CN117487081A - Environment-friendly polymer composite multielement copolymerization filtrate reducer and preparation method thereof - Google Patents
Environment-friendly polymer composite multielement copolymerization filtrate reducer and preparation method thereof Download PDFInfo
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- CN117487081A CN117487081A CN202311429169.4A CN202311429169A CN117487081A CN 117487081 A CN117487081 A CN 117487081A CN 202311429169 A CN202311429169 A CN 202311429169A CN 117487081 A CN117487081 A CN 117487081A
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- 239000000706 filtrate Substances 0.000 title claims abstract description 56
- 239000003638 chemical reducing agent Substances 0.000 title claims abstract description 53
- 239000002131 composite material Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 238000007334 copolymerization reaction Methods 0.000 title claims abstract description 17
- 229920000642 polymer Polymers 0.000 title claims abstract description 14
- 229920002472 Starch Polymers 0.000 claims abstract description 47
- 235000019698 starch Nutrition 0.000 claims abstract description 45
- 239000008107 starch Substances 0.000 claims abstract description 45
- 238000006243 chemical reaction Methods 0.000 claims abstract description 36
- 238000003756 stirring Methods 0.000 claims abstract description 28
- 239000000178 monomer Substances 0.000 claims abstract description 27
- 238000004132 cross linking Methods 0.000 claims abstract description 22
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 20
- 238000010438 heat treatment Methods 0.000 claims abstract description 19
- 239000011259 mixed solution Substances 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 16
- 239000003999 initiator Substances 0.000 claims abstract description 14
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 14
- MPNXSZJPSVBLHP-UHFFFAOYSA-N 2-chloro-n-phenylpyridine-3-carboxamide Chemical compound ClC1=NC=CC=C1C(=O)NC1=CC=CC=C1 MPNXSZJPSVBLHP-UHFFFAOYSA-N 0.000 claims abstract description 13
- MVBJSQCJPSRKSW-UHFFFAOYSA-N n-[1,3-dihydroxy-2-(hydroxymethyl)propan-2-yl]prop-2-enamide Chemical compound OCC(CO)(CO)NC(=O)C=C MVBJSQCJPSRKSW-UHFFFAOYSA-N 0.000 claims abstract description 13
- XFTALRAZSCGSKN-UHFFFAOYSA-M sodium;4-ethenylbenzenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C1=CC=C(C=C)C=C1 XFTALRAZSCGSKN-UHFFFAOYSA-M 0.000 claims abstract description 13
- 230000001105 regulatory effect Effects 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 9
- MLOKHANBEXWBKS-UHFFFAOYSA-N 3-triacetyloxysilylpropyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCCC[Si](OC(C)=O)(OC(C)=O)OC(C)=O MLOKHANBEXWBKS-UHFFFAOYSA-N 0.000 claims description 8
- 229920002261 Corn starch Polymers 0.000 claims description 8
- 239000008120 corn starch Substances 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 8
- 230000007935 neutral effect Effects 0.000 claims description 8
- JXUKBNICSRJFAP-UHFFFAOYSA-N triethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CCO[Si](OCC)(OCC)CCCOCC1CO1 JXUKBNICSRJFAP-UHFFFAOYSA-N 0.000 claims description 8
- LNOPIUAQISRISI-UHFFFAOYSA-N n'-hydroxy-2-propan-2-ylsulfonylethanimidamide Chemical compound CC(C)S(=O)(=O)CC(N)=NO LNOPIUAQISRISI-UHFFFAOYSA-N 0.000 claims description 7
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 7
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 239000000654 additive Substances 0.000 claims description 5
- 230000000996 additive effect Effects 0.000 claims description 5
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 3
- 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 2
- 244000017020 Ipomoea batatas Species 0.000 claims description 2
- 235000002678 Ipomoea batatas Nutrition 0.000 claims description 2
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 2
- 230000006837 decompression Effects 0.000 claims description 2
- 238000012704 multi-component copolymerization Methods 0.000 claims description 2
- 229920001592 potato starch Polymers 0.000 claims description 2
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 2
- 229940100445 wheat starch Drugs 0.000 claims description 2
- 230000002378 acidificating effect Effects 0.000 claims 1
- 230000001376 precipitating effect Effects 0.000 claims 1
- 150000003839 salts Chemical class 0.000 abstract description 11
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 15
- 230000036571 hydration Effects 0.000 description 12
- 238000006703 hydration reaction Methods 0.000 description 12
- 229920001577 copolymer Polymers 0.000 description 8
