CN115404061A - Preparation method of high-temperature-resistant salt-tolerant fluid loss additive composition - Google Patents
Preparation method of high-temperature-resistant salt-tolerant fluid loss additive composition Download PDFInfo
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- CN115404061A CN115404061A CN202211206630.5A CN202211206630A CN115404061A CN 115404061 A CN115404061 A CN 115404061A CN 202211206630 A CN202211206630 A CN 202211206630A CN 115404061 A CN115404061 A CN 115404061A
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- fluid loss
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- 239000000203 mixture Substances 0.000 title claims abstract description 71
- 239000000654 additive Substances 0.000 title claims abstract description 43
- 230000000996 additive effect Effects 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 82
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 53
- 229920000642 polymer Polymers 0.000 claims abstract description 52
- 238000000034 method Methods 0.000 claims abstract description 26
- 150000003839 salts Chemical class 0.000 claims abstract description 21
- 159000000007 calcium salts Chemical class 0.000 claims abstract description 7
- 239000012266 salt solution Substances 0.000 claims description 82
- 238000003756 stirring Methods 0.000 claims description 61
- 238000006243 chemical reaction Methods 0.000 claims description 44
- 238000010438 heat treatment Methods 0.000 claims description 36
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 34
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 32
- 239000000178 monomer Substances 0.000 claims description 32
- DZSVIVLGBJKQAP-UHFFFAOYSA-N 1-(2-methyl-5-propan-2-ylcyclohex-2-en-1-yl)propan-1-one Chemical compound CCC(=O)C1CC(C(C)C)CC=C1C DZSVIVLGBJKQAP-UHFFFAOYSA-N 0.000 claims description 31
- 239000003999 initiator Substances 0.000 claims description 27
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 19
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 18
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 18
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 17
- 229960003563 calcium carbonate Drugs 0.000 claims description 17
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 16
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 16
- GMSCBRSQMRDRCD-UHFFFAOYSA-N dodecyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCCOC(=O)C(C)=C GMSCBRSQMRDRCD-UHFFFAOYSA-N 0.000 claims description 16
- 230000007935 neutral effect Effects 0.000 claims description 12
- 230000002378 acidificating effect Effects 0.000 claims description 9
- 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 description 9
- SOGAXMICEFXMKE-UHFFFAOYSA-N Butylmethacrylate Chemical compound CCCCOC(=O)C(C)=C SOGAXMICEFXMKE-UHFFFAOYSA-N 0.000 claims description 8
- 229910052700 potassium Inorganic materials 0.000 claims description 6
- UIIIBRHUICCMAI-UHFFFAOYSA-N prop-2-ene-1-sulfonic acid Chemical compound OS(=O)(=O)CC=C UIIIBRHUICCMAI-UHFFFAOYSA-N 0.000 claims description 6
- CNCOEDDPFOAUMB-UHFFFAOYSA-N N-Methylolacrylamide Chemical compound OCNC(=O)C=C CNCOEDDPFOAUMB-UHFFFAOYSA-N 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
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 4
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 4
- 239000001110 calcium chloride Substances 0.000 claims description 4
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 4
- 235000011148 calcium chloride Nutrition 0.000 claims description 4
- MKJXYGKVIBWPFZ-UHFFFAOYSA-L calcium lactate Chemical compound [Ca+2].CC(O)C([O-])=O.CC(O)C([O-])=O MKJXYGKVIBWPFZ-UHFFFAOYSA-L 0.000 claims description 4
- 239000001527 calcium lactate Substances 0.000 claims description 4
- 229960002401 calcium lactate Drugs 0.000 claims description 4
- 235000011086 calcium lactate Nutrition 0.000 claims description 4
- SUPCQIBBMFXVTL-UHFFFAOYSA-N ethyl 2-methylprop-2-enoate Chemical compound CCOC(=O)C(C)=C SUPCQIBBMFXVTL-UHFFFAOYSA-N 0.000 claims description 4
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 4
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 4
- HWDDJFFLFNQAFQ-UHFFFAOYSA-M potassium;4-ethenylbenzenesulfonate Chemical compound [K+].[O-]S(=O)(=O)C1=CC=C(C=C)C=C1 HWDDJFFLFNQAFQ-UHFFFAOYSA-M 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
- 239000007787 solid Substances 0.000 claims description 4
- FOGYNLXERPKEGN-UHFFFAOYSA-N 3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfopropyl)phenoxy]propane-1-sulfonic acid Chemical compound COC1=CC=CC(CC(CS(O)(=O)=O)OC=2C(=CC(CCCS(O)(=O)=O)=CC=2)OC)=C1O FOGYNLXERPKEGN-UHFFFAOYSA-N 0.000 claims description 3
- SBVKVAIECGDBTC-UHFFFAOYSA-N 4-hydroxy-2-methylidenebutanamide Chemical compound NC(=O)C(=C)CCO SBVKVAIECGDBTC-UHFFFAOYSA-N 0.000 claims description 3
- 239000004227 calcium gluconate Substances 0.000 claims description 3
- 229960004494 calcium gluconate Drugs 0.000 claims description 3
- 235000013927 calcium gluconate Nutrition 0.000 claims description 3
- NEEHYRZPVYRGPP-UHFFFAOYSA-L calcium;2,3,4,5,6-pentahydroxyhexanoate Chemical compound [Ca+2].OCC(O)C(O)C(O)C(O)C([O-])=O.OCC(O)C(O)C(O)C(O)C([O-])=O NEEHYRZPVYRGPP-UHFFFAOYSA-L 0.000 claims description 3
- NZIDBRBFGPQCRY-UHFFFAOYSA-N octyl 2-methylprop-2-enoate Chemical compound CCCCCCCCOC(=O)C(C)=C NZIDBRBFGPQCRY-UHFFFAOYSA-N 0.000 claims description 3
- 235000010216 calcium carbonate Nutrition 0.000 claims description 2
- FUFJGUQYACFECW-UHFFFAOYSA-L calcium hydrogenphosphate Chemical compound [Ca+2].OP([O-])([O-])=O FUFJGUQYACFECW-UHFFFAOYSA-L 0.000 claims description 2
- 235000019700 dicalcium phosphate Nutrition 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 239000004568 cement Substances 0.000 abstract description 43
- 239000002002 slurry Substances 0.000 abstract description 11
- 239000003129 oil well Substances 0.000 abstract description 9
- 238000006116 polymerization reaction Methods 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 230000009471 action Effects 0.000 abstract description 2
- 238000013461 design Methods 0.000 abstract description 2
- 230000007246 mechanism Effects 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 39
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 34
- 239000008367 deionised water Substances 0.000 description 34
- 229910021641 deionized water Inorganic materials 0.000 description 34
- 238000001035 drying Methods 0.000 description 17
- 238000007670 refining Methods 0.000 description 17
- 230000000052 comparative effect Effects 0.000 description 10
- 239000000047 product Substances 0.000 description 7
- 238000001514 detection method Methods 0.000 description 5
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 4
- 239000003638 chemical reducing agent Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000011591 potassium Substances 0.000 description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 description 3
- 229960005069 calcium Drugs 0.000 description 3
- 239000011575 calcium Substances 0.000 description 3
- 229910052791 calcium Inorganic materials 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 description 3
- PQVFIKHKSFZHLT-UHFFFAOYSA-M sodium;3-ethenylbenzenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C1=CC=CC(C=C)=C1 PQVFIKHKSFZHLT-UHFFFAOYSA-M 0.000 description 3
