CN117820565A - High-temperature-resistant and composite-salt-resistant polymer filtrate reducer and preparation method thereof - Google Patents
High-temperature-resistant and composite-salt-resistant polymer filtrate reducer and preparation method thereof Download PDFInfo
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- 239000000706 filtrate Substances 0.000 title claims abstract description 64
- 239000003638 chemical reducing agent Substances 0.000 title claims abstract description 60
- 229920000642 polymer Polymers 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title abstract description 30
- 150000003839 salts Chemical class 0.000 claims abstract description 62
- 239000002131 composite material Substances 0.000 claims abstract description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000000178 monomer Substances 0.000 claims abstract description 27
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 claims abstract description 21
- 229940051841 polyoxyethylene ether Drugs 0.000 claims abstract description 21
- 229920000056 polyoxyethylene ether Polymers 0.000 claims abstract description 21
- 239000003999 initiator Substances 0.000 claims abstract description 20
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 18
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 18
- 239000006184 cosolvent Substances 0.000 claims abstract description 16
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 15
- 125000000623 heterocyclic group Chemical group 0.000 claims abstract description 15
- FDRCDNZGSXJAFP-UHFFFAOYSA-M sodium chloroacetate Chemical compound [Na+].[O-]C(=O)CCl FDRCDNZGSXJAFP-UHFFFAOYSA-M 0.000 claims abstract description 15
- 229920000536 2-Acrylamido-2-methylpropane sulfonic acid Polymers 0.000 claims abstract description 7
- XHZPRMZZQOIPDS-UHFFFAOYSA-N 2-Methyl-2-[(1-oxo-2-propenyl)amino]-1-propanesulfonic acid Chemical compound OS(=O)(=O)CC(C)(C)NC(=O)C=C XHZPRMZZQOIPDS-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims description 27
- 238000007334 copolymerization reaction Methods 0.000 claims description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 239000000654 additive Substances 0.000 claims description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- 230000000996 additive effect Effects 0.000 claims description 16
- 238000005956 quaternization reaction Methods 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 14
- 239000011259 mixed solution Substances 0.000 claims description 14
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 12
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 11
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 11
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims description 11
- 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 8
- 238000004821 distillation Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- OSSNTDFYBPYIEC-UHFFFAOYSA-N 1-ethenylimidazole Chemical compound C=CN1C=CN=C1 OSSNTDFYBPYIEC-UHFFFAOYSA-N 0.000 claims description 6
- 239000012295 chemical reaction liquid Substances 0.000 claims description 6
- 230000007935 neutral effect Effects 0.000 claims description 6
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- 239000012670 alkaline solution Substances 0.000 claims description 4
- OZFIGURLAJSLIR-UHFFFAOYSA-N 1-ethenyl-2h-pyridine Chemical compound C=CN1CC=CC=C1 OZFIGURLAJSLIR-UHFFFAOYSA-N 0.000 claims description 3
- 239000003153 chemical reaction reagent Substances 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 2
- 238000005553 drilling Methods 0.000 abstract description 29
- 239000012530 fluid Substances 0.000 abstract description 24
- 238000001914 filtration Methods 0.000 abstract description 11
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 abstract description 10
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 abstract description 6
- 239000011575 calcium Substances 0.000 abstract description 6
- 229910052791 calcium Inorganic materials 0.000 abstract description 6
- 230000001603 reducing effect Effects 0.000 abstract description 6
- 230000032683 aging Effects 0.000 abstract description 5
- 239000011780 sodium chloride Substances 0.000 abstract description 5
- 230000000052 comparative effect Effects 0.000 description 21
- 230000000694 effects Effects 0.000 description 12
- 238000006703 hydration reaction Methods 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 239000007789 gas Substances 0.000 description 6
- -1 alkenyl sulfonic acid Chemical compound 0.000 description 5
- 230000036571 hydration Effects 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 239000000440 bentonite Substances 0.000 description 4
- 229910000278 bentonite Inorganic materials 0.000 description 4
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 4
- 239000012267 brine Substances 0.000 description 4
- 229920001577 copolymer Polymers 0.000 description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 230000009467 reduction Effects 0.000 description 4
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000004927 clay Substances 0.000 description 3
- 238000004132 cross linking Methods 0.000 description 3
- 230000006866 deterioration Effects 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 230000002209 hydrophobic effect Effects 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000007664 blowing Methods 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 230000000977 initiatory effect Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002114 nanocomposite Substances 0.000 description 2
- 239000003345 natural gas Substances 0.000 description 2
- 239000003209 petroleum derivative Substances 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- 125000000542 sulfonic acid group Chemical group 0.000 description 2
- 229920001059 synthetic polymer Polymers 0.000 description 2
- FSSPGSAQUIYDCN-UHFFFAOYSA-N 1,3-Propane sultone Chemical group O=S1(=O)CCCO1 FSSPGSAQUIYDCN-UHFFFAOYSA-N 0.000 description 1
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 1
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- 241001391944 Commicarpus scandens Species 0.000 description 1
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical group C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 150000008064 anhydrides Chemical group 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 230000000887 hydrating effect Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000009533 lab test Methods 0.000 description 1
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- 238000005580 one pot reaction Methods 0.000 description 1
- 125000006353 oxyethylene group Chemical group 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000012264 purified product Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000004289 sodium hydrogen sulphite Substances 0.000 description 1
- MNCGMVDMOKPCSQ-UHFFFAOYSA-M sodium;2-phenylethenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C=CC1=CC=CC=C1 MNCGMVDMOKPCSQ-UHFFFAOYSA-M 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229920001567 vinyl ester resin Polymers 0.000 description 1
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- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention provides a high-temperature-resistant and composite-salt-resistant polymer filtrate reducer, which is prepared by copolymerizing a comonomer, a cosolvent, sodium chloroacetate and an initiator in water; the comonomer comprises acrylamide, 2-acrylamido-2-methylpropanesulfonic acid, allyl polyoxyethylene ether and vinyl N heterocyclic monomer. The preparation method of the high-temperature-resistant and composite-salt-resistant polymer filtrate reducer is simple and easy to operate, has good temperature resistance, salt resistance and calcium resistance, the temperature resistance can reach 200 ℃, and the NaCl resistance can reach 15% and CaCl resistance 2 Up to 1%; and at a high temperatureThe composite salt still has excellent filtration reducing capability after aging, and has wide application prospect in the field of high-temperature-resistant high-salt water-based drilling fluid.