- 238000001179 sorption measurement Methods 0.000 description 8
- 239000004927 clay Substances 0.000 description 6
- 125000000542 sulfonic acid group Chemical group 0.000 description 5
- 230000009471 action Effects 0.000 description 4
- 125000003368 amide group Chemical group 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000010382 chemical cross-linking Methods 0.000 description 3
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical group C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 description 3
- 238000005553 drilling Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- 230000003993 interaction Effects 0.000 description 3
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 3
- 230000001603 reducing effect Effects 0.000 description 3
- 238000007142 ring opening reaction Methods 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 150000001767 cationic compounds Chemical class 0.000 description 2
- FOCAUTSVDIKZOP-UHFFFAOYSA-N chloroacetic acid Chemical compound OC(=O)CCl FOCAUTSVDIKZOP-UHFFFAOYSA-N 0.000 description 2
- 229940106681 chloroacetic acid Drugs 0.000 description 2
- 229910021419 crystalline silicon Inorganic materials 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229910001411 inorganic cation Inorganic materials 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- -1 quaternary ammonium cations Chemical class 0.000 description 2
- OEIXGLMQZVLOQX-UHFFFAOYSA-N trimethyl-[3-(prop-2-enoylamino)propyl]azanium;chloride Chemical compound [Cl-].C[N+](C)(C)CCCNC(=O)C=C OEIXGLMQZVLOQX-UHFFFAOYSA-N 0.000 description 2
- KEQGZUUPPQEDPF-UHFFFAOYSA-N 1,3-dichloro-5,5-dimethylimidazolidine-2,4-dione Chemical compound CC1(C)N(Cl)C(=O)N(Cl)C1=O KEQGZUUPPQEDPF-UHFFFAOYSA-N 0.000 description 1
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 description 1
- SFRDXVJWXWOTEW-UHFFFAOYSA-N 2-(hydroxymethyl)propane-1,3-diol Chemical compound OCC(CO)CO SFRDXVJWXWOTEW-UHFFFAOYSA-N 0.000 description 1
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229920000881 Modified starch Polymers 0.000 description 1
- 239000004368 Modified starch Substances 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000440 bentonite Substances 0.000 description 1
- 229910000278 bentonite Inorganic materials 0.000 description 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- XTHPWXDJESJLNJ-UHFFFAOYSA-N chlorosulfonic acid Substances OS(Cl)(=O)=O XTHPWXDJESJLNJ-UHFFFAOYSA-N 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910052909 inorganic silicate Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000661 sodium alginate Substances 0.000 description 1
- 235000010413 sodium alginate Nutrition 0.000 description 1
- 229940005550 sodium alginate Drugs 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B31/00—Preparation of derivatives of starch
- C08B31/02—Esters
- C08B31/04—Esters of organic acids, e.g. alkenyl-succinated starch
-
- 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
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/02—Well-drilling compositions
- C09K8/04—Aqueous well-drilling compositions
- C09K8/14—Clay-containing compositions
- C09K8/18—Clay-containing compositions characterised by the organic compounds
- C09K8/22—Synthetic organic compounds
- C09K8/24—Polymers
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- Dispersion Chemistry (AREA)
- Graft Or Block Polymers (AREA)
Abstract
The invention belongs to the field of filtrate reducers, and particularly discloses an environment-friendly polymer composite multielement copolymerization filtrate reducer and a preparation method thereof, wherein the preparation method comprises the following steps: adding N-acryloyl (trimethylol) aminomethane, sodium p-styrenesulfonate and (3-acrylamide propyl) trimethyl ammonium chloride into water, stirring uniformly, and regulating pH to obtain a monomer mixed solution; and adding pretreated starch and a crosslinking auxiliary agent into the monomer mixed solution, uniformly stirring, heating under a nitrogen atmosphere, adding an initiator for reaction, and drying and crushing after the reaction is finished to obtain the environment-friendly composite filtrate reducer. The composite filtrate reducer prepared by the invention has excellent salt resistance and temperature resistance, and has no pollution to the environment.
Description
Technical Field
The invention belongs to the field of filtrate reducers, and particularly relates to an environment-friendly polymer composite multielement copolymerization filtrate reducer and a preparation method thereof.
