CN108531153B - High-temperature-resistant petroleum resin dispersoid blocking agent and preparation method and application thereof - Google Patents
High-temperature-resistant petroleum resin dispersoid blocking agent and preparation method and application thereof Download PDFInfo
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- CN108531153B CN108531153B CN201810413957.7A CN201810413957A CN108531153B CN 108531153 B CN108531153 B CN 108531153B CN 201810413957 A CN201810413957 A CN 201810413957A CN 108531153 B CN108531153 B CN 108531153B
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- 239000003208 petroleum Substances 0.000 title claims abstract description 121
- 239000011347 resin Substances 0.000 title claims abstract description 121
- 229920005989 resin Polymers 0.000 title claims abstract description 121
- 238000002360 preparation method Methods 0.000 title abstract description 14
- 239000002981 blocking agent Substances 0.000 title abstract description 9
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 92
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 70
- 229920002401 polyacrylamide Polymers 0.000 claims abstract description 62
- 125000002091 cationic group Chemical group 0.000 claims abstract description 55
- 239000003921 oil Substances 0.000 claims abstract description 50
- 239000006185 dispersion Substances 0.000 claims abstract description 48
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000003129 oil well Substances 0.000 claims abstract description 32
- 239000002994 raw material Substances 0.000 claims abstract description 27
- 239000004094 surface-active agent Substances 0.000 claims abstract description 19
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims abstract description 18
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000002105 nanoparticle Substances 0.000 claims abstract description 18
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims abstract description 18
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 17
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 16
- 150000003839 salts Chemical class 0.000 claims abstract description 15
- 238000006011 modification reaction Methods 0.000 claims abstract description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 33
- 238000000034 method Methods 0.000 claims description 13
- 230000033558 biomineral tissue development Effects 0.000 claims description 11
- NAPSCFZYZVSQHF-UHFFFAOYSA-N dimantine Chemical group CCCCCCCCCCCCCCCCCCN(C)C NAPSCFZYZVSQHF-UHFFFAOYSA-N 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 9
- 239000008398 formation water Substances 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- 239000000725 suspension Substances 0.000 claims description 4
- 230000000903 blocking effect Effects 0.000 claims description 3
- 230000008014 freezing Effects 0.000 claims description 3
- 238000007710 freezing Methods 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 150000001768 cations Chemical class 0.000 claims description 2
- 239000010410 layer Substances 0.000 description 16
- 238000003756 stirring Methods 0.000 description 13
- 235000011121 sodium hydroxide Nutrition 0.000 description 10
- 238000004581 coalescence Methods 0.000 description 8
- 239000000499 gel Substances 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 230000009471 action Effects 0.000 description 5
- 230000007547 defect Effects 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 235000015110 jellies Nutrition 0.000 description 4
- 239000008274 jelly Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- 238000011084 recovery Methods 0.000 description 4
- 125000000129 anionic group Chemical group 0.000 description 3
- 230000006378 damage Effects 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 239000011229 interlayer Substances 0.000 description 3
- 230000007774 longterm Effects 0.000 description 3
- 230000035699 permeability Effects 0.000 description 3
- 239000004576 sand Substances 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 235000020681 well water Nutrition 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000003708 ampul Substances 0.000 description 2
- 238000007664 blowing Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000003673 groundwater Substances 0.000 description 2
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 125000004029 hydroxymethyl group Chemical group [H]OC([H])([H])* 0.000 description 2
- 239000011146 organic particle Substances 0.000 description 2
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000008399 tap water Substances 0.000 description 2
- 235000020679 tap water Nutrition 0.000 description 2
- 239000008096 xylene Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000006004 Quartz sand Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 125000003368 amide group Chemical group 0.000 description 1
- 239000002280 amphoteric surfactant Substances 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 229920006317 cationic polymer Polymers 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000000599 controlled substance Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000010881 fly ash Substances 0.000 description 1
- 230000002431 foraging effect Effects 0.000 description 1
- 239000000295 fuel oil Substances 0.000 description 1
- 235000010299 hexamethylene tetramine Nutrition 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000010954 inorganic particle Substances 0.000 description 1