Description
Technical Field
The invention belongs to the technical field of oilfield chemistry, relates to a fluid loss additive for water-based drilling fluid, and particularly relates to a high-temperature-resistant and composite-salt-resistant polymer fluid loss additive and a preparation method thereof.
Background
With the rapid increase of petroleum and natural gas demands, the domestic main oil and gas field enters the later development stage, and oil and gas resources can be replaced and mainly concentrated in deep stratum. The deep ultra-deep oil gas resource in China has great potential, and the deep oil gas resource, especially the high-efficiency development of the deep oil gas resource at 8000m, has great significance for improving the energy guarantee level in China.
In the exploration and development process of oil and gas resources of deep wells and ultra-deep wells, complex stratum such as high temperature, salt paste layers and high-pressure salt water layers are frequently encountered in the drilling process, under the high-temperature high-pressure high-salt environment of the deep well drilling stratum, chemical treatment agents in the well drilling fluid can have high-temperature degradation, high-temperature crosslinking, high-temperature desorption, high-temperature de-hydration and other high-temperature damage effects, polymer molecular chains curl under the high-temperature condition, the de-hydration effect is obviously enhanced, the performance of the drilling fluid is worsened or even deteriorated, the requirements of drilling engineering cannot be met, the normal operation of the drilling operation is seriously influenced, and therefore, the requirement on the high-temperature salt pollution resistance capability of the drilling fluid is higher. The filtrate reducer is used as one of the important treatment agents of the water-based drilling fluid, can effectively reduce the filtrate loss of the working fluid entering the well under specific engineering conditions, and plays an important role in ensuring safe, rapid and efficient drilling.
The filtrate reducer for drilling fluid mainly comprises natural modified high molecular compounds, synthetic resins, synthetic polymers and the like. The natural polymer and the derivative have limited temperature resistance and salt resistance, the application range of the common temperature is lower than 150 ℃, and the current synthetic polymer fluid loss additive breaks through in the aspects of high temperature resistance and salt resistance. The prior art reports on improving the temperature resistance and salt resistance of the filtrate reducer, for example, CN 103602322A discloses a high temperature resistant nanocomposite filtrate reducer for drilling fluid and a preparation method thereof, and the filtrate reducer is prepared from styrene, amide, acrylic acid, azodiisobutyronitrile, alkenyl sulfonic acid and nano SiO 2 As a raw material, the invention provides a high temperature resistant nanocomposite filtrate reducer with a temperature resistance of 220 ℃. However, the salt resistance and the calcium resistance are detected at 150 ℃, and the defects of complex preparation method, large addition amount and the like exist. CN 114773539a discloses a high temperature resistant high salt resistant micro-crosslinking hydrophobic association tackifying filtrate reducer for water-based drilling fluid and a preparation method thereof, the filtrate reducer disclosed in the patent is prepared by copolymerizing a comonomer, a crosslinking agent, a cosolvent and an initiator in water: the comonomer comprises vinyl monomer, sodium styrene sulfonate, maleic anhydride and long hydrophobic chain ester monomer. The micro-crosslinked hydrophobically associating viscosity increasing filtrate reducer has a temperature resistance up to 200 ℃ and a NaCl resistance of 30%, but the ability to resist divalent salts is not disclosed. CN 112094628A discloses a high temperature resistant and salt-resistant calcium water-based drilling fluid filtrate reducer, and preparation method and application thereof, the filtrate reducer disclosed in the patent comprises a solvent and a copolymer, the copolymer comprises a first structural unit, a second structural unit, a third structural unit and a fourth junctionThe building block, the first building block is vinyl ester hydrophobic monomer, the second building block is anhydride monomer, the third building block is acrylic acid monomer, the fourth building block is N-vinyl pyrrolidone monomer. The high-temperature-resistant salt-resistant calcium water-based drilling fluid filtrate reducer has saturated salt resistance and a certain calcium resistance, but the temperature resistance of the filtrate reducer is only up to 180 ℃, and the temperature resistance is insufficient.