Background
The commonly used filtrate reducer generally has the defects of poor temperature resistance, poor filtrate reduction performance and the like, is not beneficial to exploitation of oil and gas field wells, and also has the risk of ecological pollution to the operation environment. The natural macromolecules such as starch and derivatives have the advantages of being green, nontoxic, easy to biodegrade, good in environmental protection performance and the like, and are often used as one of raw materials for manufacturing filtrate reducers, but the natural starch has a single molecular structure and general water solubility, so that the natural starch has poor temperature resistance, and the application of the starch in deep wells and ultra-deep wells is limited.
The Chinese patent No. 101787267A discloses a double-modified starch filtrate reducer for drilling fluid of oil and gas field and a preparation method thereof, which comprises the steps of adding starch, inorganic silicate and alcohol-based dispersing agent into a reaction vessel, uniformly dispersing, then dripping alkali liquor into the reaction vessel, carrying out a first-stage reaction under normal pressure, adding chloroacetic acid solution or sodium alginate and chloroacetic acid solution into the reaction vessel after finishing, dripping alkali liquor into the reaction vessel, carrying out a second-stage reaction under normal pressure, carrying out solid-liquid separation, and drying, wherein the filtrate reducer can still maintain certain filtrate reducing performance after aging at 110 ℃, 130 ℃, 150 ℃, and the method is simple, environment-friendly and pollution-free; however, the temperature resistance of the filtrate reducer is only within 150 ℃, and the environment operation with higher temperature cannot be satisfied.
Disclosure of Invention
In view of the defects existing in the prior art, the invention provides the environment-friendly polymer composite multielement copolymerization fluid loss additive, which has good high temperature resistance and salt resistance, effectively avoids the problem that the starch fluid loss additive is easy to degrade and lose effectiveness in high-temperature operation, and has good fluid loss effect after high-temperature aging at 220 ℃. The invention also provides a preparation method of the environment-friendly composite filtrate reducer.
The filtrate reducer is prepared by graft copolymerization of sodium p-styrenesulfonate, N-acryloyl (trimethylol) aminomethane and (3-acrylamide propyl) trimethyl ammonium chloride serving as monomers with pretreated starch and a crosslinking auxiliary agent under the action of an initiator; wherein, the sodium p-styrenesulfonate contains rigid benzene ring groups, strong hydration sulfonic acid groups and polymerizable unsaturated double bonds, so that the temperature resistance and salt resistance can be enhanced; the N- [ tri (hydroxymethyl) methyl ] acrylamide contains amide groups with strong adsorption capacity, hydrophilic polyhydroxy groups and polymerizable unsaturated double bonds, so that the adsorption stability under high temperature conditions can be enhanced, a hydration film is formed on the clay surface, and the dispersion capacity of the clay is improved; the (3-acrylamide propyl) trimethyl ammonium chloride contains quaternary ammonium cations which can be adsorbed on the clay surface through electrostatic action, amide groups with strong adsorption capacity and polymerizable unsaturated double bonds, so that the filtration reducing effect and the inorganic cation pollution resistance can be enhanced.
The preparation method of the environment-friendly polymer composite multielement copolymerization filtrate reducer comprises the following steps:
adding N-acryloyl (trimethylol) aminomethane, sodium p-styrenesulfonate and (3-acrylamide propyl) trimethyl ammonium chloride into water, stirring uniformly, and regulating the pH to be neutral to obtain a monomer mixed solution; and adding pretreated starch and a crosslinking auxiliary agent into the monomer mixed solution, uniformly stirring, heating under a nitrogen atmosphere, adding an initiator for reaction, and drying and crushing after the reaction is finished to obtain the environment-friendly composite filtrate reducer.
According to the invention, a self-made crosslinking auxiliary agent is introduced into the filtrate reducer, wherein the propylene group can be subjected to copolymerization reaction with unsaturated double bonds in the monomers, the glycidyl ether group can be subjected to ring opening reaction with active groups in starch, and meanwhile, the filtrate reducer has chemical crosslinking sites of starch and unsaturated monomer copolymers, and the copolymer chain segment moves under the high-temperature condition by increasing the interaction between the two, so that the high-temperature resistance of the composite filtrate reducer is improved. The composite filtrate reducer adopts a connecting mode with high bond energy and good thermal stability such as C-C, C-Si, C-N and the like, so that the copolymer can be kept stable under high temperature and high salt conditions, and rigid groups, adsorption groups, hydration groups and the like are introduced into side chains, so that the high temperature resistance and the salt pollution resistance are further improved.