- ATBDZSAENDYQDW-UHFFFAOYSA-N 3-ethenylbenzenesulfonic acid Chemical compound OS(=O)(=O)C1=CC=CC(C=C)=C1 ATBDZSAENDYQDW-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 230000003111 delayed effect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 229920005615 natural polymer Polymers 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 2
- 239000012265 solid product Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 230000008719 thickening Effects 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 125000003368 amide group Chemical group 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 239000013505 freshwater Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000015784 hyperosmotic salinity response Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- 239000003077 lignite Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 239000003209 petroleum derivative Substances 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 235000010344 sodium nitrate Nutrition 0.000 description 1
- 239000004317 sodium nitrate Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 229920001059 synthetic polymer Polymers 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
- C08F293/00—Macromolecular compounds obtained by polymerisation on to a macromolecule having groups capable of inducing the formation of new polymer chains bound exclusively at one or both ends of the starting macromolecule
-
- 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
- C09K8/487—Fluid loss control additives; Additives for reducing or preventing circulation loss
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention relates to the field of oilfield chemicals, and in particular relates to a preparation method of a high-temperature-resistant salt-tolerant fluid loss additive composition. According to the invention, through analyzing the action mechanism process of the fluid loss agent in a high-temperature and high-salt environment, the original random polymer is adjusted into the block polymer through molecular chain design by adopting a block stepwise polymerization method, and the rigid chain of the block polymer is regularly and stepwise arranged in the polymer chain, so that the high-temperature resistant and salt resistant effects are achieved, and the polymer with the hydrophilic end at the rigid chain has better water control capability, and can effectively control the water loss of cement slurry. Meanwhile, the prepared fluid loss agent and calcium salt are mixed to prepare the fluid loss agent composition, so that the dispersibility of the fluid loss agent in cement paste is improved, and the compressive strength of the cement paste can be improved by applying the fluid loss agent composition to the preparation process of the cement paste. The invention has reliable principle, is suitable for oil well cementing cement slurry and has wide application prospect.
Description
Technical Field
The invention relates to the field of oilfield chemicals, and in particular relates to a preparation method of a high-temperature-resistant salt-tolerant fluid loss additive composition.
Background
The fluid loss agent is one of three main and most important external additives in oil field well cementation cement slurry, and by adding the fluid loss agent into the cement slurry, the viscosity of a liquid phase in the cement slurry can be improved, and the purpose of controlling the filtration loss of the liquid phase to a permeable stratum is achieved, so that the filtration of a filter cake is reduced, the relatively stable water cement ratio during the solidification of the cement slurry is ensured, and the well cementation quality is improved; however, with the less and less exploitable shallow petroleum and natural gas resources, the exploration and development of oil fields gradually develop towards deep wells, ultra-deep wells and complex bottom layers, and the currently used fluid loss additive cannot meet the performance requirements and generally has the defects of poor salt resistance and high temperature resistance; when the temperature at the bottom of a well or the salt content is too high, the molecular chain of the common fluid loss agent is broken, inactivated and the like, the adsorption capacity in cement slurry is greatly weakened, the failure of well cementation is seriously caused, and safety accidents occur; meanwhile, the cementing and sealing section is long, the temperature difference between the upper part and the lower part is large, and the retarder of the fluid loss agent is weak to cement slurry when the fluid loss agent returns to the upper lower temperature well section after high-temperature circulation at the bottom of the well and is condensed, so that the difference between the temperature difference between the upper part and the lower part is too large, and the quality problem occurs when the cement slurry is not stably cured; therefore, the high-temperature resistant, large-temperature-difference resistant and salt-tolerant fluid loss additive is a development hotspot in the field of oil field chemicals at present;
at present, the polymer fluid loss additive mainly comprises natural polymer and synthetic polymer. The natural polymer is mainly a plant processing product, exists in the nature in a large amount, is widely available, low in cost, environment-friendly and degradable, is often used as a cementing fluid loss agent for early oil and gas fields, and is mainly cellulose, lignin, starch, lignite and the like. However, they have not been widely used in industrial applications because of their different drawbacks in terms of high temperature resistance, temperature difference resistance, and compatibility.
The other is a synthetic high molecular polymer which comprises nonionic, anionic, cationic and zwitterionic polymers, and 2-acrylamide-2-methylpropanesulfonic Acid (AMPS) is mainly taken as a copolymer and a polyvinyl alcohol (PVA) high molecular fluid loss agent in related technical patents; the PVA-type fluid loss agent is a non-ionic fluid loss agent, has strong water loss control capability at low temperature, has no delayed coagulation, but can only be used for the condition of low-temperature fresh water due to poor temperature resistance and salt resistance. AMPS polymerization water loss reducer, such as CN201410428963.1, discloses a high temperature and salt resistant oil well cement water loss reducer and a preparation method thereof, CN201510520863.6 discloses a temperature and salt resistant oil well cement water loss reducer and a preparation method and application thereof, and CN200810226689.4 discloses an oil well cement water loss reducer, wherein the above disclosed technologies are all generated by random copolymerization, amide groups (-CONH) in synthesized polymer molecules are easy to hydrolyze to generate organic acid and organic sulfonate with low molecular weight under the environment of ultrahigh temperature, high salt content and alkaline environment, so that the water loss reducing performance is greatly reduced, and other application performances (such as rheological property, thickening time, sedimentation stability, compatibility and compressive strength) of cement slurry are negatively influenced. Therefore, the research on the novel fluid loss agent which has high temperature resistance, salt resistance and no negative influence on other properties of cement paste is of great significance.