In view of the above, aiming at the technical requirements of complex stratum drilling fluid such as deep ultra-deep layers and salt-paste layers, a novel high-temperature-resistant and composite-salt-resistant filtrate reducer needs to be developed.
Disclosure of Invention
Aiming at the problems that a polymer is easy to generate high-temperature degradation, high-temperature crosslinking, high-temperature desorption, high-temperature de-hydration and other high-temperature damage effects at high temperature of a water-based drilling fluid filtrate reducer in the prior art, and the molecular structure is curled and the filtrate loss performance is easy to run away under a high-salt condition, the invention aims to provide a high-temperature-resistant and compound-salt-resistant polymer filtrate reducer, and a preparation method and application thereof. The high temperature resistant and composite salt resistant polymer filtrate reducer has nonionic groups and zwitterionic groups, and the preparation method thereof overcomes the problems of insufficient high temperature resistant and composite salt resistant capability and complex preparation process in the prior art.
To achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the invention provides a high temperature resistant and complex salt resistant polymer filtrate reducer, which is prepared by copolymerizing a comonomer, a cosolvent, sodium chloroacetate and an initiator in water;
the comonomer comprises acrylamide, 2-acrylamido-2-methylpropanesulfonic acid, allyl polyoxyethylene ether and vinyl N heterocyclic monomer.
The filtrate reducer provided by the invention introduces an anionic strong hydration group (carboxyl and sulfonic group), so that the hydration capacity of the polymer is enhanced, and the excellent gel protecting capacity is provided for the filtrate reducer under the conditions of high temperature and high salt; nonionic groups (polyoxyethylene groups) are introduced, so that the polymer has strong tolerance to different salts, long-chain polyoxyethylene groups form comb-shaped structures in space, and the space extensibility of the polymer molecular structure under high salt concentration is maintained; the zwitterionic groups are introduced, so that an inner salt structure is formed in the molecule, the external salt ions are insensitive, and the salt resistance is further improved; the filtrate reducer provided by the invention has excellent filtrate reducing capability after high-temperature compound salt aging, and has wide application prospect in the field of high-temperature-resistant high-salt water-based drilling fluid.
In addition, sodium chloroacetate is selected as a quaternization reaction raw material, and compared with the quaternization reaction raw material containing sulfonic acid groups such as 1, 3-propane sultone, the invention has higher reaction activity.
The synthetic route of the high temperature resistant and composite salt resistant polymer filtrate reducer is shown as follows:
as a preferable technical scheme of the invention, the mass ratio of the acrylamide, the 2-acrylamide-2-methylpropanesulfonic acid, the allyl polyoxyethylene ether and the vinyl N heterocyclic monomer is (35-50): (15-30): (10-15): (5-10), for example, may be 35:15:10:5, 35:23:12.5:7.5, 35:30:15:10, 40:22.5:13:6, 40:25:12:10, 50:21:11:7, or 50:30:15:10, but are not limited to the recited values, as are other non-recited values within the range of values.
The filtrate reducer can realize the high temperature resistance and salt resistance effect of the filtrate reducer by the mutual synergistic effect of acrylamide, 2-acrylamide-2-methylpropanesulfonic acid, allyl polyoxyethylene ether and vinyl N heterocyclic monomer, wherein the excessive content of 2-acrylamide-2-methylpropanesulfonic acid can cause the reduction of molecular weight and the deterioration of filtration failure effect; if the content is too low, a dense hydration film cannot be formed on the clay surface due to the reduction of the proportion of the strong hydration groups, so that the filtration reducing effect and the temperature resisting capability are weakened; the excessive acrylamide content can cause excessive molecular weight and excessive viscosity of the treating agent, so that molecular chains are easy to break at high temperature, and the temperature resistance is reduced; when the content is too low, the molecular weight is too low, and the filtration failure effect is poor; the excessive amount of the allyl polyoxyethylene ether can cause the decrease of the molecular weight of the polymer due to the excessive steric hindrance of the monomer, and the deterioration of the filtration failure effect; if the content is too low, a sufficient amount of long side chain nonionic chains cannot be formed, a compact comb-shaped structure cannot be formed in space, and the salt resistance is obviously reduced; the excessive content of the vinyl N heterocyclic monomer can lead to the reduction of molecular weight due to the large steric hindrance of the cyclic structure monomer and low reactivity ratio, and the deterioration of the filtration failure effect; when the content is too low, on one hand, the N heterocycle has strong adsorptivity, the content is too low, so that the binding force with clay is weakened, the capability of inhibiting the clay from being high Wen Xuning is weakened, and on the other hand, the formed zwitterion has small content, and the temperature resistance and salt resistance are weakened.
