CN117866139A - Multifunctional fluid loss agent for oil well cement paste and preparation method thereof - Google Patents
Multifunctional fluid loss agent for oil well cement paste and preparation method thereof Download PDFInfo
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- CN117866139A CN117866139A CN202211578655.8A CN202211578655A CN117866139A CN 117866139 A CN117866139 A CN 117866139A CN 202211578655 A CN202211578655 A CN 202211578655A CN 117866139 A CN117866139 A CN 117866139A
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- acrylamide
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- 239000004568 cement Substances 0.000 title claims abstract description 103
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 97
- 239000003129 oil well Substances 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 71
- ZGCZDEVLEULNLJ-UHFFFAOYSA-M benzyl-dimethyl-(2-prop-2-enoyloxyethyl)azanium;chloride Chemical compound [Cl-].C=CC(=O)OCC[N+](C)(C)CC1=CC=CC=C1 ZGCZDEVLEULNLJ-UHFFFAOYSA-M 0.000 claims abstract description 70
- IRQWEODKXLDORP-UHFFFAOYSA-N 4-ethenylbenzoic acid Chemical compound OC(=O)C1=CC=C(C=C)C=C1 IRQWEODKXLDORP-UHFFFAOYSA-N 0.000 claims abstract description 64
- 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 abstract description 56
- 239000002002 slurry Substances 0.000 claims abstract description 48
- 239000011541 reaction mixture Substances 0.000 claims abstract description 46
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 27
- 239000000654 additive Substances 0.000 claims abstract description 23
- 230000000996 additive effect Effects 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 90
- 239000000243 solution Substances 0.000 claims description 67
- 239000003999 initiator Substances 0.000 claims description 51
- 239000011259 mixed solution Substances 0.000 claims description 45
- 238000002156 mixing Methods 0.000 claims description 20
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium peroxydisulfate Substances [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 10
- VAZSKTXWXKYQJF-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)OOS([O-])=O VAZSKTXWXKYQJF-UHFFFAOYSA-N 0.000 claims description 10
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 9
- 150000002978 peroxides Chemical class 0.000 claims description 7
- 230000035484 reaction time Effects 0.000 claims description 4
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 3
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 3
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 5
- 150000003839 salts Chemical class 0.000 abstract description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 129
- 239000008186 active pharmaceutical agent Substances 0.000 description 25
- 238000003756 stirring Methods 0.000 description 25
- 230000000052 comparative effect Effects 0.000 description 20
- 229920000536 2-Acrylamido-2-methylpropane sulfonic acid Polymers 0.000 description 15
- XHZPRMZZQOIPDS-UHFFFAOYSA-N 2-Methyl-2-[(1-oxo-2-propenyl)amino]-1-propanesulfonic acid Chemical compound OS(=O)(=O)CC(C)(C)NC(=O)C=C XHZPRMZZQOIPDS-UHFFFAOYSA-N 0.000 description 15
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical class O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 14
- 239000000178 monomer Substances 0.000 description 11
- 230000001603 reducing effect Effects 0.000 description 11
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 8
- 230000015784 hyperosmotic salinity response Effects 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 6
- 239000003638 chemical reducing agent Substances 0.000 description 6
- 238000005260 corrosion Methods 0.000 description 6
- 230000007797 corrosion Effects 0.000 description 6
- 230000008719 thickening Effects 0.000 description 6
- 230000000694 effects Effects 0.000 description 4
- 239000011780 sodium chloride Substances 0.000 description 4
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000001569 carbon dioxide Substances 0.000 description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 239000013505 freshwater Substances 0.000 description 3
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 3
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910052717 sulfur Inorganic materials 0.000 description 3
- 239000011593 sulfur Substances 0.000 description 3
- 150000001768 cations Chemical class 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 230000036571 hydration Effects 0.000 description 2
- 238000006703 hydration reaction Methods 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 108010054404 Adenylyl-sulfate kinase Proteins 0.000 description 1
- 102100039024 Sphingosine kinase 1 Human genes 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 230000005465 channeling Effects 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000007580 dry-mixing Methods 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 238000010528 free radical solution polymerization reaction Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
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- 239000000047 product Substances 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
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- 229920006395 saturated elastomer Polymers 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 125000000542 sulfonic acid group Chemical group 0.000 description 1
Abstract
The invention provides a multifunctional fluid loss agent for oil well cement paste and a preparation method thereof. The preparation method of the fluid loss agent comprises the following steps: and (3) carrying out polymerization reaction on a reaction mixture containing 2-acrylamide-2-methylpropanesulfonic acid, acrylamide, p-vinylbenzoic acid and acryloyloxyethyl dimethylbenzyl ammonium chloride to obtain the multifunctional fluid loss agent for oil well cement paste. The multifunctional fluid loss additive for oil well cement slurry is prepared by the preparation method. The fluid loss agent provided by the invention has excellent high temperature resistance and salt resistance.
Description
Technical Field
The invention relates to a multifunctional fluid loss agent for oil well cement paste and a preparation method thereof, belonging to the technical field of oil field well cementation.
Background
Along with the appearance of deep wells and ultra-deep wells and the mature application of low-temperature and fresh water fluid loss agents, the development direction of the fluid loss agents is necessarily towards the high-temperature resistant and saturated salt water resistant directions. An excellent fluid loss additive should have the following five properties: the cement paste has excellent water loss reducing capacity, and the water loss can be controlled below 100mL by a small amount of the cement paste; secondly, the thickening time of cement paste can be controlled, but the strength development of cement paste is not influenced; thirdly, the salt resistance is high, and the water loss is not increased in a saline environment; fourth, can possess good compatibility with other admixtures; fifth, the cost is low, and the environment is not polluted.
In recent years, polymer fluid loss additives are fastest in development in oil well cement slurry additives, and new reports are continuously reported in various publications and patent documents. Although many products such as LW-1, FC-03, SK-1, TD-X, TD-S, J-2B, T, T-50A, W and 99 are well-suited for oilfield cementing, these fluid loss additives can only be used at temperatures below 160 ℃ and have good water loss reducing capacity only in fresh water mud.
Based on this, there is a need for improvements in fluid loss additives to further improve the temperature and salt resistance of the fluid loss additives.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a multifunctional fluid loss agent for oil well cement paste and a preparation method thereof. The fluid loss agent provided by the invention has good high temperature resistance and salt resistance.