- 229910003480 inorganic solid Inorganic materials 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000005543 nano-size silicon particle Substances 0.000 description 1
- 239000003002 pH adjusting agent Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000002028 premature Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 125000000542 sulfonic acid group Chemical group 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/50—Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls
- C09K8/504—Compositions based on water or polar solvents
- C09K8/506—Compositions based on water or polar solvents containing organic compounds
- C09K8/508—Compositions based on water or polar solvents containing organic compounds macromolecular compounds
- C09K8/514—Compositions based on water or polar solvents containing organic compounds macromolecular compounds of natural origin, e.g. polysaccharides, cellulose
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/50—Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls
- C09K8/504—Compositions based on water or polar solvents
- C09K8/506—Compositions based on water or polar solvents containing organic compounds
- C09K8/508—Compositions based on water or polar solvents containing organic compounds macromolecular compounds
- C09K8/5086—Compositions based on water or polar solvents containing organic compounds macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- E—FIXED CONSTRUCTIONS
- E21—EARTH OR ROCK DRILLING; MINING
- E21B—EARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
- E21B33/00—Sealing or packing boreholes or wells
- E21B33/10—Sealing or packing boreholes or wells in the borehole
- E21B33/13—Methods or devices for cementing, for plugging holes, crevices or the like
-
- E—FIXED CONSTRUCTIONS
- E21—EARTH OR ROCK DRILLING; MINING
- E21B—EARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
- E21B43/00—Methods or apparatus for obtaining oil, gas, water, soluble or meltable materials or a slurry of minerals from wells
- E21B43/16—Enhanced recovery methods for obtaining hydrocarbons
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- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
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- Fluid Mechanics (AREA)
- Geochemistry & Mineralogy (AREA)
- Environmental & Geological Engineering (AREA)
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Abstract
The invention provides a high-temperature resistant petroleum resin dispersoid blocking agent, a preparation method and application thereof, which are prepared from the following raw materials in percentage by weight: 5 to 15 percent of petroleum resin, 0.1 to 0.5 percent of surfactant, 0.05 to 0.4 percent of cationic polyacrylamide, 0.1 to 0.4 percent of triethanolamine, 0.1 to 0.5 percent of sodium bisulfite, 1 to 3 percent of silicon dioxide nano particles, 0.1 to 0.5 percent of pH regulator and the balance of water; the sum of the mass percentages of the raw materials is 100 percent. After the plugging agent is injected into a stratum, cationic polyacrylamide in the plugging agent can perform modification reaction at high temperature of the stratum to obtain sulfonic group modified cationic polyacrylamide, so that the high temperature resistance, salt resistance and stability of the petroleum resin dispersion plugging agent can be effectively improved, and the petroleum resin can smoothly reach the deep part of an oil reservoir and an oil well to realize high-temperature effective water plugging.
Description
Technical Field
The invention relates to a high-temperature-resistant petroleum resin dispersion plugging agent, and a preparation method and application thereof, and belongs to the technical field of oilfield chemistry.
Background
The oil well water outlet is an important phenomenon in the oil extraction process of an oil field, and the reason of the oil well water outlet is as follows: (1) injecting water and edge water for propulsion; (2) propelling bottom water; (3) the upper layer water and the lower layer water are mixed; (4) the interlayer water enters, and the interlayer water refers to interlayer water between oil layers, namely a water layer between an upper oil layer and a lower oil layer. The hazards caused by the water produced by the oil well are many, such as: (1) sand production of the oil well causes damage to a cemented and loosened sandstone layer, sand production is caused, and an oil layer collapses or the oil well stops production in severe cases; (2) the oil well stops spraying, the water content is continuously increased after water breakthrough, and the weight of a shaft liquid column is increased, so that the self-blowing well cannot perform self-blowing; (3) dead oil zones are formed, and the oil wells are exposed to water too early, so that some dead oil zones are formed underground, and the recovery ratio of the oil reservoir is greatly reduced; (4) equipment corrosion can corrode oil well equipment and destroy well body structures, increase the task and difficulty of workover operation and shorten the service life of an oil well; (5) the oil extraction cost is increased, the ground water injection quantity is increased, and the ground water source usage amount, the water injection facility usage and the electric energy consumption are correspondingly increased.