As a preferred embodiment of the present invention, the vinyl N-heterocyclic monomer comprises N-vinylimidazole and/or N-vinylpyridine.
The molecular weight of the allyl polyoxyethylene ether is preferably 300 to 2400, and may be 300, 500, 700, 900, 1300, 1700, 2000 or 2400, for example, but is not limited to the values recited, and other values not recited in the numerical range are equally applicable.
As a preferred embodiment of the present invention, the initiator comprises potassium persulfate and sodium bisulfite.
Preferably, the mass ratio of the potassium persulfate to the sodium bisulfite is (1.8-2.5): 1, for example, 1.8:1, 1.9:1, 2.0:1, 2.2:1, 2.4:1 or 2.5:1, but not limited to the recited values, and other non-recited values within the range of values are equally applicable.
Preferably, the initiator is used in an amount of 0.2 to 0.5wt% based on the total weight of the comonomer, which may be, for example, 0.2wt%, 0.3wt%, 0.4wt% or 0.5wt%, but is not limited to the values recited, other values not recited in the range of values being equally applicable.
The initiator is used as an important component for initiating the copolymerization reaction, the content of the initiator is too high, so that the molecular weight is low, the explosion polymerization is easy to occur, and the filtration failure effect is poor; when the content is too low, the generation rate of free radicals is slow, the reaction time is increased, and meanwhile, the molecular weight is too large, the viscosity is too high, so that the temperature resistance is reduced.
In a preferred embodiment of the present invention, the molar ratio of the sodium chloroacetate to the vinyl N-heterocyclic monomer is (1.2 to 1.5): 1, and for example, 1.2:1, 1.3:1, 1.4:1 or 1.5:1 may be used, but the present invention is not limited to the recited values, and other values not recited in the numerical range are equally applicable.
The sodium chloroacetate in the invention is used as a quaternization reaction raw material, has higher reactivity, and is beneficial to promoting the quaternization reaction.
As a preferred embodiment of the present invention, the cosolvent includes tetrahydrofuran and/or isopropanol.
Preferably, the tetrahydrofuran is used in an amount of 30 to 50wt% based on the total mass of the comonomer, for example 30wt%, 34wt%, 38wt%, 42wt%, 46wt% or 50wt%, but not limited to the values recited, other values not recited in the numerical range being equally applicable.
In a second aspect, the invention provides a method for preparing the high temperature resistant and composite salt resistant polymer filtrate reducer according to the first aspect, wherein the preparation method comprises the following steps:
(1) Mixing water and 2-acrylamide-2-methylpropanesulfonic acid, and mixing acrylamide, allyl polyoxyethylene ether and vinyl N heterocyclic monomer according to the formula amount after acid-base adjustment to obtain comonomer mixed solution;
(2) Introducing nitrogen into the comonomer mixed solution obtained in the step (1) and heating for one time, and then mixing an initiator according to the formula amount to carry out copolymerization reaction to obtain a copolymerization reaction solution;
(3) Mixing cosolvent, sodium chloroacetate and the copolymerization reaction liquid obtained in the step (2) according to the formula amount, carrying out quaternization reaction, and then sequentially carrying out reduced pressure distillation, washing, drying and crushing to obtain the high temperature resistant and composite salt resistant polymer filtrate reducer.
Compared with the preparation of a general zwitterionic polymer, the preparation of the zwitterionic polymer is carried out by synthesizing the zwitterionic monomer and then carrying out the polymer reaction, and the amphoteric ion in the filtrate reducer provided by the invention is prepared by quaternizing the vinyl N heterocyclic monomer and sodium chloroacetate, and can be carried out by adopting one-pot reaction, so that the preparation process of the zwitterionic polymer is simplified.
As a preferable technical scheme of the invention, the end point of the acid-base regulation in the step (1) is that the pH value is neutral.
Preferably, the reagent used in the acid-base adjustment in step (1) comprises an alkaline solution.
Preferably, the alkaline solution comprises sodium hydroxide.
In a preferred embodiment of the present invention, the nitrogen gas in the step (2) is introduced for 30 to 60 minutes, for example, 30 minutes, 35 minutes, 40 minutes, 45 minutes, 50 minutes, 55 minutes or 60 minutes, but the present invention is not limited to the recited values, and other values not recited in the numerical range are equally applicable.
The end point of the first temperature increase in the step (2) is preferably 40 to 60 ℃, and may be, for example, 40 ℃, 42 ℃, 44 ℃, 46 ℃, 48 ℃, 50 ℃, 52 ℃, 54 ℃, 56 ℃, 58 ℃ or 60 ℃, but not limited to the values listed, and other values not listed in the numerical range are equally applicable.