In order to achieve the above object, the first aspect of the present invention provides a method for preparing a multifunctional fluid loss additive for oil well cement slurry, comprising the steps of:
and (3) carrying out polymerization reaction on a reaction mixture containing 2-acrylamide-2-methylpropanesulfonic Acid (AMPS), acrylamide (AM), p-vinylbenzoic acid and acryloyloxyethyl dimethyl benzyl ammonium chloride to obtain the multifunctional fluid loss agent for oil well cement paste.
In the above preparation method, preferably, the weight ratio of 2-acrylamide-2-methylpropanesulfonic acid, acrylamide, p-vinylbenzoic acid and acryloyloxyethyl dimethylbenzyl ammonium chloride is (1-10): (0.1-8): (0.4-8): (0.2-3).
In some embodiments of the present invention, the weight ratio of 2-acrylamido-2-methylpropanesulfonic acid, acrylamide, p-vinylbenzoic acid, and acryloyloxyethyl dimethylbenzyl ammonium chloride is (1-2): (7-8): (0.4-0.6): (0.7-0.8). Preferably, the weight ratio of the 2-acrylamide-2-methylpropanesulfonic acid, the acrylamide, the p-vinylbenzoic acid and the acryloyloxyethyl dimethylbenzyl ammonium chloride is 1:7:0.5:0.72. under the above proportion condition of four monomers, the prepared fluid loss agent has excellent high temperature resistance and salt resistance, and also has excellent dispersibility.
In some embodiments of the invention, the weight ratio of 2-acrylamido-2-methylpropanesulfonic acid, acrylamide, p-vinylbenzoic acid, and acryloyloxyethyl dimethylbenzyl ammonium chloride is (4.5-5.5): (6-7): (0.7-0.8): (0.8-1.2). Preferably, the weight ratio of the 2-acrylamide-2-methylpropanesulfonic acid, the acrylamide, the p-vinylbenzoic acid and the acryloyloxyethyl dimethylbenzyl ammonium chloride is 5:6.2:0.75:1. under the above proportion condition of four monomers, the prepared fluid loss agent has excellent high temperature resistance, salt resistance and thickening performance, and is especially suitable for a low-density cement slurry system.
In some embodiments of the invention, the weight ratio of 2-acrylamido-2-methylpropanesulfonic acid, acrylamide, p-vinylbenzoic acid, and acryloyloxyethyl dimethylbenzyl ammonium chloride is (7-8): (1-2): (7-8): (1-3). Preferably, the weight ratio of 2-acrylamide-2-methylpropanesulfonic acid, acrylamide, p-vinylbenzoic acid and acryloyloxyethyl dimethylbenzyl ammonium chloride is (7-8): 1.6:7.2:2. under the above proportion condition of four monomers, the prepared fluid loss agent has excellent high temperature resistance and salt resistance, and simultaneously has excellent corrosion resistance, and is particularly suitable for being applied to cement slurry systems with combined corrosion of carbon (such as carbon dioxide) and sulfur (such as hydrogen sulfide).
In some embodiments of the invention, the weight ratio of 2-acrylamide-2-methylpropanesulfonic acid, acrylamide, p-vinylbenzoic acid, and acryloyloxyethyl dimethylbenzyl ammonium chloride is (8-10): (0.1-0.3): (0.6-0.8): (0.2-0.4). Preferably, the weight ratio of the 2-acrylamide-2-methylpropanesulfonic acid, the acrylamide, the p-vinylbenzoic acid and the acryloyloxyethyl dimethylbenzyl ammonium chloride is (8-10): 0.1:0.7:0.3. under the above proportion condition of four monomers, the prepared fluid loss agent has excellent high temperature resistance and salt resistance, and is particularly suitable for high-density cement slurry systems, such as dispersant-type cement slurry systems added with weighting materials.
In the above preparation method, preferably, the reaction mixture further includes an initiator in an amount of 0.5 to 1% based on 100% by weight of the total reaction mixture. More preferably, the initiator comprises a peroxide solution having a mass concentration of 5-20%. More preferably, the peroxide solution includes one or a combination of several of ammonium persulfate solution, potassium persulfate solution, sodium persulfate solution, and the like.
In the above preparation method, preferably, the reaction mixture further includes water, the amount of 2-acrylamide-2-methylpropanesulfonic acid is 1 to 10%, the amount of acrylamide is 0.1 to 8%, the amount of p-vinylbenzoic acid is 0.4 to 8%, and the amount of acryloyloxyethyl dimethyl benzyl ammonium chloride is 0.2 to 3% based on 100% of the total weight of the reaction mixture.
In some embodiments of the invention, the 2-acrylamido-2-methylpropanesulfonic acid is used in an amount of 1-2%, the acrylamide is used in an amount of 7-8%, the para-vinylbenzoic acid is used in an amount of 0.4-0.6%, and the acryloyloxyethyl dimethylbenzyl ammonium chloride is used in an amount of 0.7-0.8% based on 100% total weight of the reaction mixture. Preferably, the amount of 2-acrylamido-2-methylpropanesulfonic acid is 1%, the amount of acrylamide is 7%, the amount of p-vinylbenzoic acid is 0.5% and the amount of acryloyloxyethyl dimethyl benzyl ammonium chloride is 0.72% based on 100% by weight of the total reaction mixture.
In some embodiments of the invention, the 2-acrylamido-2-methylpropanesulfonic acid is used in an amount of 4.5 to 5.5%, the acrylamide is used in an amount of 6 to 7%, the para-vinylbenzoic acid is used in an amount of 0.7 to 0.8%, and the acryloyloxyethyl dimethylbenzyl ammonium chloride is used in an amount of 0.8 to 1.2% based on 100% total weight of the reaction mixture. Preferably, the amount of 2-acrylamido-2-methylpropanesulfonic acid is 5%, the amount of acrylamide is 6.2%, the amount of p-vinylbenzoic acid is 0.75% and the amount of acryloyloxyethyl dimethyl benzyl ammonium chloride is 1% based on 100% by weight of the total reaction mixture.
In some embodiments of the invention, the 2-acrylamido-2-methylpropanesulfonic acid is used in an amount of 7-8%, the acrylamide is used in an amount of 1-2%, the para-vinylbenzoic acid is used in an amount of 7-8%, and the acryloyloxyethyl dimethylbenzyl ammonium chloride is used in an amount of 1-3% based on 100% total weight of the reaction mixture. Preferably, the amount of 2-acrylamido-2-methylpropanesulfonic acid is 7-8%, the amount of acrylamide is 1.6%, the amount of p-vinylbenzoic acid is 7.2% and the amount of acryloyloxyethyl dimethyl benzyl ammonium chloride is 2% based on 100% by weight of the total reaction mixture.