The profile control water shutoff is used as a conventional measure for controlling water in an oil field, and can play a role in improving the pressure of an oil layer and the sweep coefficient of injected water, thereby improving the recovery ratio of crude oil. However, with the development of oil fields, the characteristics and environment of oil reservoirs are constantly changed, particularly after the oil reservoirs enter a high-water-content exploitation period, the contradiction of long-term water driving oil reservoir development is more prominent, and the existing profile control and water shutoff technology, particularly the technology capable of being effectively applied, always lags behind the requirements of oil field development. For certain high-temperature deep-well oil reservoirs in China, the oil reservoir temperature is as high as 130 ℃, and for the oil reservoirs, polyacrylamide high-temperature gel plugging agents and solid particle type plugging agents are commonly used in the prior art. The polyacrylamide high-temperature gel plugging agent has the defects of over-quick gelling time, easy blockage of a near-wellbore area, poor gel stability at high temperature, easy damage caused when a water-based gel system enters an oil layer in the operation process and the like. The solid particle type plugging agent is mainly composed of inorganic solid particles such as cement, fly ash and the like and other organic particles, is injected into a stratum in a suspension form, and is used for adjusting a water absorption section and water phase permeability through bridging of the organic particles and filling of the inorganic particles so as to plug a high-permeability layer and a water outlet layer and achieve the purposes of adjusting the water absorption section and plugging water. In addition, chinese patent document CN101423753A also discloses a profile control agent special for thermal recovery of heavy oil wells, aiming at high-temperature deep well oil reservoirs. The profile control agent consists of the following raw materials: anionic polyacrylamide, alkylphenol ethoxylates, petroleum resin, urotropine, xylene, caustic soda and water. The profile control agent can be used for a long time under the conditions that the temperature is 200 ℃ and the mineralization degree is more than 20000mg/L, but the profile control agent can not be applied under the condition of higher mineralization degree, the gelling time of anionic polyacrylamide is short, the overall stability of the emulsion of the profile control agent is poor, the near-wellbore area is easy to be blocked, and the defects of the polyacrylamide high-temperature gel plugging agent exist; and xylene in the used raw materials belongs to toxic substances, pollutes the environment, has great harm to human bodies after long-term contact, and belongs to controlled drugs in oil fields.
Therefore, the novel temperature-resistant salt-resistant plugging agent is developed, has strong stability at high temperature and high salinity, can smoothly reach the deep part of an oil reservoir oil well to realize water plugging, has oil-water selectivity and excellent plugging effect, and has important significance for solving the problem of oil well water outlet of a high-temperature oil reservoir.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a high-temperature resistant petroleum resin dispersoid blocking agent. After the plugging agent is injected into a stratum, cationic polyacrylamide can perform modification reaction at high temperature of the stratum, and a sulfonic group connected with carbon atoms is introduced to obtain sulfonic group modified cationic polyacrylamide. The plugging agent disclosed by the invention is excellent in temperature resistance and salt resistance, good in dispersion stability at high temperature and high salinity, and has oil-water selectivity, and can play an effective plugging role in a high-temperature oil reservoir environment at 130 ℃.
The invention also provides a preparation method and application of the high-temperature resistant petroleum resin dispersoid blocking agent. The preparation method is simple, the modified cationic polyacrylamide is generated by reaction after being injected into a stratum, a series of complex synthetic processes on the ground are avoided, and the cost and the danger (mainly personal safety) are reduced.
The technical scheme of the invention is as follows:
the high-temperature-resistant petroleum resin dispersion plugging agent is prepared from the following raw materials in percentage by mass: 5 to 15 percent of petroleum resin, 0.1 to 0.5 percent of surfactant, 0.05 to 0.4 percent of cationic polyacrylamide, 0.1 to 0.4 percent of triethanolamine, 0.1 to 0.5 percent of sodium bisulfite, 1 to 3 percent of silicon dioxide nano particles, 0.1 to 0.5 percent of pH regulator and the balance of water; the sum of the mass percentages of the raw materials is 100 percent.