Disclosure of Invention
In order to overcome the defects of the prior art and products, the invention develops the high-temperature-resistant salt-tolerant fluid loss additive composition with excellent water loss reducing performance and good compatibility effect with a cement retarder by using a special polymerization method and adopting block polymerization, and makes up the defects caused by APMS polymerization.
The invention provides a preparation method of a high-temperature-resistant salt-tolerant fluid loss agent composition, which is characterized in that through analysis of the action mechanism process of a fluid loss agent in a high-temperature and high-salt environment, a block stepwise polymerization method is adopted, the original random polymer is adjusted into a block polymer through molecular chain design, and rigid chains of the block polymer are regularly distributed in a polymer chain, so that the high-temperature-resistant salt-tolerant effect is achieved, and the optimal product is obtained.
The preparation method of the high-temperature-resistant salt-resistant fluid loss agent composition sequentially comprises the following steps:
step 1: dissolving an alkaline monomer and a neutral monomer in water to form a salt solution (1), and adjusting the pH to be alkaline by using alkali;
step 2: adding the salt solution (1) into a reaction kettle, heating under the protection of N2, slowly dropwise adding an initiator, and forming an intermediate polymer (1) after dropwise adding reaction is completed;
and step 3: dissolving an acidic monomer in water to form a salt solution (2); adding the intermediate polymer (1) into a reaction kettle, heating under the protection of N2, slowly dropwise adding a salt solution (2), and obtaining a fluid loss agent after the reaction is finished;
and 4, step 4: and (3) adding calcium carbonate into the fluid loss agent obtained in the step (3) according to a certain proportion, and stirring at a high speed until the mixture is uniform to obtain the high-temperature-resistant salt-tolerant fluid loss agent composition.
The weight of the fluid loss agent is calculated by 100 parts, the dosage of the alkaline monomer accounts for 5-88 parts, the dosage of the neutral monomer accounts for 5-88 parts, the dosage of the acidic monomer accounts for 6-89 parts, and the dosage of the initiator ammonium persulfate accounts for 0.1-5 parts; the mass of the fluid loss agent accounts for 10-50% of the total mass of the high-temperature-resistant salt-tolerant fluid loss agent composition.
In the step 1, the solid content of the salt solution (1) is 10-50%, and the pH is adjusted to 8.0-14.0;
the basic monomer is selected from one or more of p-, o-and m-alkene sulfonate containing benzene ring, and the structural formula is as follows:
Wherein n =0 to 10 Me = Na, K, ca, mg and Zn, and further the alkaline monomer is sodium p-styrene sulfonate or potassium p-styrene sulfonate;
the structural formula of the neutral monomer in the step 1 is as follows:
Wherein n =0 to 10m =0 to 15; further, the neutral monomer is specifically selected from one or more of methyl methacrylate, lauryl methacrylate, ethyl methacrylate, acrylamide, butyl methacrylate and octyl methacrylate; furthermore, the neutral monomer is a mixture of acrylamide and lauryl methacrylate in any proportion.
In the step 2, the temperature of the system is raised to 40-70 ℃, an initiator is slowly dripped, the dripping speed of the initiator is 0.1-5.0 ml/min, and the viscosity of the intermediate polymer (1) is 100-2500 mPa.s; the initiator is selected from one of sodium persulfate, potassium persulfate and ammonium persulfate.
In the step 3, the solid content of the salt solution (2) is 20 to 50 percent; the temperature of the system is raised to 50-90 ℃, the salt solution (2) is slowly added, the dropping speed of the salt solution (2) is 0.1-5.0 ml/min, and the viscosity of the fluid loss agent obtained after the reaction is finished is 2000-20000mPa.S; the acidic monomer is one or more of allyl sulfonic acid, 2-acrylamide-2-methylpropanesulfonic Acid (AMPS), lignosulfonic acid, acrylic acid, maleic anhydride, hydroxyethyl acrylamide and hydroxymethyl acrylamide, and further the acidic monomer is a mixture of 2-acrylamide-2-methylpropanesulfonic Acid (AMPS), maleic anhydride and acrylic acid in any proportion
In the step 4, the calcium salt is selected from one or more of calcium carbonate, calcium gluconate, calcium hydrogen phosphate, calcium lactate and calcium chloride, and further, the calcium salt is calcium carbonate.
The invention has the beneficial effects that:
(1) The optimized alkaline monomer is a benzene ring-containing alkene monomer, so that the temperature resistance of the fluid loss agent can be improved, the salt resistance of the fluid loss agent can be improved by a neutral monomer, namely lauryl methacrylate, and the fluid loss agent can be improved by acidic monomers, such as acrylic acid, maleic anhydride and the like;
(2) The fluid loss agent adopts a block stepwise polymerization mode, firstly neutral and basic group monomers react to form a rigid chain consisting of a benzene ring and straight-chain alkane, so that the fluid loss agent is not easy to decompose at high temperature; then the tail end is connected with an acid group monomer, the product is alkaline, and the salt resistance, the alkali resistance and the temperature resistance of the product are further improved; the polymer with the hydrophilic tail end of the rigid chain has better water control capability, and effectively controls the water loss of cement paste;
(3) The fluid loss agent composition prepared by the invention is mixed and stirred with calcium salt, can improve the dispersibility of the fluid loss agent in cement paste, and can improve the compressive strength of the cement paste when the prepared fluid loss agent composition is applied to the preparation process of the cement paste.
(4) The invention has reliable principle, is suitable for the cement paste of the oil well ancient well and has wide application prospect.