In some embodiments of the invention, the amount of 2-acrylamido-2-methylpropanesulfonic acid is 8-10%, the amount of acrylamide is 0.1-0.3%, the amount of p-vinylbenzoic acid is 0.6-0.8%, and the amount of acryloyloxyethyl dimethylbenzyl ammonium chloride is 0.2-0.4% based on 100% total weight of the reaction mixture. Preferably, the amount of 2-acrylamido-2-methylpropanesulfonic acid is 8-10%, the amount of acrylamide is 0.1%, the amount of p-vinylbenzoic acid is 0.7% and the amount of acryloyloxyethyl dimethyl benzyl ammonium chloride is 0.3% based on 100% by weight of the total reaction mixture.
According to a specific embodiment of the present invention, preferably, the above preparation method includes the steps of:
(1) Mixing 2-acrylamide-2-methylpropanesulfonic acid, acrylamide, p-vinylbenzoic acid and acryloyloxyethyl dimethyl benzyl ammonium chloride with water to obtain a mixed solution;
(2) And (3) mixing the mixed solution obtained in the step (1) with an initiator, and performing polymerization reaction to obtain the multifunctional fluid loss additive for oil well cement paste.
In the above preparation method, preferably, in the step (1), the pH of the mixed solution is 7.0 to 10.0, more preferably 8.0 to 9.0. The pH value of the mixed solution can be adjusted by adopting NaOH solution. The concentration of the NaOH solution can be conventionally set as required by those skilled in the art, and the present invention is not particularly limited thereto. For example, the concentration of the NaOH solution may be 0.05mol/L, 0.1mol/L, 0.2mol/L, or the like. It will be appreciated by those skilled in the art that the NaOH solution is also contained in the reaction mixture, but in small amounts, has little effect on the total weight of the reaction mixture.
In the above preparation method, the step (1) and/or the step (2) may be performed under stirring conditions, and the rotation speed of stirring may be adjusted conventionally by those skilled in the art.
In the above preparation method, preferably, the polymerization reaction temperature is 45-65 ℃ and the polymerization reaction time is 2-4h. More preferably, the polymerization reaction temperature is 50-60 ℃ and the polymerization reaction time is 3h.
The second aspect of the invention provides a multifunctional fluid loss additive for oil well cement slurry, which is prepared by the preparation method of the multifunctional fluid loss additive for oil well cement slurry.
The invention adopts a free radical aqueous solution polymerization method, takes 2-acrylamide-2-methylpropanesulfonic acid, acrylamide, p-vinylbenzoic acid and acryloyloxyethyl dimethylbenzyl ammonium chloride as monomers, designs the molecular structure of the fluid loss agent by controlling the weight proportion of the four monomers and controlling the temperature and time of the polymerization reaction, improves the rigidity of the fluid loss agent, further improves the temperature resistance, introduces a sulfonic acid group insensitive to attack by external cations into the molecular structure of the fluid loss agent, has stronger hydration capacity than carboxyl, and has stronger stability of the hydration film to the external cations, so that the salt resistance of the fluid loss agent is obviously enhanced. Experimental results show that the API water loss of the fluid loss agent prepared by the invention meets the requirement at 200 ℃, which indicates that the fluid loss agent has excellent high temperature resistance; the API water loss of the filtrate reducer prepared by the invention in the semi-saturated brine and the saturated brine is below 100mL, which indicates that the filtrate reducer has excellent salt resistance. Through a great deal of researches, the invention designs different weight proportions of the four monomers, so that the prepared fluid loss agent has different functions on the basis of excellent high temperature resistance and salt resistance, and is further suitable for different cement slurry systems with low density, high density and the like.
The fluid loss agent provided by the invention is a multifunctional fluid loss agent, is not only suitable for dry mixing or water mixing field processes, can be used in well temperature of 30-200 ℃, but also suitable for cement slurry systems with different densities of 1.15-2.20SG and fresh water, semi-saturated brine and saturated brine systems, and has the characteristics of small consumption and obvious water loss control effect; in addition, the utility model has the function of preventing gas channeling, and can be suitable for various systems.
The multifunctional fluid loss agent for the oil well cement paste is not easy to be degraded chemically and physically, and has weak effect on the rheological property of the cement paste; the compatibility with other additives is good; easy to manage and store; the cement slurry system added with the fluid loss agent has good slurry rheological property and adjustable slurry viscosity; the cement slurry system added with the fluid loss agent has good anti-channeling performance, has right-angle thickening function, the thickening transition time is less than or equal to 20min, and the static gelation transition time is less than or equal to 20min.
Detailed Description
The technical solution of the present invention will be described in detail below for a clearer understanding of technical features, objects and advantageous effects of the present invention, but should not be construed as limiting the scope of the present invention.
In some embodiments of the present invention, the present invention provides a method for preparing a multifunctional fluid loss additive for oil well cement slurries, comprising the steps of:
(1) Mixing 2-acrylamide-2-methylpropanesulfonic acid, acrylamide, p-vinylbenzoic acid and acryloyloxyethyl dimethyl benzyl ammonium chloride with water to obtain a mixed solution; the pH value of the mixed solution is 7.0-10.0, and NaOH solution can be adopted to adjust the pH value of the mixed solution;
(2) Mixing the mixed solution obtained in the step (1) with an initiator, and carrying out polymerization reaction at 45-65 ℃ for 2-4 hours to obtain the multifunctional fluid loss agent for oil well cement paste;
wherein the reaction mixture comprises 2-acrylamide-2-methylpropanesulfonic acid, acrylamide, p-vinylbenzoic acid, acryloxyethyl dimethyl benzyl ammonium chloride, water, an initiator, and optionally a NaOH solution;
the total weight of the reaction mixture is 100%, the dosage of the 2-acrylamide-2-methylpropanesulfonic acid is 1-2%, the dosage of the acrylamide is 7-8%, the dosage of the p-vinylbenzoic acid is 0.4-0.6%, the dosage of the acryloyloxyethyl dimethyl benzyl ammonium chloride is 0.7-0.8%, the dosage of the initiator is 0.5-1%, and the balance is water and a small amount of NaOH solution which can be selected to be adopted or not; preferably, the amount of 2-acrylamido-2-methylpropanesulfonic acid is 1%, the amount of acrylamide is 7%, the amount of p-vinylbenzoic acid is 0.5%, the amount of acryloyloxyethyl dimethylbenzyl ammonium chloride is 0.72%, the amount of initiator is 0.5-1%, the balance being water and optionally a small amount of NaOH solution, based on 100% of the total weight of the reaction mixture.