According to the invention, the petroleum resin dispersion plugging agent is preferably prepared from the following raw materials in percentage by weight: 5 to 10 percent of petroleum resin, 0.1 to 0.3 percent of surfactant, 0.05 to 0.3 percent of cationic polyacrylamide, 0.1 to 0.2 percent of triethanolamine, 0.15 to 0.4 percent of sodium bisulfite, 1 to 2 percent of silicon dioxide nano particles, 0.2 to 0.4 percent of pH regulator and the balance of water; the sum of the mass percentages of the raw materials is 100 percent.
According to the invention, the petroleum resin is preferably C5 or C9 petroleum resin, the relative molecular mass is 1000-5000, and the softening point is 100-120 ℃.
Preferably according to the invention, the surfactant is an amphoteric surfactant; preferably, the surfactant is octadecyl dimethyl ammonium oxide.
Preferably, according to the invention, the cationic polyacrylamide has a weight average molecular weight of 700 × 104～800×104The cationic degree is 20-40%.
Preferably, according to the invention, the silica nanoparticles have a particle size of 10 to 14 nm.
Preferably, according to the invention, the pH adjusting agent is sodium hydroxide.
Preferably, according to the invention, the water has a degree of mineralization (20-25) × 104mg/L of formation water, wherein Na+The content is (7-8) × 104mg/L、Ca2+The content of the active component is (0.5-1.5) × 104mg/L、Mg2+The content of the active component is (0.1-0.2) ×104mg/L、HCO3 -The content of the extract is (0.01-0.02) × 104mg/L、Cl-The content is (13-14) × 104mg/L, preferably, the degree of mineralization of the water is 22.3 × 104mg/L of formation water, wherein Na+The content is 7.3 × 104mg/L、Ca2+The content is 1.1 × 104mg/L、Mg2+The content is 0.15 × 104mg/L、HCO3 -The content is 0.018 × 104mg/L、Cl-The content is 13.7 × 104mg/L。
The preparation method of the high-temperature resistant petroleum resin dispersoid blocking agent comprises the following steps:
dissolving a surfactant in water, adding petroleum resin powder, and fully dispersing to obtain a petroleum resin dispersion liquid; dissolving cationic polyacrylamide, triethanolamine, sodium bisulfite and a pH regulator in water, adding silicon dioxide nanoparticles, and fully dispersing to obtain a mixed solution; and uniformly mixing the mixed solution and the petroleum resin dispersion solution to obtain the petroleum resin dispersion plugging agent.
According to the invention, the petroleum resin powder is preferably crushed into powder with the particle size of 0.5-10 microns by adopting a freezing and crushing method, namely, taking liquid nitrogen as a cold source.
According to the present invention, it is preferable that the petroleum resin dispersion has a concentration of 25 to 30% by mass of the petroleum resin.
The high-temperature-resistant petroleum resin dispersoid plugging agent is applied to a high-temperature oil reservoir oil well for profile control and water plugging.
According to the invention, the preferable application method is that the petroleum resin dispersion plugging agent is injected into a high-temperature oil reservoir oil well, and as the temperature in the oil reservoir oil well gradually rises from top to bottom, the cationic polyacrylamide in the petroleum resin dispersion plugging agent undergoes a sulfonic acid group modification reaction with triethanolamine and sodium bisulfite to obtain sulfonic acid group modified cationic polyacrylamide, wherein the weight average molecular weight of the sulfonic acid group modified cationic polyacrylamide is 710 × 104～810×104The petroleum resin dispersion plugging agent can effectively disperse and stabilize petroleum resin suspension, and effectively improve the high temperature resistance, salt resistance and stability of the petroleum resin dispersion plugging agentTherefore, the purpose of injecting the petroleum resin dispersion plugging agent into the deep part of the oil reservoir oil well without plugging the near well zone is achieved, and the petroleum resin entering the deep part of the oil reservoir oil well begins to soften and become sticky so as to coalesce and plug the water flow channel, thereby achieving the purpose of plugging water.
