CN114479782A - Plugging agent and preparation method and application thereof - Google Patents
Plugging agent and preparation method and application thereof Download PDFInfo
- Publication number
- CN114479782A CN114479782A CN202011166408.8A CN202011166408A CN114479782A CN 114479782 A CN114479782 A CN 114479782A CN 202011166408 A CN202011166408 A CN 202011166408A CN 114479782 A CN114479782 A CN 114479782A
- Authority
- CN
- China
- Prior art keywords
- starch
- plugging agent
- gamma
- agent according
- vinyl
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000002360 preparation method Methods 0.000 title claims abstract description 38
- 229920002472 Starch Polymers 0.000 claims abstract description 108
- 239000008107 starch Substances 0.000 claims abstract description 104
- 235000019698 starch Nutrition 0.000 claims abstract description 104
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 98
- 239000000178 monomer Substances 0.000 claims abstract description 45
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 28
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 26
- 239000002734 clay mineral Substances 0.000 claims abstract description 17
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 15
- 239000007822 coupling agent Substances 0.000 claims abstract description 12
- 229920001577 copolymer Polymers 0.000 claims abstract description 3
- 229920000578 graft copolymer Polymers 0.000 claims description 29
- 238000002156 mixing Methods 0.000 claims description 29
- 238000006243 chemical reaction Methods 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 238000001035 drying Methods 0.000 claims description 20
- 238000005553 drilling Methods 0.000 claims description 17
- 239000003960 organic solvent Substances 0.000 claims description 17
- 239000000463 material Substances 0.000 claims description 16
- OXYZDRAJMHGSMW-UHFFFAOYSA-N 3-chloropropyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)CCCCl OXYZDRAJMHGSMW-UHFFFAOYSA-N 0.000 claims description 15
- 229920002261 Corn starch Polymers 0.000 claims description 15
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 15
- 239000007864 aqueous solution Substances 0.000 claims description 15
- 239000008120 corn starch Substances 0.000 claims description 15
- 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 15
- 229910052901 montmorillonite Inorganic materials 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 14
- OOXSLJBUMMHDKW-UHFFFAOYSA-N trichloro(3-chloropropyl)silane Chemical group ClCCC[Si](Cl)(Cl)Cl OOXSLJBUMMHDKW-UHFFFAOYSA-N 0.000 claims description 13
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 12
- 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 11
- 229910052622 kaolinite Inorganic materials 0.000 claims description 11
- 239000012530 fluid Substances 0.000 claims description 10
- 229920001592 potato starch Polymers 0.000 claims description 10
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 9
- 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
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims description 8
- 229910052900 illite Inorganic materials 0.000 claims description 8
- 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 8
- 238000006116 polymerization reaction Methods 0.000 claims description 8
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 claims description 7
- 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 7
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-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
- 239000003999 initiator Substances 0.000 claims description 6
- 239000002245 particle Substances 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
- LVNLBBGBASVLLI-UHFFFAOYSA-N 3-triethoxysilylpropylurea Chemical compound CCO[Si](OCC)(OCC)CCCNC(N)=O LVNLBBGBASVLLI-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
- 239000004113 Sepiolite Substances 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
- 229960000892 attapulgite Drugs 0.000 claims description 5
- 125000001570 methylene group Chemical group [H]C([H])([*:1])[*:2] 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 229910052625 palygorskite Inorganic materials 0.000 claims description 5
- 229910052624 sepiolite Inorganic materials 0.000 claims description 5
- 235000019355 sepiolite Nutrition 0.000 claims description 5
- 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
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 4
- KSCAZPYHLGGNPZ-UHFFFAOYSA-N 3-chloropropyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)CCCCl KSCAZPYHLGGNPZ-UHFFFAOYSA-N 0.000 claims description 4
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-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
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 4
- 240000001085 Trapa natans Species 0.000 claims description 4
- 150000004645 aluminates Chemical class 0.000 claims description 4
- 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 4
- 125000000129 anionic group Chemical group 0.000 claims description 4
- 125000002091 cationic group Chemical group 0.000 claims description 4
- ZDOBWJOCPDIBRZ-UHFFFAOYSA-N chloromethyl(triethoxy)silane Chemical compound CCO[Si](CCl)(OCC)OCC ZDOBWJOCPDIBRZ-UHFFFAOYSA-N 0.000 claims description 4
- 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 4