Preferably, the copolymerization reaction in step (2) is carried out for 3 to 5 hours, for example, 3 hours, 3.2 hours, 3.4 hours, 3.6 hours, 3.8 hours, 4 hours, 4.2 hours, 4.4 hours, 4.6 hours, 4.8 hours or 5 hours, but not limited to the recited values, and other values not recited in the numerical range are equally applicable.
The temperature of the copolymerization reaction in the step (2) is preferably 40 to 60 ℃, and may be, for example, 40 ℃, 42 ℃, 44 ℃, 46 ℃, 48 ℃, 50 ℃, 52 ℃, 54 ℃, 56 ℃, 58 ℃ or 60 ℃, but is not limited to the values listed, and other values not listed in the numerical range are equally applicable.
In a preferred embodiment of the present invention, the quaternization reaction in step (3) takes 8 to 14 hours, for example, 8 hours, 8.5 hours, 9 hours, 9.5 hours, 10 hours, 10.5 hours, 11 hours, 11.5 hours, 12 hours, 12.5 hours, 13 hours, 13.5 hours or 14 hours, but the present invention is not limited to the recited values, and other values not recited in the numerical range are equally applicable.
The quaternization reaction in step (3) is preferably carried out at a temperature of 40 to 60 ℃, for example, 40 ℃, 42 ℃, 44 ℃, 46 ℃, 48 ℃, 50 ℃, 52 ℃, 54 ℃, 56 ℃, 58 ℃ or 60 ℃, but the present invention is not limited to the values listed, and other values not listed in the numerical range are equally applicable.
It is worth to say that the reaction temperature in the preparation process of the invention is 40-60 ℃, if the temperature is too high, the generation rate of free radicals is too high, and the molecular weight is reduced; when the temperature is too low, the reaction time becomes long and the molecular weight becomes large.
Preferably, the purpose of the reduced pressure distillation of step (3) is: the cosolvent and water in the reaction system are removed.
Preferably, the washing of step (3) comprises: the product was washed at least twice in ethanol solution.
Preferably, the drying of step (3) comprises: drying the mixture for 12 to 36 hours at the temperature of between 60 and 80 ℃ by adopting a blast drying box.
The drying temperature is, for example, 60 to 80 ℃, and may be, for example, 60 ℃, 65 ℃, 70 ℃, 75 ℃ or 80 ℃, but is not limited to the recited values, and other values not recited in the range of values are equally applicable; the drying time is 12 to 36 hours, and may be, for example, 12 hours, 14 hours, 16 hours, 18 hours, 20 hours, 24 hours, 28 hours, 32 hours or 36 hours, but is not limited to the recited values, and other values not recited in the numerical range are equally applicable.
As a preferred technical scheme of the invention, the preparation method of the high-temperature-resistant and composite-salt-resistant polymer filtrate reducer provided by the second aspect of the invention comprises the following steps:
(1) Mixing water and 2-acrylamide-2-methylpropanesulfonic acid, adjusting to neutrality by adopting sodium hydroxide acid-base, and mixing acrylamide, allyl polyoxyethylene ether and vinyl N heterocyclic monomer according to the formula amount to obtain comonomer mixed solution;
wherein the mass ratio of the acrylamide to the 2-acrylamido-2-methylpropanesulfonic acid to the allyl polyoxyethylene ether to the vinyl N heterocyclic monomer is (35-50): (15-30): (10-15): (5-10);
(2) Introducing nitrogen into the comonomer mixed solution obtained in the step (1) for 30-60 min, heating to 40-60 ℃ once, and then mixing an initiator according to the formula amount to perform copolymerization reaction for 3-5 h at 40-60 ℃ to obtain a copolymerization reaction solution;
wherein the initiator comprises potassium persulfate and sodium bisulphite with the mass ratio of (1.8-2.5) to 1, and the dosage of the initiator is 0.2-0.5 wt% of the total weight of the comonomer;
(3) Mixing cosolvent, sodium chloroacetate according to the formula amount, carrying out quaternization reaction for 8-14 h at 40-60 ℃ on the copolymerization reaction liquid obtained in the step (2), and then sequentially carrying out reduced pressure distillation to remove the cosolvent and water, washing, drying and crushing to obtain the high temperature resistant and composite salt resistant polymer filtrate reducer;
wherein the molar ratio of the sodium chloroacetate to the vinyl N heterocyclic monomer is (0.8 to 1.2): 1.
The numerical ranges recited herein include not only the above-listed point values, but also any point values between the above-listed numerical ranges that are not listed, and are limited in space and for the sake of brevity, the present invention is not intended to be exhaustive of the specific point values that the stated ranges include.
Compared with the prior art, the invention has the beneficial effects that:
(1) The preparation method of the high-temperature-resistant and composite salt-resistant polymer filtrate reducer provided by the invention is simple and easy to operate, has good temperature resistance, salt resistance and calcium resistance, the temperature resistance can reach 200 ℃, and the NaCl resistance can reach 15% and CaCl resistance 2 Up to 1%;
(2) The high-temperature-resistant and high-salt-resistant polymer fluid loss additive provided by the invention has excellent fluid loss reducing capacity after being aged by high-temperature composite salt, and has wide application prospects in the field of high-temperature-resistant and high-salt-water-based drilling fluid.