The invention has the following technical characteristics and beneficial effects:
1. in order to improve the defects, the invention utilizes the characteristic that cations in a cationic polymer are easy to combine, transfer, isomerize and the like with alkaline substances under the action of high temperature, triethanolamine, sodium bisulfite and silicon dioxide nanoparticles are added into the cationic polyacrylamide, the temperature is gradually increased after a plugging agent enters a stratum, the cationic polyacrylamide firstly reacts with the triethanolamine under the conditions of high temperature and strong alkali, a hydroxymethyl group replaces one hydrogen on an amido group, and a resultant then reacts with the sodium bisulfite, so that a part of hydroxyl groups on the hydroxymethyl group are replaced by sodium sulfonate groups, the high-temperature stability of the resultant is improved under the action of the nanoparticles, the hydrolysis degree of the resultant is reduced, and the finally generated modified cationic polyacrylamide (with the average molecular weight of 700 × 10) is obtained4～800×104) The temperature resistance is greatly improved, and the stability is strong. Under the wetting action of the surfactant, the petroleum resin is dispersed in the surfactant solution, and after the modified cationic polyacrylamide is generated, the dispersion stability and the temperature and salt resistance of the petroleum resin dispersion are greatly improved, and the defects of other particle-type plugging agents are obviously improved. After the petroleum resin dispersion prepared by the invention is injected into a stratum, due to the existence of the modified cationic polyacrylamide and the combination of the surfactant auxiliary agent, the petroleum resin suspension has excellent temperature resistance and salt resistance and good dispersion stability, can smoothly reach the deep part of an oil reservoir and an oil well, and has an effective plugging effect in a high-temperature oil reservoir environment at 130 ℃.
2. The petroleum resin dispersion plugging agent has good stability under high temperature and high salinity, can be injected into the deep part of an oil reservoir and an oil well without plugging a near wellbore region, and the petroleum resin entering the deep part of the oil reservoir and the oil well begins to soften and become sticky so as to coalesce and plug a water flow channel to achieve the purpose of water plugging. The petroleum resin has higher viscosity at the formation temperature, is adhered and adsorbed on the surface of pore rock by utilizing the high viscosity characteristic of the petroleum resin after being softened and coalesced into a liquid state to seal the formation pores, and has good sealing effect and long sealing time under high temperature and high salt; the petroleum resin is insoluble in ethanol and water, can be dissolved in oil, can realize selective water plugging and oil plugging, and can effectively plug a high permeable layer. The water-based jelly has no oil-water selectivity, the polymer is gelatinized in pores under the action of a cross-linking agent, the plugging effect on a water layer is poorer than that of petroleum resin, the water layer is easy to dehydrate and lose efficacy under high temperature and high salinity, the reservoir stratum is easy to pollute, and the water-based jelly can plug an oil layer but can cause the reduction of the water drive recovery ratio.
3. The raw materials are cheap and easy to obtain, and the preparation method is simple; after the petroleum resin dispersion plugging agent is injected into a stratum, the cationic polyacrylamide in the petroleum resin dispersion plugging agent reacts under the action of high temperature of the stratum to generate modified cationic polyacrylamide, so that a series of complex synthetic processes on the ground are avoided, and the cost and the danger (mainly personal safety) are reduced.
4. The petroleum resin dispersion prepared by the invention has good stability after high-temperature reaction, the dispersion stability time can reach 22h under high temperature and high mineralization degree, and the plugging agent has higher plugging rate and high mineralization degree (22 × 10)4mg/L) and high temperature (130 ℃), the plugging rate is as high as 98.3%.
Detailed Description
The present invention is further illustrated by, but is not limited to, the following specific examples.
The raw materials used in the examples are conventional raw materials and can be obtained commercially; the methods are prior art unless otherwise specified.