- TZIHFWKZFHZASV-UHFFFAOYSA-N methyl formate Chemical compound COC=O TZIHFWKZFHZASV-UHFFFAOYSA-N 0.000 claims description 4
- 235000009165 saligot 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
- 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
- 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
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 3
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-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
- 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 claims description 2
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 claims description 2
- 229910002808 Si–O–Si Inorganic materials 0.000 claims description 2
- JXASPPWQHFOWPL-UHFFFAOYSA-N Tamarixin Natural products C1=C(O)C(OC)=CC=C1C1=C(OC2C(C(O)C(O)C(CO)O2)O)C(=O)C2=C(O)C=C(O)C=C2O1 JXASPPWQHFOWPL-UHFFFAOYSA-N 0.000 claims description 2
- PBIMORRGPOOPMC-UHFFFAOYSA-N [Na].C(C=C)(=O)OC(=C)C(C)C Chemical compound [Na].C(C=C)(=O)OC(=C)C(C)C PBIMORRGPOOPMC-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
- CADWTSSKOVRVJC-UHFFFAOYSA-N benzyl(dimethyl)azanium;chloride Chemical compound [Cl-].C[NH+](C)CC1=CC=CC=C1 CADWTSSKOVRVJC-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
- 125000004432 carbon atom Chemical group C* 0.000 claims description 2
- WBJINCZRORDGAQ-UHFFFAOYSA-N formic acid ethyl ester Natural products CCOC=O WBJINCZRORDGAQ-UHFFFAOYSA-N 0.000 claims description 2
- NUKZAGXMHTUAFE-UHFFFAOYSA-N hexanoic acid methyl ester Natural products CCCCCC(=O)OC NUKZAGXMHTUAFE-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
- KCXFHTAICRTXLI-UHFFFAOYSA-N propane-1-sulfonic acid Chemical compound CCCS(O)(=O)=O KCXFHTAICRTXLI-UHFFFAOYSA-N 0.000 claims description 2
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 2
- 230000008961 swelling Effects 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
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 238000003756 stirring Methods 0.000 description 17
- 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
- 238000012360 testing method Methods 0.000 description 7
- 239000000835 fiber Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- -1 polypropylene Polymers 0.000 description 5
- 239000002002 slurry Substances 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- 240000007049 Juglans regia Species 0.000 description 3
- 235000009496 Juglans regia Nutrition 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 3
- 230000002265 prevention Effects 0.000 description 3
- 238000010298 pulverizing process Methods 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
- 230000032683 aging Effects 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
- 238000005516 engineering process Methods 0.000 description 2
- 239000002657 fibrous material Substances 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- 239000010902 straw Substances 0.000 description 2
- 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
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-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
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical compound [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 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
- 230000000903 blocking effect Effects 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- 229920002301 cellulose acetate Polymers 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000002708 enhancing effect Effects 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
- 238000002329 infrared spectrum Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000019426 modified starch Nutrition 0.000 description 1
- VNBLTKHUCJLFSB-UHFFFAOYSA-N n-(trimethoxysilylmethyl)aniline Chemical compound CO[Si](OC)(OC)CNC1=CC=CC=C1 VNBLTKHUCJLFSB-UHFFFAOYSA-N 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 239000011118 polyvinyl acetate Substances 0.000 description 1
- 229920002689 polyvinyl acetate Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 229910052895 riebeckite Inorganic materials 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 238000001308 synthesis method Methods 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 and 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-containing monomer structural unit; the structural unit C is a clay mineral unit. The preparation method of the plugging agent combines organic starch and inorganic clay minerals together by using a coupling agent. 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 oil exploitation, and particularly relates to a plugging material and a preparation method thereof.
Background
The well leakage is a technical problem which exists in the processes of well drilling, well cementing, well logging and well repairing, and can cause the drilling fluid to leak into a leakage channel from a well hole, so that not only is a large amount of mud and leakage blocking materials consumed, but also serious accidents such as well collapse, drill sticking, blowout, even well hole abandonment and the like can be caused, and huge economic loss is caused. The plugging material is necessary in the process of well drilling and leakage prevention, and the success rate of well drilling, leakage prevention and leakage prevention directly depends on the quality of the performance of the plugging material. Therefore, the research on the plugging material has very important significance.