In the specific embodiment of the invention, the fluid loss agent prepared under the above proportion conditions of the four monomers has excellent high temperature resistance and salt resistance, and also has excellent dispersibility.
In other embodiments of the present invention, the present invention provides a method for preparing a multifunctional fluid loss additive for oil well cement slurries, comprising the steps of:
(1) Mixing 2-acrylamide-2-methylpropanesulfonic acid, acrylamide, p-vinylbenzoic acid and acryloyloxyethyl dimethyl benzyl ammonium chloride with water to obtain a mixed solution; the pH value of the mixed solution is 7.0-10.0, and NaOH solution can be adopted to adjust the pH value of the mixed solution;
(2) Mixing the mixed solution obtained in the step (1) with an initiator, and carrying out polymerization reaction at 45-65 ℃ for 2-4 hours to obtain the multifunctional fluid loss agent for oil well cement paste;
wherein the reaction mixture comprises 2-acrylamide-2-methylpropanesulfonic acid, acrylamide, p-vinylbenzoic acid, acryloxyethyl dimethyl benzyl ammonium chloride, water, an initiator, and optionally a NaOH solution;
based on 100 percent of the total weight of the reaction mixture, the dosage of the 2-acrylamide-2-methylpropanesulfonic acid is 4.5 to 5.5 percent, the dosage of the acrylamide is 6 to 7 percent, the dosage of the p-vinylbenzoic acid is 0.7 to 0.8 percent, the dosage of the acryloyloxyethyl dimethyl benzyl ammonium chloride is 0.8 to 1.2 percent, the dosage of the initiator is 0.5 to 1 percent, and the balance is water and a small amount of NaOH solution which can be adopted or not; preferably, the amount of 2-acrylamido-2-methylpropanesulfonic acid is 5%, the amount of acrylamide is 6.2%, the amount of p-vinylbenzoic acid is 0.75%, the amount of acryloyloxyethyl dimethyl benzyl ammonium chloride is 1%, the amount of initiator is 0.5-1%, the balance being water and optionally a small amount of NaOH solution, based on 100% of the total weight of the reaction mixture.
In the specific embodiment of the invention, the prepared fluid loss agent has excellent high temperature resistance, salt resistance and thickening performance under the proportion condition of four monomers, and is particularly suitable for a low-density cement slurry system.
In other embodiments of the present invention, the present invention provides a method for preparing a multifunctional fluid loss additive for oil well cement slurries, comprising the steps of:
(1) Mixing 2-acrylamide-2-methylpropanesulfonic acid, acrylamide, p-vinylbenzoic acid and acryloyloxyethyl dimethyl benzyl ammonium chloride with water to obtain a mixed solution; the pH value of the mixed solution is 7.0-10.0, and NaOH solution can be adopted to adjust the pH value of the mixed solution;
(2) Mixing the mixed solution obtained in the step (1) with an initiator, and carrying out polymerization reaction at 45-65 ℃ for 2-4 hours to obtain the multifunctional fluid loss agent for oil well cement paste;
wherein the reaction mixture comprises 2-acrylamide-2-methylpropanesulfonic acid, acrylamide, p-vinylbenzoic acid, acryloxyethyl dimethyl benzyl ammonium chloride, water, an initiator, and optionally a NaOH solution;
based on 100 percent of the total weight of the reaction mixture, the dosage of the 2-acrylamide-2-methylpropanesulfonic acid is 7-8 percent, the dosage of the acrylamide is 1-2 percent, the dosage of the p-vinylbenzoic acid is 7-8 percent, the dosage of the acryloyloxyethyl dimethyl benzyl ammonium chloride is 1-3 percent, the dosage of the initiator is 0.5-1 percent, and the balance is water and a small amount of NaOH solution which can be selected to be adopted or not; preferably, the amount of 2-acrylamido-2-methylpropanesulfonic acid is 7-8%, the amount of acrylamide is 1.6%, the amount of p-vinylbenzoic acid is 7.2%, the amount of acryloyloxyethyl dimethyl benzyl ammonium chloride is 2%, the amount of initiator is 0.5-1%, the balance being water and optionally a small amount of NaOH solution, based on 100% of the total weight of the reaction mixture.
In the specific embodiment of the invention, under the condition of the proportion of four monomers, the prepared fluid loss agent has excellent high temperature resistance and salt resistance, and simultaneously has excellent corrosion resistance, and is particularly suitable for being applied to cement slurry systems with combined corrosion of carbon (such as carbon dioxide) and sulfur (such as hydrogen sulfide).
In other embodiments of the present invention, the present invention provides a method for preparing a multifunctional fluid loss additive for oil well cement slurries, comprising the steps of:
(1) Mixing 2-acrylamide-2-methylpropanesulfonic acid, acrylamide, p-vinylbenzoic acid and acryloyloxyethyl dimethyl benzyl ammonium chloride with water to obtain a mixed solution; the pH value of the mixed solution is 7.0-10.0, and NaOH solution can be adopted to adjust the pH value of the mixed solution;
(2) Mixing the mixed solution obtained in the step (1) with an initiator, and carrying out polymerization reaction at 45-65 ℃ for 2-4 hours to obtain the multifunctional fluid loss agent for oil well cement paste;
wherein the reaction mixture comprises 2-acrylamide-2-methylpropanesulfonic acid, acrylamide, p-vinylbenzoic acid, acryloxyethyl dimethyl benzyl ammonium chloride, water, an initiator, and optionally a NaOH solution;
based on 100 percent of the total weight of the reaction mixture, the dosage of the 2-acrylamide-2-methylpropanesulfonic acid is 8-10 percent, the dosage of the acrylamide is 0.1-0.3 percent, the dosage of the p-vinylbenzoic acid is 0.6-0.8 percent, the dosage of the acryloyloxyethyl dimethyl benzyl ammonium chloride is 0.2-0.4 percent, the dosage of the initiator is 0.5-1 percent, and the balance is water and a small amount of NaOH solution which can be adopted or not; preferably, the amount of 2-acrylamido-2-methylpropanesulfonic acid is 8-10%, the amount of acrylamide is 0.1%, the amount of p-vinylbenzoic acid is 0.7%, the amount of acryloyloxyethyl dimethyl benzyl ammonium chloride is 0.3%, the amount of initiator is 0.5-1%, the balance being water and optionally a small amount of NaOH solution, based on 100% of the total weight of the reaction mixture.