Detailed Description
The technical scheme of the invention is further described by the following specific embodiments. It will be apparent to those skilled in the art that the examples are merely to aid in understanding the invention and are not to be construed as a specific limitation thereof.
The experimental methods described in the following examples and comparative examples are conventional methods unless otherwise specified; the reagents, materials, and apparatus, unless otherwise specified, are all commercially available.
Example 1
The embodiment provides a high temperature resistant and composite salt resistant polymer filtrate reducer, and the preparation method of the high temperature resistant and composite salt resistant polymer filtrate reducer comprises the following steps:
(1) Mixing 150mL of water and 15g of 2-acrylamido-2-methylpropanesulfonic acid, adjusting the pH to be neutral by adopting sodium hydroxide, and then mixing 25g of acrylamide, 7.5g of allyl polyoxyethylene ether (with the molecular weight of 500) and 5g N-vinylimidazole to obtain a comonomer mixed solution;
(2) Introducing nitrogen into the comonomer mixed solution obtained in the step (1) for 30min, heating to 50 ℃ once, and then mixing 0.07g of potassium persulfate and 0.035g of sodium bisulfite for 5h copolymerization reaction at 50 ℃ to obtain a copolymerization reaction solution;
(3) Mixing 50mL of tetrahydrofuran solution, 6.18g of sodium chloroacetate and the copolymerization reaction liquid obtained in the step (2) to carry out quaternization reaction at 60 ℃ for 12 hours, then sequentially carrying out reduced pressure distillation to remove cosolvent and water, then washing in ethanol solution for three times, drying in a blowing drying oven at 80 ℃ for 24 hours, and crushing to obtain the high temperature resistant and composite salt resistant polymer filtrate reducer.
Example 2
The embodiment provides a high temperature resistant and composite salt resistant polymer filtrate reducer, and the preparation method of the high temperature resistant and composite salt resistant polymer filtrate reducer comprises the following steps:
(1) Mixing 150mL of water and 22.5g of 2-acrylamide-2-methylpropanesulfonic acid, adjusting the mixture to be neutral by adopting sodium hydroxide acid-base, and then mixing 42.5g of acrylamide, 12.5g of allyl polyoxyethylene ether (with the molecular weight of 1000) and 7.5g N-vinylimidazole to obtain a comonomer mixed solution;
(2) Introducing nitrogen into the comonomer mixed solution obtained in the step (1) for 40min, heating to 40 ℃ once, and then mixing 0.14g of potassium persulfate and 0.07g of sodium bisulfite initiator to carry out copolymerization reaction for 5h at 40 ℃ to obtain a copolymerization reaction solution;
(3) Mixing 50mL of tetrahydrofuran solution, 12.36g of sodium chloroacetate and the copolymerization reaction liquid obtained in the step (2) to carry out quaternization reaction at 40 ℃ for 14 hours, and then sequentially carrying out reduced pressure distillation to remove cosolvent and water, washing, drying and crushing to obtain the high temperature resistant and composite salt resistant polymer filtrate reducer.
Example 3
The embodiment provides a high temperature resistant and composite salt resistant polymer filtrate reducer, and the preparation method of the high temperature resistant and composite salt resistant polymer filtrate reducer comprises the following steps:
(1) Mixing 150mL of water and 20g of 2-acrylamide-2-methylpropanesulfonic acid, adjusting the mixture to be neutral by adopting sodium hydroxide acid-base, and then mixing 35g of acrylamide, 10g of allyl polyoxyethylene ether and 5g N-vinylimidazole to obtain a comonomer mixed solution;
(2) Introducing nitrogen into the comonomer mixed solution obtained in the step (1) for 60min, heating to 60 ℃ once, and then mixing 0.093g of potassium persulfate and 0.047g of sodium bisulfite for 3h copolymerization reaction at 60 ℃ to obtain a copolymerization reaction solution;
(3) Mixing 50mL of tetrahydrofuran solution, 6.18g of sodium chloroacetate and the copolymerization reaction liquid obtained in the step (2) to carry out quaternization reaction at 50 ℃ for 8 hours, and then sequentially carrying out reduced pressure distillation to remove cosolvent and water, washing, drying and crushing to obtain the high temperature resistant and composite salt resistant polymer filtrate reducer.
Example 4
The embodiment provides a high temperature resistant and composite salt resistant polymer filtrate reducer, and the preparation method of the high temperature resistant and composite salt resistant polymer filtrate reducer is different from that of embodiment 1 only in that:
in this example, the 5g N-vinylimidazole in step (1) was modified to 5g N-vinylpyridine, and the temperature of the quaternization reaction in step (3) was modified to 50℃for 14 hours.
Example 5
The embodiment provides a high temperature resistant and composite salt resistant polymer filtrate reducer, and the preparation method of the high temperature resistant and composite salt resistant polymer filtrate reducer is different from that of embodiment 1 only in that:
in this example, the molecular weight of the allyl polyoxyethylene ether in the step (1) is modified to 1000.