At present, the research on the leakage-proof and plugging technology of the drilling well is developed rapidly at home and abroad, various solutions are provided, and a series of novel plugging materials and leakage-proof and plugging systems are developed and developed simultaneously. Bridging plugging is a plugging technology which is most widely applied and has the characteristics of itself, inert materials with different shapes and sizes are mixed in a drilling fluid system according to a certain proportion and then injected into a leaking stratum section for plugging, and the requirement on a material matching level is high. The existing commonly used bridging particles mainly comprise walnut shells and other rigid particles and sawdust, bagasse and other fiber materials, wherein the walnut shells and other rigid particles have the characteristics of high pressure bearing capacity and difficult deformation, but are easy to carbonize under the high-temperature condition; and the fiber materials such as sawdust and bagasse are easy to lose efficacy under high pressure conditions, so that the conventional plugging material and well slurry cannot form an effective plugging layer. Other types of plugging materials also generally have the problems of high price, complex plugging process, small improvement range of the pressure-bearing capacity of the leaking layer, poor environmental protection index 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. The problems of poor bearing capacity and plugging effect of the plugging agent, easy leakage, high production cost and low cost performance are effectively solved. CN 201910318778. X discloses an acid-soluble pressure-bearing plugging agent for drilling fluid and a preparation method thereof. Consists of crop straw extract fiber, polyester fiber, cellulose acetate, glass fiber, asbestos fiber, cotton-flax plant fiber, rock-making mineral powder, alginate, dimethyl diallyl ammonium chloride, polyvinyl acetate, n-octyl alpha-cyanoacrylate, diatomite and a 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 are well realized.
Disclosure of Invention
Aiming at the defects of the prior art, the invention mainly aims to provide the plugging agent, the preparation method and the application thereof.
The invention provides a plugging agent, which comprises a structural unit A, a structural unit B and a structural unit D, wherein the structural units A and D form a copolymer through a crosslinking agent;
the structural unit A is starch;
the structural unit B is a vinyl-containing monomer 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
(ii) a Wherein R is1And R3Is a monomer side chain structure except a vinyl structure in a vinyl polymerization monomer, R2Is CH-or N (nitrogen).
R is a methylene chain in the coupling agent, and Si-O-Si forms a covalent bond 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), specifically-CH2-、-CH2CH2-、-CH2CH2CH2-、-CH2CH2CH2-、-CH2CH2CH2CH2-、-CH2CH2CH2 CH2CH2-；
m is the polymerization degree of a starch structural unit, x is the polymerization degree of a vinyl monomer, and m + x = 800-1600.
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 0.5-10 wt%.
In the plugging agent, the pressure bearing capacity of the plugging agent is not lower than 4 MPa.
In the plugging agent, the starch can be one or more of mung bean starch, cassava starch, sweet potato starch, wheat starch, water caltrop starch, lotus root starch and corn starch, and 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; the zwitterionic monomer is one or more of methacryloyloxyethyl-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 methacryloyloxyethyl trimethyl ammonium chloride (DMC), acryloyloxyethyl trimethyl ammonium chloride (DAC), acryloyloxyethyl dimethyl benzyl ammonium chloride (DBC), dimethyl diallyl ammonium chloride (DMDAAC) and diethyl diallyl ammonium chloride (DEDAAC), and is preferably dimethyl diallyl ammonium chloride. The anionic monomer is one or more of AA (acrylic acid), 2-methyl-2-acrylamido propanesulfonic Acid (AMPS), Fumaric Acid (FA), sodium allyl sulfonate (SSS) and sodium 2-acryloyloxy isopentene sulfonate (AOIAS), and preferably is 2-methyl-2-acrylamido propanesulfonic acid. The nonionic monomer is one or more of N-vinyl pyrrolidone (NVP), Acrylonitrile (AN), vinyl formamide (NVF) and vinyl acetamide (NVA), and is preferably N-vinyl pyrrolidone.
In the plugging agent, 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 gamma-chloropropyltrichlorosilane, gamma-chloropropylmethyldichlorosilane, gamma-chloropropyltrimethoxysilane, gamma-chloropropyltriethoxysilane, chloromethyltriethoxysilane, gamma-aminopropyltriethoxysilane, gamma-aminopropyltrimethoxysilane, the material is one or more of gamma- (beta-aminoethyl) aminopropyltrimethoxysilane, gamma-ureidopropyltriethoxysilane and aniline methyl trimethoxysilane, preferably one or more of gamma-chloropropyltrichlorosilane, gamma-chloropropyltrimethoxysilane, gamma-aminopropyltriethoxysilane and gamma-aminopropyltrimethoxysilane, and further preferably gamma-chloropropyltrichlorosilane and/or gamma-chloropropyltrimethoxysilane.