Preferably, the preparation method of the crosslinking assistant comprises the following steps:
3-6 parts by weight of 3-glycidoxypropyl triethoxysilane and 2-5 parts by weight of 3-methacryloxypropyl triacetoxy silane are added into 20-30 parts by weight of 80-95wt% ethanol water solution, the mixture is stirred uniformly, the pH is adjusted to 2-3, and the mixture is heated to 50-60 ℃ for reaction for 2-8 hours under the nitrogen atmosphere; after the reaction is finished, the solvent is removed by decompression concentration, and the cross-linking auxiliary agent is obtained.
According to the preparation method, a part of strong hydration sulfonic acid groups are introduced through pretreatment of the starch, so that the starch filtrate reducer can still maintain good hydration capacity at high temperature and high salt, and the molecular chain curl can be effectively prevented, and the temperature resistance can be further enhanced. The invention selects sulfamic acid with mild reaction, avoids the strong degradation of starch by using strong acid, toxic sulfuric acid/chlorosulfonic acid and the like, and has simple and convenient method and little environmental pollution.
Preferably, the preparation method of the pretreated starch comprises the following steps:
adding 5-10 parts by weight of starch and 1-3 parts by weight of sulfamic acid into 30-50 parts by weight of water, stirring uniformly, heating to 100-120 ℃ for reaction for 4-6 hours, separating out with methanol after the reaction is finished, filtering, washing and drying to obtain the pretreated starch.
Preferably, the preparation method of the environment-friendly polymer composite multi-component copolymerization fluid loss additive comprises the following steps:
adding 2-5 parts by weight of N-acryloyl (trimethylol) aminomethane, 1-3 parts by weight of sodium p-styrenesulfonate and 1-2 parts by weight of (3-acrylamide propyl) trimethyl ammonium chloride into 30-50 parts by weight of water, stirring uniformly, and regulating the pH to be neutral to obtain a monomer mixed solution; adding 5-7 parts by weight of pretreated starch and 1-2 parts by weight of crosslinking auxiliary agent into the monomer mixed solution, stirring uniformly, heating to 55-60 ℃ under nitrogen atmosphere, adding 0.2-0.5 part by weight of initiator, reacting for 3-5h, drying and crushing after the reaction is finished, and obtaining the environment-friendly composite filtrate reducer.
Preferably, the starch is one or more than two of corn starch, sweet potato starch, pea starch and wheat starch.
Preferably, the initiator is one or more than two of potassium persulfate, sodium persulfate, ammonium persulfate, azobisisobutyronitrile hydrochloride and azobisiso Ding Mi hydrochloride.
The invention also provides an environment-friendly composite filtrate reducer prepared by the method.
The invention has the beneficial effects that:
(1) The composite filtrate reducer prepared by the invention adopts a connecting mode with high bond energy and good thermal stability such as C-C, C-Si, C-N and the like, so that the copolymer can be kept stable under the conditions of high temperature and high salt, and rigid groups, adsorption groups, hydration groups and the like are introduced into side chains, thereby further improving the high temperature resistance and salt pollution resistance.
(2) According to the invention, a self-made crosslinking auxiliary agent is introduced into the filtrate reducer, wherein the propylene group can be subjected to copolymerization reaction with unsaturated double bonds in the monomers, the glycidyl ether group can be subjected to ring opening reaction with active groups in starch, and meanwhile, the filtrate reducer has chemical crosslinking sites of starch and unsaturated monomer copolymers, and the copolymer chain segment moves under the high-temperature condition by increasing the interaction between the two, so that the high-temperature resistance of the composite filtrate reducer is improved.
(3) The invention takes the starch as the raw material, has no pollution to the environment, and introduces a part of strong hydration sulfonic acid groups into the pretreatment of the starch, so that the starch filtrate reducer can still maintain good hydration capability under high temperature and high salt, and can effectively prevent the molecular chain from curling and further enhance the temperature resistance.
Detailed Description
The above summary of the present invention is described in further detail below in conjunction with the detailed description, but it should not be understood that the scope of the above-described subject matter of the present invention is limited to the following examples.
3-glycidoxypropyl triethoxysilane, CAS:2602-34-8.
3-methacryloxypropyl triacetoxy silane, CAS:51772-85-1.
N-acrylamido (trimethylol) methane, CAS:13880-05-2.