Example 6
The embodiment provides a high temperature resistant and composite salt resistant polymer filtrate reducer, and the preparation method of the high temperature resistant and composite salt resistant polymer filtrate reducer is different from that of embodiment 1 only in that:
in this example, the molecular weight of the allyl polyoxyethylene ether in step (1) was modified to 2400.
Comparative example 1
The comparative example provides a fluid loss additive, and the preparation method of the fluid loss additive comprises the following steps:
(1) Mixing 150mL of water and 15g of 2-acrylamido-2-methylpropanesulfonic acid, adjusting the pH to be neutral by using 2.89g of sodium hydroxide, and then mixing 25g of acrylamide and 7.5g of allyl polyoxyethylene ether (with the molecular weight of 500) to obtain a comonomer mixed solution;
(2) Introducing nitrogen into the comonomer mixed solution obtained in the step (1) for 30min, heating to 50 ℃ once, and then mixing 0.07g of potassium persulfate and 0.035g of sodium bisulfite for 5h copolymerization reaction at 50 ℃ to obtain a product;
(3) Washing the product obtained in the step (2) in ethanol solution for three times, drying the purified product in a blowing drying oven at 80 ℃ for 24 hours, and crushing to obtain the filtrate reducer.
Comparative example 2
This comparative example provides a fluid loss additive whose preparation method differs from example 1 only in that:
the comparative example was carried out by modifying the added amount of the allyl polyoxyethylene ether in the step (1) to 0g.
Comparative example 3
This comparative example provides a fluid loss additive whose preparation method differs from example 1 only in that:
this comparative example modifies the initiator described in step (2) to 0.21g of potassium persulfate and 0.105 g of sodium bisulfite.
Comparative example 4
This comparative example provides a fluid loss additive whose preparation method differs from example 1 only in that:
this comparative example modifies the initiator described in step (2) to 0.035g of potassium persulfate and 0.0175 g of sodium bisulfite.
And (3) performance detection:
the fluid loss additives provided in the above examples and comparative examples were evaluated for performance in a composite brine drilling fluid and at different temperatures, and the results are shown in tables 1 and 2, respectively.
Wherein, table 1 shows the performance evaluation of the fluid loss additives provided in the above examples and comparative examples in a composite brine drilling fluid; table 2 shows the performance of the fluid loss additive provided in example 1 at different temperatures;
the properties include: the Apparent Viscosity (AV), the Plastic Viscosity (PV), the dynamic shear force (YP) and the high-temperature high-pressure Fluid Loss (FL) of the drilling fluid prepared by referring to national standard GB/T29170-2012 drilling fluid laboratory test of petroleum and natural gas industry HTHP )。
Further, the performance evaluation of the filtrate reducer in the composite brine drilling fluid and the performance evaluation at different temperatures provided in the above examples and comparative examples specifically include the following steps:
(a) Preparation of 4% bentonite-based slurry: adding 16g of bentonite and 0.56g of anhydrous sodium carbonate into 400mL of water, stirring for 20min at a rotating speed of 8000r/min, sealing, standing and hydrating for 24h at room temperature;
(b) Sample configuration of composite brine drilling fluid: 400mL of 4% bentonite slurry is taken, 12g (3%) of the filtrate reducer prepared in the examples and the comparative examples are respectively added, and the mixture is stirred for 20min at 8000 r/min; subsequently, 60g (15%) of sodium chloride and 4g (1%) of calcium chloride were added and stirred at 8000r/min for 20min;
(c) Aging treatment of drilling fluid samples: and placing the drilling fluid sample into a roller heating furnace, wherein the aging temperature is 180 ℃, 200 ℃, 220 ℃ and the aging time is 16 hours.
TABLE 1
TABLE 2
From Table 1, the following points can be seen:
(1) Analysis examples 1-6 show that when the addition amount of the filtrate reducer provided by the invention is 3wt.% and the composite salt in 4wt.% bentonite slurry, and after the filtrate reducer is cured for 16 hours at 200 ℃, good high-temperature rheological property and filtrate reducing effect are maintained;
(2) Analysis example 1 and comparative example 1 show that the polymer filtrate reducer prepared in comparative example 1 does not introduce a zwitterionic structure in the preparation process, and polymer hydration groups (sulfonic acid groups, oxyethylene groups and the like) are sensitive to salt concentration under the conditions of high temperature and high composite salt, so that the polymer double electric layers are obviously compressed, and the salt resistance of the filtrate reducer is reduced;
(3) Analysis of example 1 and comparative example 2 shows that comparative example 2 does not add allyl polyoxyethylene ether, so that the copolymer cannot form a long side chain comb structure, and the molecular chain is easy to curl under high-concentration salt, so that the temperature resistance of the product is obviously reduced;
(4) Analysis example 1 and comparative examples 3 to 4 show that when the addition amount of the initiator is small, the initiation efficiency is low, the molecular weight of the synthesized product is too large, the filtration reduction effect is poor, and the monomer utilization rate is low; when the addition amount of the initiator is too large, the polymerization degree of the copolymer is smaller, the average molecular weight is too low, and the filtration failure effect is poor.