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 a 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) drying and crushing the starch graft copolymer obtained in the step (3) to obtain a powdery starch graft copolymer;
(5) and (3) dispersing the powdery starch graft copolymer obtained in the step (4) into an organic solvent, then adding clay minerals and a cross-linking agent, and after the reaction is finished, separating and drying to obtain the plugging agent.
In the preparation method of the plugging agent, the mixing temperature in the step (1) is 50-100 ℃, and 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 5-20 wt%.
In the preparation method of the plugging agent, the starch in the step (1) is one or more of mung bean starch, cassava starch, sweet potato starch, wheat starch, water caltrop starch, lotus root starch and corn starch, and 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 amount of the initiator is 0.5-1.5 wt% of 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) in the step (3) to the gelatinized starch obtained in the step (1) is 1: 4-2: 1.
in the preparation method of the plugging agent, the drying condition in the step (4) is drying for 8-16 hours at the temperature of 60-120 ℃.
In the preparation method of the plugging agent, any one of the conventional ways capable of crushing the solid-phase material, such as a crusher, can be adopted for crushing in the step (4), and the specific conditions of crushing can be selected by those skilled in the art according to the actual needs of the product.
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 cross-linking agent, and specifically 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 gamma-chloropropyltrichlorosilane, gamma-chloropropylmethyldichlorosilane, gamma-chloropropyltrimethoxysilane, gamma-chloropropyltriethoxysilane, chloromethyltriethoxysilane, gamma-aminopropyltriethoxysilane, gamma-aminopropyltrimethoxysilane, the material is one or more of gamma- (beta-aminoethyl) aminopropyltrimethoxysilane, gamma-ureidopropyltriethoxysilane and aniline methyl trimethoxysilane, preferably one or more of gamma-chloropropyltrichlorosilane, gamma-chloropropyltrimethoxysilane, gamma-aminopropyltriethoxysilane and gamma-aminopropyltrimethoxysilane, and further preferably gamma-chloropropyltrichlorosilane and/or gamma-chloropropyltrimethoxysilane.
In the preparation method of the plugging agent, the clay mineral in the step (5) 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 of the 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 adopt one or more of standing, layering and filtering, centrifugal separation, spray drying and direct powdering and the like.
In the preparation method of the plugging agent, the drying condition in the step (5) is drying for 8-16 hours at the temperature of 60-120 ℃.
The third aspect of the invention provides a drilling fluid, which comprises the plugging agent, wherein the content of the plugging agent is 0.5-20 wt%, preferably 2-10 wt%, and more preferably 3-7 wt% 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 microcracks, prevents a large amount of filtrate from permeating into a stratum, reduces the filtrate loss and has good plugging effect. .
The fourth aspect of the invention provides the use of the plugging agent in a drilling process.
When the plugging agent is used in a 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 provided by the invention have the following advantages:
1. the plugging agent provided by the invention uses vinyl polymerization monomer grafted modified starch, so that the starch has functionality, and the temperature resistance, salt resistance and calcium resistance of the plugging agent in drilling fluid are improved while the plugging characteristic of the plugging agent is ensured, wherein the temperature resistance is not lower than 160 ℃, the salt resistance can reach saturation, and the calcium resistance is not less than 5 wt%.
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 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 the clay minerals of the inert part with the stratum, thereby enhancing the interface effect and further improving the pressure bearing capacity. The clay mineral has the same lithology as the stratum, and the silicon-oxygen containing structure can be further condensed at high temperature and high pressure to form a bonding structure, so that the plugging and bearing capacity at 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 non-toxic 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 really achieves the aims of environment-friendly raw materials, production and application.
Drawings
FIG. 1 is an infrared spectrum of the plugging agent prepared in example 1 of the present invention.
Detailed Description
The plugging agent, the preparation method and the application thereof are further described by the following specific examples, but the invention is not limited thereto.