(3-acrylamidopropyl) trimethylammonium chloride, CAS:45021-77-0.
Corn starch, content: 98% or more, goods number: 1589-8 available from Jiangsu Hua Xin chemical engineering Co.
Example 1
The preparation method of the environment-friendly polymer composite multielement copolymerization filtrate reducer comprises the following steps:
step one: adding 4.5 parts by weight of 3-glycidoxypropyl triethoxysilane and 3 parts by weight of 3-methacryloxypropyl triacetoxysilane into 25 parts by weight of 90wt% ethanol water solution, stirring uniformly, adjusting the pH to 2.5, and heating to 52 ℃ under nitrogen atmosphere for reaction for 5 hours; after the reaction is finished, concentrating under reduced pressure to remove the solvent to obtain a crosslinking auxiliary agent;
step two: adding 8 parts by weight of corn starch and 2.5 parts by weight of sulfamic acid into 35 parts by weight of water, stirring uniformly, heating to 115 ℃ for reacting for 5.5 hours, separating out with methanol after the reaction is finished, filtering, washing and drying to obtain pretreated starch;
step three: adding 3.5 parts by weight of N-acryloyl (trimethylol) aminomethane, 2.2 parts by weight of sodium p-styrenesulfonate and 1.8 parts by weight of (3-acrylamide propyl) trimethyl ammonium chloride into 45 parts by weight of water, uniformly stirring, and regulating the pH to be neutral to obtain a monomer mixed solution; and adding 6.5 parts by weight of pretreated starch and 1.2 parts by weight of crosslinking auxiliary agent into the monomer mixed solution, uniformly stirring, heating to 58 ℃ under nitrogen atmosphere, adding 0.3 part by weight of initiator potassium persulfate, reacting for 4.5 hours, and drying and crushing after the reaction is finished to obtain the environment-friendly composite filtrate reducer.
Example 2
The preparation method of the environment-friendly polymer composite multielement copolymerization filtrate reducer comprises the following steps:
step one: adding 8 parts by weight of corn starch and 2.5 parts by weight of sulfamic acid into 35 parts by weight of water, stirring uniformly, heating to 115 ℃ for reacting for 5.5 hours, separating out with methanol after the reaction is finished, filtering, washing and drying to obtain pretreated starch;
step two: adding 3.5 parts by weight of N-acryloyl (trimethylol) aminomethane, 2.2 parts by weight of sodium p-styrenesulfonate and 1.8 parts by weight of (3-acrylamide propyl) trimethyl ammonium chloride into 45 parts by weight of water, uniformly stirring, and regulating the pH to be neutral to obtain a monomer mixed solution; and adding 6.5 parts by weight of pretreated starch into the monomer mixed solution, uniformly stirring, heating to 58 ℃ under nitrogen atmosphere, adding 0.3 part by weight of initiator potassium persulfate, reacting for 4.5 hours, and drying and crushing after the reaction is finished to obtain the environment-friendly composite filtrate reducer.
Example 3
The preparation method of the environment-friendly polymer composite multielement copolymerization filtrate reducer comprises the following steps:
step one: mixing 4.5 parts by weight of 3-glycidoxypropyl triethoxysilane and 3 parts by weight of 3-methacryloxypropyl triacetoxysilane to obtain a crosslinking auxiliary agent;
step two: adding 8 parts by weight of corn starch and 2.5 parts by weight of sulfamic acid into 35 parts by weight of water, stirring uniformly, heating to 115 ℃ for reacting for 5.5 hours, separating out with methanol after the reaction is finished, filtering, washing and drying to obtain pretreated starch;
step three: adding 3.5 parts by weight of N-acryloyl (trimethylol) aminomethane, 2.2 parts by weight of sodium p-styrenesulfonate and 1.8 parts by weight of (3-acrylamide propyl) trimethyl ammonium chloride into 45 parts by weight of water, uniformly stirring, and regulating the pH to be neutral to obtain a monomer mixed solution; and adding 6.5 parts by weight of pretreated starch and 1.2 parts by weight of crosslinking auxiliary agent into the monomer mixed solution, uniformly stirring, heating to 58 ℃ under nitrogen atmosphere, adding 0.3 part by weight of initiator potassium persulfate, reacting for 4.5 hours, and drying and crushing after the reaction is finished to obtain the environment-friendly composite filtrate reducer.