Detailed Description
Example 1
Step 1: dissolving 5 parts of sodium p-styrene sulfonate, 3 parts of acrylamide and 2 parts of lauryl methacrylate in deionized water, and adjusting the pH value to 8.5 to prepare a salt solution (1);
and 2, step: then adding the salt solution (1) into a reaction kettle under N 2 Under the protection condition, starting stirring and heating; slowly dripping 1 part of initiator ammonium persulfate to react for 50min when the temperature of the system rises to 65 ℃, so as to form an intermediate polymer (1), wherein the test viscosity is 800MPa.s;
and step 3: dissolving 39 parts of 2-acrylamide-2-methylpropanesulfonic Acid (AMPS), 25 parts of maleic anhydride and 25 parts of acrylic acid in deionized water, and stirring until the components are completely dissolved to form a salt solution (2); adding the obtained intermediate polymer (1) into a reaction kettle in N 2 Under the protection condition, starting stirring and heating; slowly adding the salt solution (2) when the temperature of the system rises to 70 ℃, controlling the dropping speed to be 12min, and reacting for 80min to obtain the colorless viscous high-temperature-resistant salt-tolerant fluid loss agent; the viscosity was measured at 5000MPa.S, while the molecular weight was measured by ethanol refining and oven drying, and its Mn was 1.5 x 10 5 Mw of 2.8 x 10 5 PDI of 1.87;
and 4, step 4: adding 100 parts of the high-temperature-resistant salt-tolerant fluid loss additive obtained in the step 3 and 400 parts of calcium carbonate into a container, and stirring at a high speed until a uniform white viscous mixture is obtained, namely the fluid loss additive composition;
example 2
Step 1: dissolving 20 parts of sodium p-styrene sulfonate, 5 parts of acrylamide and 5 parts of lauryl methacrylate in deionized water, and adjusting the pH value to 9 to prepare a salt solution (1);
step 2: then adding the salt solution (1) into a reaction kettle under N 2 Under the protection condition, starting stirring and heating; when the temperature of the system rises to 40 ℃, 5 parts of initiator ammonium persulfate is slowly dripped to react for 60min to form an intermediate polymer (1), and the test viscosity is shown in data table 1;
and 3, step 3: then 60 parts of 2-acrylamide-2-methylpropanesulfonic Acid (AMPS), 2 parts of maleic anhydride and 3 parts of acrylic acid are dissolved in deionized water and stirred until complete dissolution, so as to form a salt solution (2); adding the obtained intermediate polymer (1) into a reaction kettle in N 2 Under the protection condition, starting stirring and heating; slowly adding the salt solution (2) when the temperature of the system rises to 75 ℃, controlling the dropping speed to be 10min, and reacting for 120min to obtain the colorless viscous high-temperature-resistant salt-tolerant fluid loss agent; testing viscosity, simultaneously refining ethanol, drying and testing molecular weight, wherein the data are shown in a data table 1;
and 4, step 4: adding 100 parts of the high-temperature-resistant salt-tolerant fluid loss additive obtained in the step 3 and 900 parts of calcium carbonate into a container, and stirring at a high speed until a uniform white viscous mixture is obtained, namely the fluid loss additive composition;
example 3
Step 1: dissolving 40 parts of potassium p-styrene sulfonate, 2 parts of acrylamide and 18 parts of lauryl methacrylate in deionized water, and adjusting the pH value to 8 to prepare a salt solution (1);
step 2: then adding the salt solution (1) into a reaction kettle under N 2 Under the protection condition, starting stirring and heating; when the temperature of the system rises to 70 ℃,2 parts of initiator ammonium persulfate is slowly dripped to react for 55min to form an intermediate polymer (1), and the viscosity is tested and shown in data table 1;
and step 3: dissolving 5 parts of 2-acrylamide-2-methylpropanesulfonic Acid (AMPS), 10 parts of maleic anhydride and 23 parts of acrylic acid in deionized water, and stirring until the components are completely dissolved to form a salt solution (2); adding the obtained intermediate polymer (1) into a reaction kettle in N 2 Under the protection condition, starting stirring and heating; when the temperature of the system rises to 80 ℃, slowly adding the salt solution (2), and controlling the dropping speedAfter 15min, reacting for 90min to obtain colorless viscous high-temperature-resistant salt-tolerant fluid loss agent; testing viscosity, and simultaneously, refining ethanol, drying and testing molecular weight, and referring to data table 1;
and 4, step 4: adding 300 parts of the high-temperature-resistant salt-tolerant fluid loss additive obtained in the step 3 and 700 parts of calcium carbonate into a container, and stirring at a high speed until a uniform white viscous mixture is obtained, namely the fluid loss additive composition;
example 4
Step 1: dissolving 60 parts of potassium m-styrene sulfonate, 24 parts of acrylamide and 6 parts of lauryl methacrylate in deionized water, and adjusting the pH value to 9.5 to prepare a salt solution (1);
step 2: then adding the salt solution (1) into a reaction kettle under N 2 Under the protection condition, starting stirring and heating; when the temperature of the system rises to 50 ℃, 0.5 part of initiator ammonium persulfate is slowly dripped to react for 70min to form an intermediate polymer (1), and the viscosity is tested and shown in data table 1;
and step 3: dissolving 0.5 part of 2-acrylamide-2-methylpropanesulfonic Acid (AMPS), 2 parts of maleic anhydride and 7 parts of acrylic acid in deionized water, and stirring until the components are completely dissolved to form a salt solution (2); adding the obtained intermediate polymer (1) into a reaction kettle, and reacting under N 2 Under the protection condition, starting stirring and heating; slowly adding the salt solution (2) when the temperature of the system rises to 60 ℃, controlling the dropwise adding speed to be 10min, and reacting for 60min to obtain a colorless viscous high-temperature-resistant salt-tolerant fluid loss agent; testing viscosity, and simultaneously refining ethanol and drying to test molecular weight, see data table 1;
and 4, step 4: adding 200 parts of the high-temperature-resistant salt-tolerant fluid loss additive obtained in the step 3 and 300 parts of calcium carbonate into a container, and stirring at a high speed until a uniform white viscous mixture is obtained, namely the fluid loss additive composition;
example 5
Step 1: dissolving 88 parts of sodium m-styrene sulfonate, 4.8 parts of acrylamide and 0.2 part of lauryl methacrylate in deionized water, and adjusting the pH value to 14 to prepare a salt solution (1);
