer is N-methyldiallyl propane sulfonate; the cationic monomer is dimethyl diallyl ammonium chloride; the anionic monomer is 2-methyl-2-acrylamidopropane sulfonic acid; the nonionic monomer is N-vinyl pyrrolidone.
7. The plugging agent according to claim 1, wherein the silane coupling agent is one or more of gamma-chloropropyl trichlorosilane, gamma-chloropropyl trimethoxysilane, gamma-aminopropyl triethoxysilane, and gamma-aminopropyl trimethoxysilane.
8. The plugging agent of claim 7, wherein the silane coupling agent is gamma-chloropropyl trichlorosilane and/or gamma-chloropropyl trimethoxysilane.
9. The plugging agent according to claim 1, wherein the clay mineral is one or more of kaolinite, montmorillonite, illite, sepiolite and attapulgite.
10. The plugging agent of claim 1 or 9, wherein the clay mineral is montmorillonite.
11. A method of preparing the plugging agent of any one of claims 1-10, the method comprising:
(1) Mixing starch with water, and uniformly mixing to obtain gelatinized starch;
(2) Mixing vinyl-containing monomer with water, and uniformly mixing to obtain a vinyl-containing monomer aqueous solution;
(3) Mixing the vinyl monomer-containing aqueous solution obtained in the step (2) with the gelatinized starch obtained in the step (1), adding an initiator after uniformly mixing, and reacting to obtain a starch graft copolymer;
(4) The starch graft copolymer obtained in the step (3) is dried and crushed to obtain powdery starch graft copolymer;
(5) Dispersing the powdery starch graft copolymer obtained in the step (4) into an organic solvent, then adding clay mineral and a cross-linking agent, and separating and drying after the reaction is completed to obtain a plugging agent;
the vinyl-containing monomer is water-soluble vinyl monomer, and is one or more of cationic monomer, anionic monomer, nonionic monomer and zwitterionic monomer; the cross-linking agent is a silane coupling agent.
12. The process for producing a plugging agent according to claim 11, wherein the mixing temperature in the step (1) is 50 to 100 ℃.
13. The process for producing a plugging agent according to claim 11 or 12, wherein the mixing temperature in the step (1) is 80 to 95 ℃.
14. The method for producing a plugging agent according to claim 11, wherein the mass fraction of starch in the gelatinized starch in the step (1) is 5 to 20wt%.
15. The method for preparing a plugging agent according to claim 11, wherein the starch in the step (1) is one or more of mung bean starch, tapioca starch, sweet potato starch, wheat starch, water chestnut starch, lotus root starch and corn starch.
16. The process for producing a plugging agent according to claim 11 or 15, wherein the starch in the step (1) is corn starch and/or potato starch.
17. The process for producing a plugging agent according to claim 11, wherein the aqueous solution of a vinyl-containing polymer monomer in the step (2) has a mass fraction of 30 to 60% by weight.
18. The process for producing a plugging agent according to claim 11, wherein the mixing temperature in the step (3) is 40 to 90℃and the reaction temperature is 50 to 80 ℃.
19. The method for producing a plugging agent according to claim 11, wherein the initiator in the step (3) is one or more of potassium persulfate, sodium persulfate and ammonium persulfate; the initiator is used in an amount of 0.5 to 1.5wt% based on the total mass of the starch and the vinyl-containing monomer.
20. The process for producing a plugging agent according to claim 11, wherein the ratio of the aqueous vinyl-containing monomer solution obtained in the step (2) to the gelatinized starch obtained in the step (1) in the step (3) is 1: 4-2: 1.
21. the process for producing a plugging agent according to claim 11, wherein the drying in the step (4) is carried out at 60 to 120℃for 8 to 16 hours.
22. The method for producing a plugging agent according to claim 11, wherein the organic solvent in the step (5) is an organic solvent which is insoluble in the swollen starch but soluble in the crosslinking agent.
23. The method for producing a plugging agent according to claim 11 or 22, wherein the organic solvent in the step (5) is one or more of methanol, ethanol, propanol, butanol, methyl formate, ethyl acetate, ethyl formate, methyl acetate, butyl acetate.
24. The process for producing a plugging agent according to claim 11, wherein the amount of the organic solvent used in the step (5) is 2 to 8 times the total mass of the starch and the vinyl-containing monomer.
25. The process for producing a plugging agent according to claim 11, wherein the reaction temperature of adding the crosslinking agent in the step (5) is 30 to 70 ℃.
26. The process for producing a plugging agent according to claim 11, wherein the drying in the step (5) is carried out at 60 to 120℃for 8 to 16 hours.
27. A drilling fluid comprising the plugging agent of any one of claims 1-10 in an amount of 0.5-20 wt% based on the total weight of the drilling fluid.
28. The drilling fluid of claim 27, wherein the plugging agent is present in an amount of 2 to 10wt%, based on the total weight of the drilling fluid.
29. The drilling fluid of claim 27, wherein the plugging agent is present in an amount of 3 to 7wt%, based on the total weight of the drilling fluid.
30. Use of a plugging agent according to any one of claims 1-10 in a drilling process.
31. The use according to claim 30, wherein the plugging agent is added in an amount of 0.1 to 5wt%.
32. The use according to claim 30, wherein the plugging agent is added in an amount of 0.5 to 5wt%.
33. The use according to claim 30, wherein the plugging agent is present in an amount of 1 to 5wt%.
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