Example 4
The preparation method of the environment-friendly polymer composite multielement copolymerization filtrate reducer comprises the following steps:
step one: adding 4.5 parts by weight of 3-glycidoxypropyl triethoxysilane and 3 parts by weight of 3-methacryloxypropyl triacetoxysilane into 25 parts by weight of 90wt% ethanol water solution, stirring uniformly, adjusting the pH to 2.5, and heating to 52 ℃ under nitrogen atmosphere for reaction for 5 hours; after the reaction is finished, concentrating under reduced pressure to remove the solvent to obtain a crosslinking auxiliary agent;
step two: adding 3.5 parts by weight of N-acryloyl (trimethylol) aminomethane, 2.2 parts by weight of sodium p-styrenesulfonate and 1.8 parts by weight of (3-acrylamide propyl) trimethyl ammonium chloride into 45 parts by weight of water, uniformly stirring, and regulating the pH to be neutral to obtain a monomer mixed solution; and adding 6.5 parts by weight of corn starch and 1.2 parts by weight of crosslinking auxiliary agent into the monomer mixed solution, uniformly stirring, heating to 58 ℃ under a nitrogen atmosphere, adding 0.3 part by weight of initiator potassium persulfate, reacting for 4.5 hours, and drying and crushing after the reaction is finished to obtain the environment-friendly composite filtrate reducer.
Example 5
The preparation method of the environment-friendly polymer composite multielement copolymerization filtrate reducer comprises the following steps:
step one: adding 4.5 parts by weight of 3-glycidoxypropyl triethoxysilane and 3 parts by weight of 3-methacryloxypropyl triacetoxysilane into 25 parts by weight of 90wt% ethanol water solution, stirring uniformly, adjusting the pH to 2.5, and heating to 52 ℃ under nitrogen atmosphere for reaction for 5 hours; after the reaction is finished, concentrating under reduced pressure to remove the solvent to obtain a crosslinking auxiliary agent;
step two: adding 8 parts by weight of corn starch and 2.5 parts by weight of sulfamic acid into 35 parts by weight of water, stirring uniformly, heating to 115 ℃ for reacting for 5.5 hours, separating out with methanol after the reaction is finished, filtering, washing and drying to obtain pretreated starch;
step three: adding 3.5 parts by weight of acrylamide, 2.2 parts by weight of sodium p-styrenesulfonate and 1.8 parts by weight of (3-acrylamide propyl) trimethyl ammonium chloride into 45 parts by weight of water, uniformly stirring, and regulating the pH to be neutral to obtain a monomer mixed solution; and adding 6.5 parts by weight of pretreated starch and 1.2 parts by weight of crosslinking auxiliary agent into the monomer mixed solution, uniformly stirring, heating to 58 ℃ under nitrogen atmosphere, adding 0.3 part by weight of initiator potassium persulfate, reacting for 4.5 hours, and drying and crushing after the reaction is finished to obtain the environment-friendly composite filtrate reducer.
Test example 1
60g of bentonite for slurry preparation in a drilling fluid test, 2.1g of anhydrous sodium carbonate and 40g of evaluation soil for the drilling fluid test are added into 1L of water, stirred for 0.5h, and maintained for 24h in a sealing mode at room temperature to obtain base slurry for later use. 10g of the environment-friendly composite filtrate reducer prepared in the example was added to 0.5L of the base slurry, stirred for 0.5h, then 150g of sodium chloride and 12.5mL of aqueous sodium hydroxide solution (40 wt%) were added, stirred for 0.5h, then aged at 220℃for 16h with rolling, cooled to room temperature, stirred for 0.5h, and then HTHP filtrate loss at 150℃and 3.5MPa was measured.