Example 1
Weighing 40g of corn starch, adding the corn starch into deionized water, and preparing into starch suspension with the mass fraction of 15%. Stirring at 90 deg.C for 60min to obtain gelatinized starch; then 30g of methacryloyloxyethyl-N, N-dimethyl propane sulfonate is weighed and prepared into an aqueous solution with the mass fraction of 50%. Adding into gelatinized starch, and mixing at 70 deg.C for 30 min; adding 0.56g of potassium persulfate, and reacting at 70 ℃ for 3h to obtain a viscous starch graft copolymer; drying at 110 deg.C to remove water, and pulverizing to obtain powdered starch graft copolymer. Dispersing the powdery starch graft copolymer in 300mL ethyl acetate, and fully stirring and dispersing for 30 min; then is added to30g of kaolinite, and mixing and dispersing for 30 min; 5g of gamma-chloropropyltrimethoxysilane were added and the reaction was carried out at 45 ℃ for 4 h. After the reaction, the organic solvent is separated and removed, the mixture is dried for 8 hours at the temperature of 110 ℃ and crushed to obtain the plugging agent. The infrared spectrogram of the plugging agent is shown in figure 1, and 3434cm can be seen from the analysis of figure 1-1Is a characteristic peak of OH in starch, 2931 cm-1、2846 cm-1And 1386 cm-1is-CH-, -CH2-、CH3Characteristic peak, 1640 cm-1Is a C = O characteristic peak in the monomer, 1048 cm-1Is a characteristic peak of Si-O-C.
Example 2
20g of potato starch is weighed and added into deionized water to prepare starch suspension with the mass fraction of 8%. Stirring at 85 deg.C for 80min to obtain gelatinized starch; then 35g of 2-methyl-2-acrylamidopropanesulfonic acid was weighed out and prepared into an aqueous solution with a mass fraction of 52%. Adding into gelatinized starch, and mixing at 60 deg.C for 30 min; adding 0.61g of ammonium persulfate, and reacting for 4 hours at 60 ℃ to obtain a sticky starch graft copolymer; drying and dewatering at 120 deg.c and crushing to obtain powdered starch graft copolymer. Dispersing starch graft copolymer powder in 450mL of methanol, and fully stirring and dispersing for 30 min; adding 15g of montmorillonite, mixing and dispersing for 30 min; 4g of gamma-chloropropyltrichlorosilane is added to react for 4 hours at 55 ℃. After the reaction, the organic solvent is separated and removed, dried for 12 hours at the temperature of 90 ℃ and crushed 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 80 deg.C for 90min to obtain gelatinized starch; then 15g of methacryloyloxyethyl trimethyl ammonium chloride is weighed and prepared into an aqueous solution with the mass fraction of 30%. Adding into gelatinized starch, and mixing at 55 deg.C for 30 min; adding 0.62g of sodium persulfate, and reacting for 4 hours at 55 ℃ to obtain a sticky 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 fully stirring and dispersing for 30 min; adding 27g of montmorillonite, mixing and dispersing for 30 min; 2.5g of gamma-aminopropyltriethoxysilane was added and reacted at 50 ℃ for 3 h. After the reaction, the organic solvent is separated and removed, dried for 10 hours at the temperature of 120 ℃ and crushed to obtain the plugging agent.
Example 4
25g of mung bean starch is weighed and added into deionized water to prepare starch suspension with the mass fraction of 5%. Stirring at 90 deg.C for 70min to obtain gelatinized starch; then weighing 40g N-vinyl pyrrolidone to prepare an aqueous solution with the mass fraction of 60%. Adding into gelatinized starch, and mixing at 75 deg.C for 30 min; adding 0.33g of potassium persulfate, and reacting for 2 hours at 75 ℃ to obtain a viscous starch graft copolymer; drying and dewatering at 70 ℃, and crushing to obtain the powdery starch graft copolymer. Dispersing starch graft copolymer powder in 420ml butyl acetate, fully stirring and dispersing for 30 min; adding 10g attapulgite, mixing and dispersing for 30 min; 4.5g of anilinomethyltrimethoxysilane were added and the reaction was carried out at 60 ℃ for 3 h. After the reaction, the organic solvent is separated and removed, dried for 9 hours at the temperature of 100 ℃ and crushed to obtain the plugging agent.
Example 5
35g of lotus root starch is weighed and added into deionized water to prepare starch suspension with the mass fraction of 16%. Stirring at 93 deg.C for 60min to obtain gelatinized starch; then 10g of sodium allylsulfonate is weighed to prepare an aqueous solution with the mass fraction of 42%. Adding into gelatinized starch, and mixing at 80 deg.C for 30 min; adding 0.68g of sodium persulfate, and reacting at 80 ℃ for 2.5h 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 fully stirring and dispersing for 30 min; adding 40g of sepiolite, mixing and dispersing for 30 min; 1g of gamma-chloropropyltrimethoxysilane was added and the reaction was carried out at 55 ℃ for 2 h. After the reaction, the organic solvent is separated and removed, dried for 11 hours at the temperature of 95 ℃ and crushed to obtain the plugging agent.