In the specific embodiment of the invention, the fluid loss agent prepared under the above proportion conditions of the four monomers has excellent high temperature resistance and salt resistance, and is particularly suitable for high-density cement slurry systems, such as dispersant-type cement slurry systems added with weighting materials.
In the above-described embodiment, the concentration of the NaOH solution may be conventionally set by those skilled in the art as needed, and the present invention is not particularly limited thereto. For example, the concentration of the NaOH solution may be 0.05mol/L, 0.1mol/L, 0.2mol/L, or the like.
In the above embodiment, preferably, the pH of the mixed solution is 8.0 to 9.0.
In the above specific embodiment, preferably, the initiator comprises a peroxide solution, and the mass concentration of the peroxide solution is 5-20%. More preferably, the peroxide solution includes one or a combination of several of ammonium persulfate solution, potassium persulfate solution, sodium persulfate solution, and the like.
In the above embodiment, preferably, the polymerization reaction temperature is 50 to 60 ℃ and the polymerization reaction time is 3 hours.
In the above embodiments, step (1) and/or step (2) may be performed under stirring conditions, and the rotation speed of stirring may be adjusted conventionally by those skilled in the art.
Example 1
The embodiment provides a multifunctional fluid loss agent for oil well cement paste, which is prepared by the following steps:
(1) Mixing 2-acrylamide-2-methylpropanesulfonic acid, acrylamide, p-vinylbenzoic acid and acryloyloxyethyl dimethyl benzyl ammonium chloride with water under stirring to obtain a mixed solution; adjusting the pH value of the mixed solution to 8.0 by adopting NaOH solution;
(2) Slowly dripping an initiator into the mixed solution with the pH value adjusted, which is obtained in the step (1), at 50 ℃ under the stirring condition, and continuing to perform polymerization reaction for 3 hours under the stirring condition at 50 ℃ to obtain the multifunctional fluid loss agent for oil well cement paste;
wherein the reaction mixture comprises 2-acrylamide-2-methylpropanesulfonic acid, acrylamide, p-vinylbenzoic acid, acryloxyethyl dimethyl benzyl ammonium chloride, water, an initiator and a NaOH solution;
the total weight of the reaction mixture is 100%, the dosage of the 2-acrylamide-2-methylpropanesulfonic acid is 1%, the dosage of the acrylamide is 7%, the dosage of the p-vinylbenzoic acid is 0.5%, the dosage of the acryloyloxyethyl dimethyl benzyl ammonium chloride is 0.72%, the dosage of the initiator is 0.5%, and the balance is water and a small amount of NaOH solution;
the initiator is ammonium persulfate solution with the mass concentration of 10%.
The fluid loss agent prepared by the embodiment has excellent high temperature resistance and salt resistance, and also has excellent dispersibility.
Example 2
The embodiment provides a multifunctional fluid loss agent for oil well cement paste, which is prepared by the following steps:
(1) Mixing 2-acrylamide-2-methylpropanesulfonic acid, acrylamide, p-vinylbenzoic acid and acryloyloxyethyl dimethyl benzyl ammonium chloride with water under stirring to obtain a mixed solution; adjusting the pH value of the mixed solution to 9.0 by adopting NaOH solution;
(2) Slowly dripping an initiator into the mixed solution with the pH value adjusted, which is obtained in the step (1), under the condition of stirring at 55 ℃, and continuing to perform polymerization reaction for 3 hours under the condition of stirring at 55 ℃ to obtain the multifunctional fluid loss agent for oil well cement paste;
wherein the reaction mixture comprises 2-acrylamide-2-methylpropanesulfonic acid, acrylamide, p-vinylbenzoic acid, acryloxyethyl dimethyl benzyl ammonium chloride, water, an initiator and a NaOH solution;
the total weight of the reaction mixture is 100%, the dosage of the 2-acrylamide-2-methylpropanesulfonic acid is 5%, the dosage of the acrylamide is 6.2%, the dosage of the p-vinylbenzoic acid is 0.75%, the dosage of the acryloyloxyethyl dimethyl benzyl ammonium chloride is 1%, the dosage of the initiator is 0.7%, and the balance is water and a small amount of NaOH solution;
the initiator is ammonium persulfate solution with the mass concentration of 10%.
The fluid loss agent prepared by the embodiment has excellent high temperature resistance, salt resistance and thickening performance, and is particularly suitable for a low-density cement slurry system.
Example 3
The embodiment provides a multifunctional fluid loss agent for oil well cement paste, which is prepared by the following steps:
(1) Mixing 2-acrylamide-2-methylpropanesulfonic acid, acrylamide, p-vinylbenzoic acid and acryloyloxyethyl dimethyl benzyl ammonium chloride with water under stirring to obtain a mixed solution; adjusting the pH value of the mixed solution to 8.0 by adopting NaOH solution;
(2) Slowly dripping an initiator into the mixed solution with the pH value adjusted, which is obtained in the step (1), under the condition of stirring at 55 ℃, and continuing to perform polymerization reaction for 3 hours under the condition of stirring at 55 ℃ to obtain the multifunctional fluid loss agent for oil well cement paste;
wherein the reaction mixture comprises 2-acrylamide-2-methylpropanesulfonic acid, acrylamide, p-vinylbenzoic acid, acryloxyethyl dimethyl benzyl ammonium chloride, water, an initiator and a NaOH solution;
based on 100 percent of the total weight of the reaction mixture, the dosage of the 2-acrylamide-2-methylpropanesulfonic acid is 7.5 percent, the dosage of the acrylamide is 1.6 percent, the dosage of the p-vinylbenzoic acid is 7.2 percent, the dosage of the acryloyloxyethyl dimethyl benzyl ammonium chloride is 2 percent, the dosage of the initiator is 1 percent, and the balance is water and a small amount of NaOH solution;
the initiator is ammonium persulfate solution with the mass concentration of 10%.
The fluid loss agent prepared by the embodiment has excellent high temperature resistance and salt resistance, and simultaneously has excellent corrosion resistance, and is particularly suitable for being applied to cement slurry systems with combined corrosion of carbon (such as carbon dioxide) and sulfur (such as hydrogen sulfide).