step 2: then adding the salt solution (1) into a reaction kettle under N 2 Under the protection condition, starting stirring and heating; when the temperature of the system rises to 45 ℃,1 part of initiator is slowly drippedAmmonium sulfate reaction for 120min to form intermediate polymer (1), viscosity was measured, see data table 1;
and step 3: then 0.12 part of 2-acrylamide-2-methylpropanesulfonic Acid (AMPS), 0.12 part of maleic anhydride and 5.76 parts of acrylic acid are dissolved in deionized water and stirred until complete dissolution, so as to form a salt solution (2); adding the obtained intermediate polymer (1) into a reaction kettle in N 2 Under the protection condition, starting stirring and heating; slowly adding the salt solution (2) when the temperature of the system rises to 90 ℃, controlling the dropping speed to be 13min, and reacting for 70min to obtain the colorless viscous high-temperature-resistant salt-tolerant fluid loss agent; testing viscosity, and simultaneously refining ethanol and drying to test molecular weight, see data table 1;
and 4, step 4: adding 100 parts of the high-temperature-resistant salt-tolerant fluid loss additive obtained in the step 3 and 100 parts of calcium carbonate into a container, and stirring at a high speed until a uniform white viscous mixture is obtained, namely the fluid loss additive composition;
example 6
Step 1: dissolving 5 parts of sodium p-styrene sulfonate, 1 part of acrylamide and 87 parts of lauryl methacrylate in deionized water, and adjusting the pH value to 12 to prepare a salt solution (1);
step 2: then adding the salt solution (1) into a reaction kettle in N 2 Under the protection condition, starting stirring and heating; when the temperature of the system rises to 60 ℃, slowly dropwise adding 1 part of initiator ammonium persulfate to react for 30min to form an intermediate polymer (1), and testing the viscosity, which is shown in data table 1; 400MPa.s;
and 3, step 3: dissolving 0.4 part of 2-acrylamide-2-methylpropanesulfonic Acid (AMPS), 5.2 parts of maleic anhydride and 0.4 part of acrylic acid in deionized water, and stirring until the materials are completely dissolved to form a salt solution (2); adding the obtained intermediate polymer (1) into a reaction kettle, and reacting under N 2 Under the protection condition, starting stirring and heating; slowly adding the salt solution (2) when the temperature of the system rises to 70 ℃, controlling the dropping speed to be 12min, and reacting for 100min to obtain the colorless viscous high-temperature-resistant salt-tolerant fluid loss agent; the viscosity is tested, and the molecular weight is tested by refining, drying and testing the ethanol at the same time, which is shown in data table 1;
and 4, step 4: adding 100 parts of the high-temperature-resistant salt-tolerant fluid loss additive obtained in the step 3 and 400 parts of calcium carbonate into a container, and stirring at a high speed until a uniform white viscous mixture is obtained, namely the fluid loss additive composition;
example 7
Step 1: dissolving 5 parts of sodium p-styrene sulfonate and 5 parts of acrylamide in deionized water, and adjusting the pH value to 11 to prepare a salt solution (1);
and 2, step: then adding the salt solution (1) into a reaction kettle under N 2 Under the protection condition, starting stirring and heating; when the temperature of the system rises to 65 ℃,1 part of initiator sodium persulfate is slowly dripped to react for 40min to form an intermediate polymer (1), and the viscosity is tested and shown in data table 1;
and 3, step 3: then 89 parts of maleic anhydride is dissolved in deionized water and stirred until the maleic anhydride is completely dissolved to form a salt solution (2); adding the obtained intermediate polymer (1) into a reaction kettle in N 2 Under the protection condition, starting stirring and heating; slowly adding the salt solution (2) when the temperature of the system rises to 75 ℃, controlling the dropping speed to be 11min, and reacting for 75min to obtain the colorless viscous high-temperature-resistant salt-tolerant fluid loss agent; testing viscosity, and simultaneously, refining ethanol, drying and testing molecular weight, and referring to data table 1;
and 4, step 4: adding 100 parts of the high-temperature-resistant salt-tolerant fluid loss agent obtained in the step 3 and 400 parts of calcium chloride into a container, and stirring at a high speed until a uniform white viscous mixture is obtained, namely the fluid loss agent composition;
example 8
Step 1: dissolving 20 parts of potassium p-styrene sulfonate, 5 parts of acrylamide and 5 parts of ethyl methacrylate in deionized water, and adjusting the pH value to 10 to prepare a salt solution (1);
step 2: then adding the salt solution (1) into a reaction kettle in N 2 Under the protection condition, starting stirring and heating; when the temperature of the system rises to 50 ℃, 5 parts of initiator potassium persulfate is slowly dripped to react for 100min to form an intermediate polymer (1), and the viscosity is tested and shown in data table 1;
and step 3: dissolving 15 parts of lignosulfonic acid, 15 parts of allylsulfonic acid and 35 parts of hydroxyethyl acrylamide in deionized water, and stirring until completely dissolved to form a salt solution (2); adding the obtained intermediate polymer (1) into a reaction kettle in N 2 Under the protection condition, starting stirring and heating; slowly adding the mixture when the temperature of the system rises to 85 DEG CThe salt solution (2) is added after the dropwise adding speed is controlled to be 25min, and the colorless viscous high-temperature-resistant salt-tolerant fluid loss agent is obtained after reaction for 85 min; testing viscosity, and simultaneously refining ethanol and drying to test molecular weight, see data table 1;
and 4, step 4: adding 200 parts of the high-temperature-resistant salt-tolerant fluid loss additive obtained in the step 3, 100 parts of calcium hydrophosphate and 200 parts of calcium lactate into a container, and stirring at a high speed until a white viscous mixture is uniform, namely the fluid loss additive composition;
example 9
Step 1: dissolving 40 parts of sodium m-styrene sulfonate, 5 parts of methyl methacrylate, 5 parts of butyl methacrylate and 10 parts of octyl methacrylate in deionized water, and adjusting the pH value to 13 to prepare a salt solution (1);
step 2: then adding the salt solution (1) into a reaction kettle in N 2 Under the protection condition, starting stirring and heating; when the temperature of the system rises to 40 ℃,2 parts of initiator ammonium persulfate is slowly dripped to react for 45min to form an intermediate polymer (1), and the viscosity is tested and shown in data table 1;