Example 6
22g of corn starch is weighed and added into deionized water to prepare starch suspension with the mass fraction of 10%. Stirring at 88 deg.C for 75min to obtain gelatinized starch; then 18g of 4-vinylpyridine propanesulfonate is weighed and prepared into an aqueous solution with the mass fraction of 36%. Adding into gelatinized starch, and mixing at 65 deg.C for 30 min; adding 0.4g of potassium persulfate, and reacting at 65 ℃ for 3 hours to obtain a viscous starch graft copolymer; drying at 105 ℃ to remove water, and crushing to obtain the powdery starch graft copolymer. Dispersing starch graft copolymer powder in 620ml butanol, fully stirring and dispersing for 30 min; adding 36g of montmorillonite, mixing and dispersing for 30 min; 3g of gamma-ureidopropyltriethoxysilane was added and reacted at 50 ℃ for 3 hours. After the reaction, the organic solvent is separated and removed, dried for 13 hours at the temperature of 90 ℃ and crushed to obtain the plugging agent.
Comparative example 1
Weighing 40g of corn starch, adding the corn starch into deionized water, and preparing into starch suspension with the mass fraction of 15%. Stirring at 90 deg.C for 60min to obtain gelatinized starch, drying at 110 deg.C to remove water, and pulverizing to obtain powdered starch. Dispersing powdery starch in 300mL ethyl acetate, and fully stirring and dispersing for 30 min; then 30g of kaolinite is added, and the mixture is mixed and dispersed for 30 min; 5g of gamma-chloropropyltrimethoxysilane were added and the reaction was carried out at 45 ℃ for 4 h. After the reaction, the organic solvent is separated and removed, the mixture is dried for 8 hours at the temperature of 110 ℃ and crushed to obtain the plugging agent.
Comparative example 2
Weighing 40g of corn starch, adding the corn starch into deionized water, and preparing into a starch suspension with the mass fraction of 15%. Stirring at 90 deg.C for 60min to obtain gelatinized starch; then 30g of methacryloyloxyethyl-N, N-dimethyl propane sulfonate is weighed and prepared into an aqueous solution with the mass fraction of 50%. Adding into gelatinized starch, and mixing at 70 deg.C for 30 min; adding 0.56g of potassium persulfate, and reacting at 70 ℃ for 3h to obtain a viscous starch graft copolymer; drying at 110 deg.C to remove water, and pulverizing to obtain powdered starch graft copolymer. Dispersing the powdery starch graft copolymer in 300mL ethyl acetate, and fully stirring and dispersing for 30 min; then 30g of kaolinite is added, and the mixture is mixed and dispersed for 30 min; the reaction was carried out at 45 ℃ for 4 h. After the reaction, the organic solvent is separated and removed, the mixture is dried for 8 hours at the temperature of 110 ℃ and crushed to obtain the plugging agent.
The samples of the examples and the comparative examples are taken, and a pressure bearing capacity test is carried out by using a QD-2 type leak stoppage instrument and selecting different gap plates under the condition that the adding amount is 5 weight percent. The test results are shown in tables 1 and 2. The experimental slurry is mixed saline water-based slurry, and the preparation method comprises the following steps: weighing 40g of test soil, adding the test soil into 1000mL of water, adding 1.4g of anhydrous sodium carbonate, stirring for 20min, and adding 100g of NaCl and 50g CaCl2And performing closed maintenance at room temperature for 24 hours for later use. Before testing the pressure-bearing capacity, 350mL of base slurry is added with 5wt% of plugging agent, stirred for 20min and then added into an aging kettle, rolling and aging are carried out for 16h at 160 ℃, and the base slurry is taken out after cooling and stirred for 20min and then the pressure-bearing capacity is tested.