Example 4
The embodiment provides a multifunctional fluid loss agent for oil well cement paste, which is prepared by the following steps:
(1) Mixing 2-acrylamide-2-methylpropanesulfonic acid, acrylamide, p-vinylbenzoic acid and acryloyloxyethyl dimethyl benzyl ammonium chloride with water under stirring to obtain a mixed solution; adjusting the pH value of the mixed solution to 8.0 by adopting NaOH solution;
(2) Slowly dripping an initiator into the mixed solution with the pH value adjusted, which is obtained in the step (1), under the condition of 60 ℃ and stirring, and continuing to perform polymerization reaction for 3 hours under the condition of 60 ℃ and stirring to obtain the multifunctional fluid loss agent for oil well cement paste;
wherein the reaction mixture comprises 2-acrylamide-2-methylpropanesulfonic acid, acrylamide, p-vinylbenzoic acid, acryloxyethyl dimethyl benzyl ammonium chloride, water, an initiator and a NaOH solution;
the total weight of the reaction mixture is 100%, the dosage of the 2-acrylamide-2-methylpropanesulfonic acid is 9%, the dosage of the acrylamide is 0.1%, the dosage of the p-vinylbenzoic acid is 0.7%, the dosage of the acryloyloxyethyl dimethyl benzyl ammonium chloride is 0.3%, the dosage of the initiator is 0.5%, and the balance is water and a small amount of NaOH solution;
the initiator is ammonium persulfate solution with the mass concentration of 10%.
The fluid loss agent prepared by the embodiment has excellent high temperature resistance and salt resistance, and is particularly suitable for a high-density cement slurry system, such as a dispersant-type cement slurry system added with a weighting material.
Comparative example 1
The comparative example provides a preparation method of a fluid loss agent, which is prepared through the following steps:
(1) Mixing 2-acrylamide-2-methylpropanesulfonic acid, acrylamide, acrylic acid and acryloyloxyethyl dimethylbenzyl ammonium chloride with water under stirring to obtain a mixed solution; adjusting the pH value of the mixed solution to 8.0 by adopting NaOH solution;
(2) Slowly dripping an initiator into the mixed solution with the pH value adjusted, which is obtained in the step (1), under the condition of stirring at 55 ℃, and continuing to perform polymerization reaction for 3 hours under the condition of stirring at 55 ℃ to obtain the multifunctional fluid loss agent for oil well cement paste;
wherein the reaction mixture comprises 2-acrylamide-2-methylpropanesulfonic acid, acrylamide, acrylic acid, acryloxyethyl dimethyl benzyl ammonium chloride, water, an initiator and a NaOH solution;
the total weight of the reaction mixture is 100%, the dosage of the 2-acrylamide-2-methylpropanesulfonic acid is 1%, the dosage of the acrylamide is 7%, the dosage of the acrylic acid is 0.5%, the dosage of the acryloyloxyethyl dimethyl benzyl ammonium chloride is 0.72%, the dosage of the initiator is 0.5%, and the balance is water and a small amount of NaOH solution;
the initiator is ammonium persulfate solution with the mass concentration of 10%.
Comparative example 2
The comparative example provides a preparation method of a fluid loss agent, which is prepared through the following steps:
(1) Mixing 2-acrylamide-2-methylpropanesulfonic acid, acrylamide, maleic anhydride and acryloyloxyethyl dimethylbenzyl ammonium chloride with water under stirring to obtain a mixed solution; adjusting the pH value of the mixed solution to 8.0 by adopting NaOH solution;
(2) Slowly dripping an initiator into the mixed solution with the pH value adjusted, which is obtained in the step (1), under the condition of stirring at 55 ℃, and continuing to perform polymerization reaction for 3 hours under the condition of stirring at 55 ℃ to obtain the multifunctional fluid loss agent for oil well cement paste;
wherein the reaction mixture comprises 2-acrylamide-2-methylpropanesulfonic acid, acrylamide, maleic anhydride, acryloyloxyethyl dimethyl benzyl ammonium chloride, water, an initiator and a NaOH solution;
based on 100 percent of the total weight of the reaction mixture, the dosage of the 2-acrylamide-2-methylpropanesulfonic acid is 5 percent, the dosage of the acrylamide is 6.2 percent, the dosage of the maleic anhydride is 0.75 percent, the dosage of the acryloyloxyethyl dimethyl benzyl ammonium chloride is 1 percent, the dosage of the initiator is 0.7 percent, and the balance is water and a small amount of NaOH solution;
the initiator is ammonium persulfate solution with the mass concentration of 10%.
Comparative example 3
The comparative example provides a preparation method of a fluid loss agent, which is prepared through the following steps:
(1) Mixing 2-acrylamide-2-methylpropanesulfonic acid, acrylamide, p-vinylbenzoic acid and acryloyloxyethyl dimethyl benzyl ammonium chloride with water under stirring to obtain a mixed solution; adjusting the pH value of the mixed solution to 8.0 by adopting NaOH solution;
(2) Slowly dripping an initiator into the mixed solution with the pH value adjusted, which is obtained in the step (1), under the condition of stirring at 55 ℃, and continuing to perform polymerization reaction for 3 hours under the condition of stirring at 55 ℃ to obtain the multifunctional fluid loss agent for oil well cement paste;
wherein the reaction mixture comprises 2-acrylamide-2-methylpropanesulfonic acid, acrylamide, p-vinylbenzoic acid, acryloxyethyl dimethyl benzyl ammonium chloride, water, an initiator and a NaOH solution;
based on 100 percent of the total weight of the reaction mixture, the dosage of the 2-acrylamide-2-methylpropanesulfonic acid is 3 percent, the dosage of the acrylamide is 2 percent, the dosage of the p-vinylbenzoic acid is 3 percent, the dosage of the acryloyloxyethyl dimethyl benzyl ammonium chloride is 2 percent, the dosage of the initiator is 0.5 percent, and the balance is water and a small amount of NaOH solution;
the initiator is ammonium persulfate solution with the mass concentration of 10%.
Test case
The fluid loss additives prepared in examples 1 to 4 and comparative examples 1 to 3 were subjected to the following performance tests.
1. Dehydration reducing performance of fluid loss agent
The water loss reducing agent prepared in example 1 was tested at 90℃for water loss reducing properties at 0.5%, 1%, 1.5%, 2%, 2.5%, 5% and 7% by weight of cement ash, and the results are shown in Table 1.
Wherein, the formula of the cement paste is as follows: 100 parts by weight of G-grade oil well cement, 0.5-7 parts by weight of a fluid loss agent and 42 parts by weight of water; the density of the cement slurry was 1.90SG.
Table 1 water loss reducing properties of the fluid loss agent of example 1
| Fluid loss agent addition (%) | API water loss (mL) at 90 DEG C |
| 0.5 | 77 |
| 1 | 65 |
| 1.5 | 45 |
| 2 | 32 |
| 2.5 | 20 |
| 5 | 10 |
| 7 | 5 |
As can be seen from Table 1, in the cement slurry with the density of 1.90SG at 90 ℃, when the dosage of the fluid loss agent is 0.5-7%, the API water loss is less than 100mL, and when the dosage is increased from 0.5% to 7%, the API water loss is reduced from 77mL to 5mL.