From the test results of Table 2, it can be seen that the polymer viscosity and the high temperature and high pressure fluid loss increase with increasing temperature. At the temperature below 200 ℃, the polymer keeps good high-temperature rheological property and filtration reducing effect. The temperature is higher than 220 ℃, and the filtration loss is obviously increased.
In conclusion, the high-temperature-resistant and composite salt-resistant polymer filtrate reducer provided by the invention has the temperature resistance up to 200 ℃, 15% NaCl and 1% CaCl 2 . By introducing the zwitterionic groups and the long-chain nonionic groups into the molecular structure, the composite salt resistance of the polymer is enhanced, and the drilling requirements of high-temperature high-salt complex stratum can be met.
While the foregoing is directed to embodiments of the present invention, other and further details of the invention may be had by the present invention, it should be understood that the foregoing description is merely illustrative of the present invention and that no limitations are intended to the scope of the invention, except insofar as modifications, equivalents, improvements or modifications are within the spirit and principles of the invention.
Claims (10)
1. The high temperature resistant and composite salt resistant polymer filtrate reducer is characterized in that the filtrate reducer is prepared by copolymerizing a comonomer, a cosolvent, sodium chloroacetate and an initiator in water;
the comonomer comprises acrylamide, 2-acrylamido-2-methylpropanesulfonic acid, allyl polyoxyethylene ether and vinyl N heterocyclic monomer.
2. The high temperature resistant and composite salt resistant polymer fluid loss additive according to claim 1, wherein the mass ratio of the acrylamide, the 2-acrylamido-2-methylpropanesulfonic acid, the allyl polyoxyethylene ether and the vinyl N heterocyclic monomer is (35-50): (15-30): (10-15): (5-10).
3. The high temperature and complex salt resistant polymeric fluid loss additive of claim 1 or 2, wherein the vinyl N-heterocyclic monomer comprises N-vinyl imidazole and/or N-vinyl pyridine;
preferably, the molecular weight of the allyl polyoxyethylene ether is 300-2400.
4. A high temperature and complex salt resistant polymeric fluid loss additive according to any of claims 1-3 wherein the initiator comprises potassium persulfate and sodium bisulfite;
preferably, the mass ratio of the potassium persulfate to the sodium bisulfite is (1.8-2.5): 1;
preferably, the initiator is used in an amount of 0.2 to 0.5wt% based on the total weight of the comonomer.
5. The high temperature and complex salt resistant polymer fluid loss additive according to any one of claims 1 to 4, wherein the molar ratio of sodium chloroacetate to vinyl N heterocyclic monomer is 1.2 to 1.5.
6. The high temperature and complex salt resistant polymeric fluid loss additive of any of claims 1-5, wherein the co-solvent comprises tetrahydrofuran and/or isopropanol;
preferably, the co-solvent is used in an amount of 30 to 50wt% based on the total mass of the comonomer.
7. A method for preparing the high temperature resistant and composite salt resistant polymer fluid loss additive according to any one of claims 1 to 6, wherein the method comprises the following steps:
(1) Mixing water and 2-acrylamide-2-methylpropanesulfonic acid, and mixing acrylamide, allyl polyoxyethylene ether and vinyl N heterocyclic monomer according to the formula amount after acid-base adjustment to obtain comonomer mixed solution;
(2) Introducing nitrogen into the comonomer mixed solution obtained in the step (1) and heating for one time, and then mixing an initiator according to the formula amount to carry out copolymerization reaction to obtain a copolymerization reaction solution;
(3) Mixing cosolvent, sodium chloroacetate and the copolymerization reaction liquid obtained in the step (2) according to the formula amount, carrying out quaternization reaction, and then sequentially carrying out reduced pressure distillation, washing, drying and crushing to obtain the high temperature resistant and composite salt resistant polymer filtrate reducer.
8. The method according to claim 7, wherein the acid-base adjustment in step (1) is terminated by neutral ph;
preferably, the reagent used in the acid-base adjustment of step (1) comprises an alkaline solution;
preferably, the alkaline solution comprises sodium hydroxide.
9. The method according to claim 7 or 8, wherein the nitrogen gas is introduced in step (2) for 30 to 60 minutes;
preferably, the end point of the primary temperature rise in the step (2) is 40-60 ℃;
preferably, the time of the copolymerization reaction in the step (2) is 3-5 h;
preferably, the temperature of the copolymerization reaction in the step (2) is 40-60 ℃.
10. The process according to any one of claims 7 to 9, wherein the quaternization reaction in step (3) takes 8 to 14 hours;
preferably, the temperature of the quaternization reaction in the step (3) is 40-60 ℃;
preferably, the purpose of the reduced pressure distillation of step (3) is: the cosolvent and water in the reaction system are removed.
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