TABLE 1 test result of pressure bearing capacity of sample in 1mm gap plate
| Serial number | Sample (I) | 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 test results of the pressure-bearing capacity of the sample in the 3mm gap plate
| Serial number | Sample (I) | 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 (29)
1. A plugging agent comprises a structural unit A, a structural unit B and a structural unit D, wherein the structural units A and D form a copolymer through a cross-linking agent;
the structural unit A is starch;
the structural unit B is a vinyl-containing monomer 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
(ii) a Wherein R is1And R3Is a monomer side chain structure except a vinyl structure in a vinyl polymerization monomer, R2Is CH-or N, R is a methylene chain in a coupling agent, and Si-O-Si forms a covalent bond with HO-Si in the clay mineral through Si; the number of carbon atoms in the methylene chain is an integer between 1 and 5, preferably an integer between 1 and 3;
m is the degree of polymerization of the starch structural unit, x is the degree of polymerization of the vinyl monomer, and m + x = 800-1600.
2. A plugging agent according to claim 1, wherein based on the total amount of the plugging agent, 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 C is 12-55wt%, and the content of the cross-linking agent is 0.5-10 wt%.
3. A plugging agent according to claim 1, wherein the methylene chain is-CH2-、-CH2CH2-、-CH2CH2CH2-、-CH2CH2CH2-、-CH2CH2CH2CH2-、-CH2CH2CH2 CH2CH2-。
4. A plugging agent according to claim 1, wherein the pressure-bearing capacity of the plugging agent is not lower than 4 MPa.
5. 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 caltrop starch, lotus root starch and corn starch, and preferably corn starch and/or potato starch.
6. The plugging agent according to claim 1, wherein the vinyl-containing monomer is a water-soluble vinyl monomer, and specifically is one or more of a cationic monomer, an anionic monomer, a nonionic monomer and a zwitterionic monomer.
7. A plugging agent according to claim 1, wherein the zwitterionic monomer is one or more of methacryloyloxyethyl-N, N-Dimethylpropanesulfonate (DMAPS), N-dimethylallylamine propanesulfonate (DAPS), 4-vinylpyridine propanesulfonate (VPPS), N-Methyldiallylpropylpropanesulfonate (MAPS), N-Methyldiallylbutanesulfonate (MABS), preferably N-methyldiallylpropylpropanesulfonate; the cationic monomer is one or more of methacryloyloxyethyl trimethyl ammonium chloride (DMC), acryloyloxyethyl trimethyl ammonium chloride (DAC), acryloyloxyethyl dimethyl benzyl ammonium chloride (DBC), dimethyl diallyl ammonium chloride (DMDAAC) and diethyl diallyl ammonium chloride (DEDAAC), and is preferably dimethyl diallyl ammonium chloride; the anionic monomer is one or more of AA (acrylic acid), 2-methyl-2-acrylamido propanesulfonic Acid (AMPS), Fumaric Acid (FA), sodium allyl sulfonate (SSS) and sodium 2-acryloyloxy isopentene sulfonate (AOIAS), and preferably is 2-methyl-2-acrylamido propanesulfonic acid; the nonionic monomer is one or more of N-vinyl pyrrolidone (NVP), Acrylonitrile (AN), vinyl formamide (NVF) and vinyl acetamide (NVA), and is preferably N-vinyl pyrrolidone.
8. The plugging agent according to claim 1, wherein the crosslinking agent is one or more of a silane coupling agent, a titanate coupling agent and an aluminate coupling agent, and is preferably a silane coupling agent.
9. A plugging agent according to claim 8, wherein the silane coupling agent is gamma-chloropropyltrichlorosilane, gamma-chloropropylmethyldichlorosilane, gamma-chloropropyltrimethoxysilane, gamma-chloropropyltriethoxysilane, chloromethyltriethoxysilane, gamma-aminopropyltriethoxysilane, gamma-aminopropyltrimethoxysilane, the material is one or more of gamma- (beta-aminoethyl) aminopropyltrimethoxysilane, gamma-ureidopropyltriethoxysilane and aniline methyl trimethoxysilane, preferably one or more of gamma-chloropropyltrichlorosilane, gamma-chloropropyltrimethoxysilane, gamma-aminopropyltriethoxysilane and gamma-aminopropyltrimethoxysilane, and further preferably gamma-chloropropyltrichlorosilane and/or gamma-chloropropyltrimethoxysilane.
10. The plugging agent according to claim 1, wherein the clay mineral is one or more of kaolinite, montmorillonite, illite, sepiolite and attapulgite, preferably kaolinite, montmorillonite and illite, and further preferably montmorillonite.