The water loss reducing agent prepared in example 2 was tested at 90℃for water loss reducing properties at 0.5%, 1%, 1.5%, 2%, 2.5%, 5% and 7% by weight of cement ash, and the results are shown in Table 2.
Wherein, the formula of the cement paste is as follows: 100 parts by weight of G-grade oil well cement, 0.5-7 parts by weight of a fluid loss agent and 44 parts by weight of water; the cement paste had a density of 1.85SG.
Table 2 water loss reducing properties of the fluid loss agent of example 2
| Fluid loss agent addition (%) | API water loss (mL) at 90 DEG C |
| 0.5 | 75 |
| 1 | 61 |
| 1.5 | 43 |
| 2 | 30 |
| 2.5 | 22 |
| 5 | 11 |
| 7 | 6 |
As can be seen from Table 2, in the cement slurry with the density of 1.85SG at 90 ℃, when the dosage of the fluid loss agent is 0.5-7%, the API water loss is less than 100mL, and when the dosage is increased from 0.5% to 7%, the API water loss is reduced from 75mL to 6mL.
The water loss reducing agent prepared in example 3 was tested at 90℃for water loss reducing properties at 0.5%, 1%, 1.5%, 2%, 2.5%, 5% and 7% by weight of cement ash, and the results are shown in Table 3.
Wherein, the formula of the cement paste is as follows: 100 parts by weight of G-grade oil well cement, 0.5-7 parts by weight of a fluid loss agent and 44 parts by weight of water; the cement paste had a density of 1.85SG.
TABLE 3 Water loss reduction Property of fluid loss agent of example 3
As can be seen from Table 3, in the cement slurry with the density of 1.85SG at 90 ℃, when the dosage of the fluid loss agent is 0.5-7%, the API water loss is less than 100mL, and when the dosage is increased from 0.5% to 7%, the API water loss is reduced from 78mL to 6mL.
The water loss reducing agent prepared in example 4 was tested at 90℃for water loss reducing properties at 0.5%, 1%, 1.5%, 2%, 2.5%, 5% and 7% by weight of cement ash, and the results are shown in Table 4.
Wherein, the formula of the cement paste is as follows: 100 parts by weight of G-grade oil well cement, 0.5-7 parts by weight of a fluid loss agent and 31 parts by weight of water; the density of the cement slurry was 2.02SG.
Table 4 water loss reducing properties of the fluid loss agent of example 4
| Fluid loss agent addition (%) | API water loss (mL) at 90 DEG C |
| 0.5 | 69 |
| 1 | 56 |
| 1.5 | 40 |
| 2 | 30 |
| 2.5 | 21 |
| 5 | 11 |
| 7 | 5 |
As can be seen from Table 4, in the cement slurry with a density of 2.02SG at 90 ℃, the API water loss is 100mL or less when the amount of the fluid loss agent is 0.5-7%, and the API water loss is reduced from 69mL to 5mL when the amount is increased from 0.5% to 7%.
As can be seen from the test results, with the increase of the dosage of the fluid loss additive in the embodiment of the invention, the fluid loss additive molecules in unit volume in the cement slurry system are increased, the adsorbed groups generated by cement particles are also increased, and the cross-linking points of the net structure of the whole cement slurry system are also more, so that the compactness of the structure of the cement slurry filter cake is better, and the fluid loss reducing capability is stronger.
2. High temperature resistance of fluid loss agent
The fluid loss agent prepared in test example 1 was added to cement slurry, and the API fluid loss was measured at 70-200 ℃ and the results are shown in table 5. Wherein, the formula of the cement paste is as follows: 100 parts by weight of G-grade oil well cement, 2 parts by weight of a fluid loss agent and 42 parts by weight of water; the density of the cement slurry was 1.90SG.
TABLE 5 high temperature resistance of fluid loss agent of example 1
As can be seen from Table 5, the temperature of the fluid loss agent is increased from 70 ℃ to 200 ℃ and the API fluid loss amount is only increased from 30mL to 40mL, and the temperature is increased to 90 ℃, 130 ℃, 160 ℃ and 200 ℃ and the fluid loss amount is increased to a certain extent, but the increment is within 10mL, which shows that the fluid loss agent prepared in the embodiment 1 has excellent high temperature resistance.
The fluid loss agents prepared in examples 1 to 4 and comparative examples 1 to 3 were tested for API fluid loss at 200℃after being added to cement slurries, and the results are shown in Table 6. Wherein, the formula of the cement paste is as follows: 100 parts by weight of G-grade oil well cement, 2 parts by weight of a fluid loss agent and 42 parts by weight of water; the density of the cement slurry was 1.90SG.
TABLE 6 API Water loss at 200℃for fluid loss additives of examples 1-4 and comparative examples 1-3
| Numbering device | Testing temperature (. Degree. C.) | API water loss (mL) |
| Example 1 | 200 | 40 |
| Example 2 | 200 | 42 |
| Example 3 | 200 | 36 |
| Example 4 | 200 | 45 |
| Comparative example 1 | 200 | 86 |
| Comparative example 2 | 200 | 98 |
| Comparative example 3 | 200 | 79 |
As can be seen from Table 6, the high temperature resistance of the fluid loss agent provided by the example of the present invention is superior to that of the comparative example.
3. Salt resistance of fluid loss agent
(1) EXAMPLE 1 salt tolerance in half saturated brine
The fluid loss agent prepared in example 1 was tested for salt resistance in semi-saturated brine after being added to cement slurry, and the results are shown in table 7.
Wherein, the formula of the cement paste is as follows: 100 parts by weight of G-grade oil well cement, 3 parts by weight of a fluid loss agent, 42 parts by weight of water and 7.5 parts by weight of NaCl; the density of the cement slurry was 1.90SG.
TABLE 7 salt tolerance of fluid loss agent of example 1 in semi-saturated brine
| Numbering device | Testing temperature (. Degree. C.) | API water loss (mL) |
| 1 | 90 | 36 |
| 2 | 120 | 42 |
| 3 | 140 | 46 |
| 4 | 160 | 50 |
| 5 | 200 | 57 |
As can be seen from Table 7, the API water loss of the fluid loss agent prepared in example 1 in the semi-saturated brine is below 100mL at 90-200 ℃, which indicates that the fluid loss agent prepared in example 1 has excellent salt tolerance.