and step 3: then 5 parts of hydroxymethyl acrylamide, 10 parts of allyl sulfonic acid and 23 parts of acrylic acid are dissolved in deionized water and stirred until the materials are completely dissolved to form a salt solution (2); adding the obtained intermediate polymer (1) into a reaction kettle, and reacting under N 2 Under the protection condition, starting stirring and heating; slowly adding the salt solution (2) when the temperature of the system rises to 50 ℃, controlling the dropwise adding speed to be 15min, and reacting for 90min to obtain a colorless viscous high-temperature-resistant salt-tolerant fluid loss agent; testing viscosity, and simultaneously refining ethanol and drying to test molecular weight, see data table 1;
and 4, step 4: adding 200 parts of the high-temperature-resistant salt-tolerant fluid loss agent obtained in the step 3 and 300 parts of calcium gluconate into a container, and stirring at a high speed until a uniform white viscous mixture is obtained, namely the fluid loss agent composition;
example 10
Step 1: dissolving 60 parts of calcium orthophthalenesulfonate and 30 parts of butyl methacrylate in deionized water, and adjusting the pH value to 8.5 to prepare a salt solution (1);
step 2: then adding the salt solution (1) into a reaction kettle in N 2 Under the protection condition, starting stirring and heating; wait bodyRaising the temperature to 55 ℃, slowly adding 0.5 part of initiator potassium persulfate dropwise for reaction for 110min to form an intermediate polymer (1), and testing the viscosity, wherein the data is shown in a data table 1;
and step 3: dissolving 9.5 parts of allyl sulfonic acid in deionized water, and stirring until the allyl sulfonic acid is completely dissolved to form a salt solution (2); adding the obtained intermediate polymer (1) into a reaction kettle in N 2 Under the protection condition, starting stirring and heating; slowly adding the salt solution (2) when the temperature of the system rises to 80 ℃, controlling the dropping speed to be 20min, and reacting for 80min to obtain the colorless viscous high-temperature-resistant salt-tolerant fluid loss agent; testing viscosity, refining ethanol, drying and testing molecular weight, and the data are shown in a data table 1;
and 4, step 4: adding 100 parts of the high-temperature-resistant salt-tolerant fluid loss additive obtained in the step 3 and 400 parts of calcium hydrophosphate into a container, and stirring at a high speed until a uniform white viscous mixture is obtained, namely the fluid loss additive composition;
example 11
Step 1: dissolving 40 parts of sodium p-styrenesulfonate, 48 parts of potassium o-propylsulfonate, 2 parts of lauryl methacrylate and 3 parts of methyl methacrylate in deionized water, and adjusting the pH value to 9 to prepare a salt solution (1);
and 2, step: then adding the salt solution (1) into a reaction kettle under N 2 Under the protection condition, starting stirring and heating; slowly dripping 1 part of initiator sodium persulfate to react for 80min when the temperature of the system rises to 65 ℃, and forming an intermediate polymer (1), and testing the viscosity, which is shown in data table 1;
and step 3: dissolving 6 parts of hydroxymethyl acrylamide in deionized water, and stirring until the hydroxymethyl acrylamide is completely dissolved to form a salt solution (2); adding the obtained intermediate polymer (1) into a reaction kettle in N 2 Under the protection condition, starting stirring and heating; slowly adding the salt solution (2) when the temperature of the system rises to 85 ℃, controlling the dropping speed to be 30min, and reacting for 75min to obtain the colorless viscous high-temperature-resistant salt-tolerant fluid loss agent; testing viscosity, and simultaneously refining ethanol and drying to test molecular weight, see data table 1;
and 4, step 4: adding 100 parts of the high-temperature-resistant salt-tolerant fluid loss additive obtained in the step 3, 50 parts of calcium lactate and 50 parts of calcium chloride into a container, and stirring at a high speed until a white viscous mixture is uniform, namely the fluid loss additive composition;
example 12
Step 1: dissolving 5 parts of potassium p-propenesulfonate and 88 parts of ethyl methacrylate in deionized water, and adjusting the pH value to 10 to prepare a salt solution (1);
step 2: then adding the salt solution (1) into a reaction kettle under N 2 Under the protection condition, starting stirring and heating; when the temperature of the system rises to 60 ℃, slowly dropwise adding 1 part of initiator ammonium persulfate to react for 90min to form an intermediate polymer (1), and testing the viscosity, which is shown in data table 1;
and step 3: dissolving 2 parts of acrylic acid and 4 parts of maleic anhydride in deionized water, and stirring until the acrylic acid and the maleic anhydride are completely dissolved to form a salt solution (2); adding the obtained intermediate polymer (1) into a reaction kettle in N 2 Under the protection condition, starting stirring and heating; slowly adding the salt solution (2) when the temperature of the system rises to 75 ℃, controlling the dropping speed to be 10min, and reacting for 95min to obtain the colorless viscous high-temperature-resistant salt-tolerant fluid loss agent; testing viscosity, and simultaneously refining ethanol and drying to test molecular weight, see data table 1;
and 4, step 4: adding 100 parts of the high-temperature-resistant salt-tolerant fluid loss additive obtained in the step 3 and 100 parts of calcium carbonate into a container, and stirring at a high speed until a uniform white viscous mixture is obtained, namely the fluid loss additive composition;
comparative example 1
Step 1: dissolving 5 parts of sodium p-styrene sulfonate, 3 parts of acrylamide and 2 parts of lauryl methacrylate in deionized water, and adjusting the pH value to 8.5 to prepare a salt solution (1);
and 2, step: dissolving 39 parts of 2-acrylamide-2-methylpropanesulfonic Acid (AMPS), 25 parts of maleic anhydride and 25 parts of acrylic acid in deionized water, and stirring until the components are completely dissolved to form a salt solution (2);
and step 3: firstly adding a salt solution (1) and a salt solution (2) into a reaction kettle, and adding N 2 Under the protection condition, starting stirring and heating; slowly dripping 1 part of initiator ammonium persulfate to react for 40min when the temperature of the system rises to 60 ℃ to obtain a colorless viscous fluid loss agent; ethanol refining and drying to test the molecular weight, see data table 1; (ii) a
And 4, step 4: and (4) adding 100 parts of the fluid loss agent obtained in the step (3) and 400 parts of calcium carbonate into a container, and stirring at a high speed until the fluid loss agent composition is uniformly obtained.