TABLE 1 test results of high temperature resistance
As can be seen from Table 1, the composite fluid loss additive prepared by the invention can still maintain good fluid loss effect under high-salt and high-temperature environments, and especially the best effect of example 1. The filtrate reducer is prepared by graft copolymerization of specific monomers, pretreated starch and crosslinking auxiliary agent under the action of an initiator. Wherein, the sodium p-styrenesulfonate contains rigid benzene ring groups, strong hydration sulfonic acid groups and polymerizable unsaturated double bonds, so that the temperature resistance and salt resistance can be enhanced; the N- [ tri (hydroxymethyl) methyl ] acrylamide contains amide groups with strong adsorption capacity, hydrophilic polyhydroxy groups and polymerizable unsaturated double bonds, so that the adsorption stability under high temperature conditions can be enhanced, a hydration film is formed on the clay surface, and the dispersion capacity of the clay is improved; the (3-acrylamide propyl) trimethyl ammonium chloride contains quaternary ammonium cations which can be adsorbed on the clay surface through electrostatic action, amide groups with strong adsorption capacity and polymerizable unsaturated double bonds, so that the filtration reducing effect and the inorganic cation pollution resistance can be enhanced; in addition, the self-made crosslinking auxiliary agent is introduced into the filtrate reducer, wherein the propylene group can be subjected to copolymerization reaction with unsaturated double bonds in the monomers, the glycidyl ether group can be subjected to ring opening reaction with active groups in starch, and meanwhile, the filtrate reducer has chemical crosslinking sites of the starch and unsaturated monomer copolymer, and the copolymer chain segment moves under the high-temperature condition by increasing the interaction between the two, so that the high-temperature resistance of the composite filtrate reducer is improved; and a part of strong hydration sulfonic acid groups are introduced by pretreatment of the starch, so that the starch filtrate reducer can still maintain good hydration capacity at high temperature and high salt, and the molecular chain curl can be effectively prevented, and the temperature resistance can be further enhanced.
The foregoing describes in detail preferred embodiments of the present invention. It should be understood that numerous modifications and variations can be made in accordance with the concepts of the invention by one of ordinary skill in the art without undue burden. Therefore, all technical solutions which can be obtained by logic analysis, reasoning or limited experiments based on the prior art by the person skilled in the art according to the inventive concept shall be within the scope of protection defined by the claims.
Claims (8)
1. The preparation method of the environment-friendly polymer composite multielement copolymerization filtrate reducer is characterized by comprising the following steps of:
adding N-acryloyl (trimethylol) aminomethane, sodium p-styrenesulfonate and (3-acrylamide propyl) trimethyl ammonium chloride into water, stirring uniformly, and regulating the pH to be neutral to obtain a monomer mixed solution; and adding pretreated starch and a crosslinking auxiliary agent into the monomer mixed solution, uniformly stirring, heating under a nitrogen atmosphere, adding an initiator for reaction, and drying and crushing after the reaction is finished to obtain the environment-friendly composite filtrate reducer.
2. The method for preparing the environment-friendly composite filtrate reducer as claimed in claim 1, wherein the preparation method of the crosslinking aid is as follows:
adding 3-glycidoxypropyl triethoxysilane and 3-methacryloxypropyl triacetoxy silane into ethanol water solution, stirring uniformly, adjusting pH to be acidic, and heating to react under nitrogen atmosphere; after the reaction is finished, the solvent is removed by decompression concentration, and the cross-linking auxiliary agent is obtained.
3. The method for preparing the environment-friendly composite filtrate reducer as claimed in claim 1, wherein the preparation method of the pretreated starch is as follows:
adding starch and sulfamic acid into water, stirring uniformly, heating for reaction, precipitating after the reaction is finished, filtering, washing and drying to obtain the pretreated starch.
4. The method for preparing the environment-friendly composite filtrate reducer as claimed in claim 1, wherein the raw materials comprise the following components in parts by weight: 5-7 parts by weight of pretreated starch, 1-2 parts by weight of cross-linking auxiliary agent and 0.2-0.5 part by weight of initiator.
5. The method for preparing the environment-friendly composite filtrate reducer as claimed in claim 1, wherein the monomer mixed solution comprises the following components in parts by weight: 2-5 parts by weight of N-acryloyl (trimethylol) aminomethane, 1-3 parts by weight of sodium p-styrenesulfonate, 1-2 parts by weight of (3-acrylamide propyl) trimethyl ammonium chloride and 30-50 parts by weight of water.
6. The method for preparing the environment-friendly composite filtrate reducer according to claim 1, wherein the starch is one or more of corn starch, sweet potato starch, pea starch and wheat starch.
7. The method for preparing the environment-friendly composite filtrate reducer according to claim 1, wherein the initiator is one or more than two of potassium persulfate, sodium persulfate, ammonium persulfate, azobisisobutyronitrile, azobisisobutyronimidine hydrochloride and azobisisobutyronitrile Ding Mi hydrochloride.
8. An environment-friendly polymer composite multi-component copolymerization fluid loss additive, which is characterized by being obtained by adopting the preparation method of any one of claims 1-7.
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