11. A preparation method of a plugging agent comprises the following steps:
mixing starch with water, and uniformly mixing to obtain gelatinized starch;
(2) mixing a 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) drying and crushing the starch graft copolymer obtained in the step (3) to obtain a powdery starch graft copolymer;
(5) and (3) dispersing the powdery starch graft copolymer obtained in the step (4) into an organic solvent, then adding clay minerals and a cross-linking agent, and after the reaction is finished, separating and drying to obtain the plugging agent.
12. The method for preparing a plugging agent according to claim 11, wherein the mixing temperature in the step (1) is 50-100 ℃, preferably 80-95 ℃.
13. The preparation method of the plugging agent according to claim 11, wherein the mass fraction of starch in the gelatinized starch in the step (1) is 5 to 20 wt%.
14. The preparation method of the 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 caltrop starch, lotus root starch and corn starch, and preferably corn starch and/or potato starch.
15. The method for preparing a plugging agent according to claim 11, wherein the mass fraction of the aqueous solution containing vinyl polymerization monomers in the step (2) is 30-60 wt%.
16. The method for preparing the plugging agent according to claim 11, wherein the mixing temperature in the step (3) is 40-90 ℃, and the reaction temperature is 50-80 ℃.
17. The preparation method of the 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 amount of the initiator is 0.5-1.5 wt% of the total mass of the starch and the vinyl-containing monomer.
18. A method for preparing a plugging agent according to claim 11, wherein the ratio of the amount of the vinyl-containing monomer 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.
19. the method for preparing a plugging agent according to claim 11, wherein the drying condition in the step (4) is drying at 60 to 120 ℃ for 8 to 16 hours.
20. The method for preparing a plugging agent according to claim 11, wherein the organic solvent in the step (5) is an organic solvent which can not dissolve the swelling starch but can dissolve the cross-linking agent, and is specifically one or more of methanol, ethanol, propanol, butanol, methyl formate, ethyl acetate, ethyl formate, methyl acetate and butyl acetate.
21. The preparation method of the plugging agent according to claim 11, wherein the amount of the organic solvent used in the step (5) is 2-8 times of the total mass of the starch and the vinyl-containing monomer.
22. The preparation method of the plugging agent according to claim 11, wherein the crosslinking agent in the step (5) is one or more of a silane coupling agent, a titanate coupling agent and an aluminate coupling agent, and is preferably a silane coupling agent.
23. A method for preparing a plugging agent according to claim 22, wherein the silane coupling agent is gamma-chloropropyltrichlorosilane, gamma-chloropropylmethyldichlorosilane, gamma-chloropropyltrimethoxysilane, gamma-chloropropyltriethoxysilane, chloromethyltriethoxysilane, gamma-aminopropyltriethoxysilane, gamma-aminopropyltrimethoxysilane, the material is one or more of gamma- (beta-aminoethyl) aminopropyltrimethoxysilane, gamma-ureidopropyltriethoxysilane and aniline methyl trimethoxysilane, preferably one or more of gamma-chloropropyltrichlorosilane, gamma-chloropropyltrimethoxysilane, gamma-aminopropyltriethoxysilane and gamma-aminopropyltrimethoxysilane, and further preferably gamma-chloropropyltrichlorosilane and/or gamma-chloropropyltrimethoxysilane.
24. The preparation method of the plugging agent according to claim 11, wherein the clay mineral in the step (5) is one or more of kaolinite, montmorillonite, illite, sepiolite and attapulgite, preferably kaolinite, montmorillonite and illite, and further preferably montmorillonite; the particle size of the clay mineral is not less than 200 meshes.
25. The preparation method of the plugging agent according to claim 11, wherein the reaction temperature of the adding of the cross-linking agent in the step (5) is 30-70 ℃.
26. The method for preparing a plugging agent according to claim 11, wherein the drying condition in the step (5) is drying at 60 to 120 ℃ for 8 to 16 hours.
27. A drilling fluid, which comprises the plugging agent as described in any one of claims 1 to 10, wherein the content of the plugging agent is 0.5 to 20wt%, preferably 2 to 10wt%, and more preferably 3 to 7wt% based on the total weight of the drilling fluid.
28. Use of a plugging agent according to any of claims 1-10 in a drilling process.
29. The use according to claim 28, wherein the plugging agent is added in an amount of 0.1 to 5wt%, preferably 0.5 to 5wt%, and more preferably 1 to 5 wt%.
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