(2) EXAMPLE 1 salt tolerance in saturated saline
The fluid loss agent prepared in example 1 was tested for salt resistance in saturated brine after being added to cement slurry, and the results are shown in table 8.
Wherein, the formula of the cement paste is as follows: 100 parts by weight of G-grade oil well cement, 4 parts by weight of a fluid loss agent, 42 parts by weight of water and 15 parts by weight of NaCl; the density of the cement slurry was 1.90SG.
TABLE 8 salt tolerance of fluid loss agent of example 1 in saturated brine
| Numbering device | Testing temperature (. Degree. C.) | API water loss (mL) |
| 1 | 90 | 50 |
| 2 | 120 | 56 |
| 3 | 160 | 62 |
| 4 | 200 | 69 |
As can be seen from Table 8, the API water loss amounts of the fluid loss agent prepared in example 1 in saturated brine are all below 100mL at 90-200 ℃, which indicates that the fluid loss agent prepared in example 1 has excellent salt tolerance.
(3) Other examples and comparative examples salt tolerance in saturated brine
The fluid loss agents prepared in examples 1 to 4 and comparative examples 1 to 3 were tested for API fluid loss in saturated brine at 200 ℃ after being added to cement slurries, and the results are shown in table 9.
Wherein, the formula of the cement paste is as follows: 100 parts by weight of G-grade oil well cement, 4 parts by weight of a fluid loss agent, 42 parts by weight of water and 15 parts by weight of NaCl; the density of the cement slurry was 1.90SG.
TABLE 9 API Water loss of fluid loss agents of examples 1-4 and comparative examples 1-3 at 200℃in saturated brine
| Numbering device | Testing temperature (. Degree. C.) | API water loss (mL) |
| Example 1 | 200 | 69 |
| Example 2 | 200 | 72 |
| Example 3 | 200 | 64 |
| Example 4 | 200 | 65 |
| Comparative example 1 | 200 | 112 |
| Comparative example 2 | 200 | 128 |
| Comparative example 3 | 200 | 106 |
From the above experimental data, the fluid loss agent provided by the embodiment of the invention has better high temperature and salt resistance than the fluid loss agent of the comparative example.
Claims (10)
1. A preparation method of a multifunctional fluid loss agent for oil well cement paste comprises the following steps:
and (3) carrying out polymerization reaction on a reaction mixture containing 2-acrylamide-2-methylpropanesulfonic acid, acrylamide, p-vinylbenzoic acid and acryloyloxyethyl dimethylbenzyl ammonium chloride to obtain the multifunctional fluid loss agent for oil well cement paste.
2. The preparation method according to claim 1, wherein the weight ratio of 2-acrylamide-2-methylpropanesulfonic acid, acrylamide, p-vinylbenzoic acid and acryloyloxyethyl dimethylbenzyl ammonium chloride is (1-10): (0.1-8): (0.4-8): (0.2-3).
3. The production method according to claim 1 or 2, wherein the weight ratio of 2-acrylamide-2-methylpropanesulfonic acid, acrylamide, p-vinylbenzoic acid and acryloyloxyethyl dimethylbenzyl ammonium chloride is (1-2): (7-8): (0.4-0.6): (0.7-0.8);
preferably, the weight ratio of the 2-acrylamide-2-methylpropanesulfonic acid, the acrylamide, the p-vinylbenzoic acid and the acryloyloxyethyl dimethylbenzyl ammonium chloride is 1:7:0.5:0.72.
4. the production method according to claim 1 or 2, wherein the weight ratio of 2-acrylamide-2-methylpropanesulfonic acid, acrylamide, p-vinylbenzoic acid and acryloyloxyethyl dimethylbenzyl ammonium chloride is (4.5-5.5): (6-7): (0.7-0.8): (0.8-1.2);
preferably, the weight ratio of the 2-acrylamide-2-methylpropanesulfonic acid, the acrylamide, the p-vinylbenzoic acid and the acryloyloxyethyl dimethylbenzyl ammonium chloride is 5:6.2:0.75:1.
5. the production method according to claim 1 or 2, wherein the weight ratio of 2-acrylamide-2-methylpropanesulfonic acid, acrylamide, p-vinylbenzoic acid and acryloyloxyethyl dimethylbenzyl ammonium chloride is (7-8): (1-2): (7-8): (1-3);
preferably, the weight ratio of 2-acrylamide-2-methylpropanesulfonic acid, acrylamide, p-vinylbenzoic acid and acryloyloxyethyl dimethylbenzyl ammonium chloride is (7-8): 1.6:7.2:2.
6. the production method according to claim 1 or 2, wherein the weight ratio of 2-acrylamide-2-methylpropanesulfonic acid, acrylamide, p-vinylbenzoic acid and acryloyloxyethyl dimethylbenzyl ammonium chloride is (8-10): (0.1-0.3): (0.6-0.8): (0.2-0.4);
preferably, the weight ratio of the 2-acrylamide-2-methylpropanesulfonic acid, the acrylamide, the p-vinylbenzoic acid and the acryloyloxyethyl dimethylbenzyl ammonium chloride is (8-10): 0.1:0.7:0.3.
7. the method of claim 1, wherein the reaction mixture further comprises an initiator in an amount of 0.5-1% based on 100% total weight of the reaction mixture;
preferably, the initiator comprises a peroxide solution, the mass concentration of which is 5-20%;
more preferably, the peroxide solution comprises one or a combination of several of ammonium persulfate solution, potassium persulfate solution and sodium persulfate solution;
preferably, the reaction mixture further comprises water.
8. The preparation method according to claim 1, wherein the preparation method comprises the steps of:
(1) Mixing 2-acrylamide-2-methylpropanesulfonic acid, acrylamide, p-vinylbenzoic acid and acryloyloxyethyl dimethyl benzyl ammonium chloride with water to obtain a mixed solution;
(2) Mixing the mixed solution obtained in the step (1) with an initiator, and performing polymerization reaction to obtain the multifunctional fluid loss additive for oil well cement paste;
preferably, in step (1), the pH of the mixed solution is 7.0-10.0, more preferably 8.0-9.0.
9. The production method according to claim 1 or 8, wherein the polymerization reaction temperature is 45 to 65 ℃ and the polymerization reaction time is 2 to 4 hours;
preferably, the temperature of the polymerization reaction is 50-60 ℃, and the time of the polymerization reaction is 3h.
10. A multifunctional fluid loss additive for oil well cement slurry prepared by the method for preparing a multifunctional fluid loss additive for oil well cement slurry according to any one of claims 1 to 9.
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