Comparative example 2
Step 1: dissolving 30 parts of sodium p-styrene sulfonate in deionized water, adjusting the pH value to 9, and preparing a salt solution (1);
and 2, step: then adding the salt solution (1) into a reaction kettle in N 2 Under the protection condition, starting stirring and heating; when the temperature of the system rises to 65 ℃, 5 parts of initiator ammonium persulfate is slowly dripped to react for 100min to form an intermediate polymer (1), and the test viscosity is 800MPa.s;
and 3, step 3: dissolving 60 parts of 2-acrylamide-2-methylpropanesulfonic Acid (AMPS), 2 parts of maleic anhydride and 3 parts of acrylic acid in deionized water, and stirring until the components are completely dissolved to form a salt solution (2); adding the obtained intermediate polymer (1) into a reaction kettle in N 2 Under the protection condition, starting stirring and heating; slowly adding the salt solution (2) when the temperature of the system rises to 75 ℃, controlling the dropping speed to be 20min, and reacting for 80min to obtain the colorless viscous high-temperature-resistant salt-tolerant fluid loss agent; the test viscosity is 5000MPa.S, and the molecular weight is tested by refining and drying ethanol at the same time, see data table 1; (ii) a
And 4, step 4: adding 100 parts of the high-temperature-resistant salt-tolerant fluid loss agent obtained in the step 3 and 900 parts of calcium carbonate into a container, and stirring at a high speed until a uniform white viscous mixture is obtained, namely the fluid loss agent composition;
comparative example 3
Step 1: dissolving 42 parts of acrylamide and 18 parts of lauryl methacrylate in deionized water, and adjusting the pH value to 14 to prepare a salt solution (1);
step 2: then adding the salt solution (1) into a reaction kettle under N 2 Under the protection condition, starting stirring and heating; when the temperature of the system rises to 70 ℃,2 parts of initiator ammonium persulfate is slowly dripped to react for 800min to form an intermediate polymer (1), and the test viscosity is 700MPa.s;
and step 3: dissolving 5 parts of 2-acrylamide-2-methylpropanesulfonic Acid (AMPS), 10 parts of maleic anhydride and 23 parts of acrylic acid in deionized water, and stirring until the materials are completely dissolved to form a salt solution (2); adding the obtained intermediate polymer (1) into a reaction kettle in N 2 Under the protection condition, openStirring and heating; slowly adding the salt solution (2) when the temperature of the system rises to 90 ℃, controlling the dropping speed to be 15min, and reacting for 90min to obtain the colorless viscous high-temperature-resistant salt-tolerant fluid loss agent; the test viscosity is 3000MPa.S, and the molecular weight is tested by refining and drying ethanol, which is shown in data table 1; (ii) a
And 4, step 4: adding 300 parts of the high-temperature-resistant salt-tolerant fluid loss agent obtained in the step 3 and 700 parts of calcium carbonate into a container, and stirring at a high speed until a uniform white viscous mixture is obtained, namely the fluid loss agent composition;
comparative example 4
Step 1: dissolving 60.5 parts of potassium m-styrene sulfonate, 26 parts of acrylamide and 13 parts of lauryl methacrylate in deionized water, and adjusting the pH value to 10 to prepare a salt solution (1);
step 2: adding the salt solution (1) into a 1L reaction kettle in N 2 Under the protection condition, starting stirring and heating; slowly dripping 0.5 part of initiator ammonium persulfate to react for 120min when the temperature of the system rises to 50 ℃ to obtain a colorless viscous high-temperature-resistant salt-tolerant fluid loss agent; the viscosity is tested, and the molecular weight is tested by refining and drying the ethanol at the same time, which is shown in data table 1;
and step 3: and (3) adding 100 parts of the high-temperature-resistant salt-tolerant fluid loss agent obtained in the step (3) and 400 parts of calcium carbonate into a container, and stirring at a high speed until a uniform white viscous mixture is obtained, namely the fluid loss agent composition.
Comparative example 5
Step 1: dissolving 88 parts of sodium m-styrene sulfonate, 4.8 parts of acrylamide and 0.2 part of lauryl methacrylate in deionized water, and adjusting the pH value to 12 to prepare a salt solution (1);
step 2: then adding the salt solution (1) into a reaction kettle under N 2 Under the protection condition, starting stirring and heating; slowly dripping 1 part of initiator ammonium persulfate to react for 120min when the temperature of the system rises to 40 ℃ to form an intermediate polymer (1), wherein the test viscosity is 300MPa.s;
and step 3: dissolving 0.12 part of 2-acrylamide-2-methylpropanesulfonic Acid (AMPS), 0.12 part of maleic anhydride and 5.76 parts of acrylic acid in deionized water, and stirring until the materials are completely dissolved to form a salt solution (2); adding the obtained intermediate polymer (1) into a reaction kettle in N 2 Under the protection condition, starting stirring and heating; slowly adding the salt solution (2) when the temperature of the system rises to 50 ℃, controlling the dropping speed to be 30min, and reacting for 100min to obtain the colorless viscous high-temperature-resistant salt-tolerant fluid loss agent; testing viscosity, and simultaneously refining ethanol and drying to test molecular weight, see data table 1; .
Comparative example 6
Commercial fluid loss agent polyvinyl alcohol PVA1788
Performance test
The fluid loss agent compositions of examples 1 to 12, the fluid loss agent compositions of comparative examples 1 to 5 and the fluid loss agent of comparative example 6 were subjected to performance tests, and specific test methods and test results were as follows:
preparation of the experiment:
(1) Treating fluid loss additive composition: uniformly spreading the fluid loss agent compositions obtained in the examples 1-12 and the comparative examples 1-5 on a tray, drying at 105 ℃ for 6 hours, and crushing and grinding to obtain a fluid loss agent poly solid product;
(2) Preparing cement paste, namely 800G of Jiahua G-grade oil well cement, 352G of deionized water (the water-cement ratio is 0.44), adding 20G of NaCl, and adding 1.5% of the obtained fluid loss additive solid product to obtain the cement paste for later use.
The test method comprises the following steps:
1. molecular weight detection method
The number average molecular weight (Mn), weight average molecular weight (Mw) and polydispersity index (PDI) of the synthesized fluid loss additive were tested by a differential refractometer using shimadzu model 20A gel permeation chromatograph.
A detector: RI detector
Mobile phase: taking 0.5mol/L sodium nitrate solution as a mobile phase, and the testing flow rate is 1.0ml/min
Injection volume: 50uL
Temperature of the column oven: 40 deg.C
Concentration: 3 to 5g/L
Standard sample preparation: polyethylene glycol as standard sample
2. Viscosity detection method
The test is carried out according to the method GB/T10247-2008.
3. Detection method for water loss of cement paste
The water loss of the cement paste is tested according to the GB/T19139-2003 oil well cement experimental method and the technical requirement of Q/SHCG 33-2016 oil well cement fluid loss agent.
4. Cement paste density detection method
Tested according to the SY/T5546-92 method.
5. Method for detecting initial consistency performance of cement paste
Tested according to the SY/T5546-92 method.
6. Method for detecting thickening time of cement paste
Tested according to the SY/T5546-92 method.
7. Cement stone compressive strength detection method
Tested according to the SY/T5546-92 method.
Results of Performance testing
Table 1 product Performance data
TABLE 2 Cement slurry Performance data
As can be seen from tables 1 and 2:
compared with the comparative examples 1 to 6, the fluid loss agent obtained by the block stepwise polymerization method in the examples of the invention has excellent comprehensive performance, especially in the aspects of high temperature resistance and salt tolerance, the polymer obtained by the invention is added into oil well cement, so that the water loss amount of the cement is reduced, the retardation time is delayed, and the tensile strength of the cement is higher, which shows that the addition of the fluid loss agent has slight retardation effect on the cement and reinforced cement strength; the high-temperature resistant rigid structure is regularly distributed in a polymer chain by a block polymerization method, so that the generated fluid loss agent has better tolerance in a high-temperature and high-salt environment; meanwhile, due to the introduction of a rigid structure and calcium salt, the overall mechanical property of the product is improved, so that the cement has better performance after being cured in the using process.
Claims (15)
1. A preparation method of a high-temperature-resistant salt-tolerant fluid loss additive composition comprises the following steps:
step 1: dissolving an alkaline monomer and a neutral monomer in water to form a salt solution (1), and adjusting the pH value to be alkaline;
step 2: adding the salt solution (1) into a reaction kettle under the condition of N 2 Under the protection condition, heating and then dripping an initiator for reaction to form an intermediate polymer (1);
and step 3: dissolving an acidic monomer in water to form a salt solution (2); adding the intermediate polymer (1) into a reaction kettle, heating and dropwise adding a salt solution (2) under the protection of N2, and reacting to obtain a fluid loss agent;
and 4, step 4: and (3) adding calcium carbonate into the fluid loss agent obtained in the step (3) according to a certain proportion, and stirring at a high speed until the mixture is uniform to obtain the high-temperature-resistant salt-tolerant fluid loss agent composition.
2. The method for preparing the high temperature resistant, salt resistant and fluid loss agent composition according to claim 1, wherein the fluid loss agent comprises, by weight, 100 parts, 5 to 88 parts of the basic monomer, 5 to 88 parts of the neutral monomer, 6 to 89 parts of the acidic monomer, and 0.1 to 5 parts of the initiator ammonium persulfate; the mass of the fluid loss agent accounts for 10-50% of the total mass of the high-temperature-resistant salt-tolerant fluid loss agent composition.
3. The preparation method of the high temperature resistant, salt tolerant and fluid loss additive composition according to claim 1, wherein the salt solution (1) in the step 1 has a solid content of 10-50% and the pH is adjusted to 8.0-14.0.
4. The preparation method of the high-temperature-resistant salt-tolerant fluid loss additive composition as claimed in claim 1, wherein in the step 2, the system temperature is raised to 40-70 ℃, the initiator is slowly dropped, the dropping speed of the initiator is 0.1-5.0 ml/min, and the viscosity of the intermediate polymer (1) is 100-2500 mPa.s.
5. The preparation method of the high-temperature-resistant salt-tolerant fluid loss additive composition as claimed in claim 1, wherein the solid content of the salt solution (2) in the step 3 is 20-50%; and (3) raising the temperature of the system to 50-90 ℃, slowly adding the salt solution (2), wherein the dropping speed of the salt solution (2) is 0.1-5.0 ml/min, and the viscosity of the obtained fluid loss agent after the reaction is finished is 2000-20000mPa.S.
6. The method for preparing the high-temperature-resistant, salt-resistant and fluid loss additive composition according to claim 1, wherein the basic monomer in step 1 is one or more selected from p-, o-, and m-alkene sulfonates containing benzene rings, and the structural formula is as follows:
Wherein n =0 to 10 Me = Na, K, ca, mg and Zn.
7. The method for preparing the high temperature resistant, salt resistant and fluid loss additive composition of claim 6, wherein the basic monomer in step 1 is selected from sodium p-styrenesulfonate or potassium p-styrenesulfonate.
8. The method for preparing the high temperature resistant, salt resistant and fluid loss additive composition according to claim 1, wherein the neutral monomer in step 1 has the following structural formula:
Wherein n =0 to 10m =0 to 15.
9. The method for preparing the high temperature resistant, salt tolerant, fluid loss additive composition according to claim 8, wherein the neutral monomer in step 1 is selected from one or more of methyl methacrylate, lauryl methacrylate, ethyl methacrylate, acrylamide, butyl methacrylate, and octyl methacrylate.
10. The method for preparing the high temperature resistant, salt resistant and fluid loss additive composition according to claim 9, wherein the neutral monomer in step 1 is a mixture of acrylamide and lauryl methacrylate in any proportion.
11. The method for preparing the high temperature resistant, salt resistant and fluid loss agent composition according to claim 1, wherein the initiator in step 2 is one selected from sodium persulfate, potassium persulfate and ammonium persulfate.
12. The method for preparing the high temperature resistant, salt resistant and fluid loss additive composition according to claim 1, wherein the acidic monomer in step 3 is one or more selected from allyl sulfonic acid, 2-acrylamide-2-methylpropanesulfonic Acid (AMPS), lignosulfonic acid, acrylic acid, maleic anhydride, hydroxyethyl acrylamide and hydroxymethyl acrylamide.
13. The method for preparing the high-temperature-resistant, salt-tolerant and fluid loss additive composition according to claim 12, wherein the acidic monomer in the step 3 is a mixture of 2-acrylamide-2-methylpropanesulfonic Acid (AMPS), maleic anhydride and acrylic acid in any proportion.
14. The method for preparing the high temperature resistant, salt tolerant, fluid loss agent reducing composition of claim 1, wherein in step 4 the calcium salt is selected from one or more of calcium carbonate, calcium gluconate, calcium hydrogen phosphate, calcium lactate, and calcium chloride.
15. The method of claim 14, wherein the calcium salt in step 4 is calcium carbonate.
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