In the examples, the petroleum resin used was C9 petroleum resin commercially available from Guangzhou Lianben GmbH, having an average relative molecular mass of 3500 and a softening point of 120 ℃ and cationic polyacrylamide having a weight average molecular weight of 750 × 104The cationic degree is 30 percent, and the cationic degree is sold by Anhui McSt fine chemical industry Co.Ltd; the used dioxideThe silicon nanoparticles have an average particle size of 12nm and are commercially available from Sigma-Aldrich.
The water has a degree of mineralization of 22.3 × 104mg/L of formation water, wherein Na+The content is 7.3 × 104mg/L、Ca2+The content is 1.1 × 104mg/L、Mg2+The content is 0.15 × 104mg/L、HCO3 -The content is 0.018 × 104mg/L、Cl-The content is 13.7 × 104mg/L。
Petroleum resin powder used: the petroleum resin is crushed into petroleum resin powder with the grain size of 0.5-2 microns by a freezing and crushing method, namely taking liquid nitrogen as a cold source.
Example 1
A high-temperature resistant petroleum resin dispersoid plugging agent is prepared from the following raw materials in percentage by weight: 10% of C9 petroleum resin, 0.2% of octadecyl dimethyl ammonium oxide, 0.1% of cationic polyacrylamide, 0.2% of triethanolamine, 0.2% of sodium bisulfite, 1.1% of silicon dioxide nano particles, 0.3% of sodium hydroxide and the balance of water; the sum of the mass percentages of the raw materials is 100 percent.
The preparation method of the high-temperature resistant petroleum resin dispersoid blocking agent comprises the following steps:
mineralization degree to 25g of 22.3 × 104Adding 0.2g of octadecyl dimethyl ammonium oxide into mg/L formation water, fully dissolving and stirring uniformly, slowly adding 10g of petroleum resin powder (the adding process is controlled to be 5-10 min), fully stirring and dispersing uniformly to obtain a mixed solution A, adding 13g of mixed solution A with the mineralization degree of 22.3 × 104Adding 0.2g of sodium bisulfite and 0.2g of triethanolamine into mg/L formation water, stirring uniformly to fully dissolve the formation water, adding 50g of cationic polyacrylamide aqueous solution with the mass concentration of 0.2%, adding 0.3g of sodium hydroxide and 1.1g of silicon dioxide nanoparticles, fully dispersing and stirring uniformly to obtain a mixed solution B; and fully mixing the mixed solution A and the mixed solution B to obtain the petroleum resin dispersoid plugging agent.
Simulating the conditions of the high-temperature oil reservoir oil well: stirring the petroleum resin dispersoid plugging agent obtained above at 90 ℃ for 5h to obtain the plugging agent after high-temperature treatment. In the plugging agent, cationic polyacrylamide is subjected to modification reaction to generate sulfonic acid groupModified cationic polyacrylamide having a weight average molecular weight of 750 × 104(ii) a After the plugging agent subjected to high-temperature treatment is placed at 130 ℃ for 15 hours, the petroleum resin is still stably dispersed, and no coalescence phenomenon occurs, which shows that the sulfonic group modified cationic polyacrylamide formed after the plugging agent is used can improve the stability of the petroleum resin under high temperature and high salt conditions.
Example 2
A high-temperature resistant petroleum resin dispersoid plugging agent is prepared from the following raw materials in percentage by weight: 10% of C9 petroleum resin, 0.25% of octadecyl dimethyl ammonium oxide, 0.1% of cationic polyacrylamide, 0.2% of triethanolamine, 0.2% of sodium bisulfite, 1.1% of silicon dioxide nano particles, 0.3% of sodium hydroxide and the balance of water; the sum of the mass percentages of the raw materials is 100 percent.
The preparation method of the high-temperature resistant petroleum resin dispersion plugging agent is consistent with the example 1, except that: the amount of the surfactant, octadecyl dimethyl ammonium oxide, was 0.25g, and other steps and conditions were the same as in example 1.
Simulating the conditions of a high-temperature oil reservoir and an oil well, namely stirring the obtained petroleum resin dispersoid plugging agent for 5 hours at the temperature of 90 ℃ to obtain the plugging agent after high-temperature treatment, wherein in the plugging agent, cationic polyacrylamide is subjected to modification reaction to generate sulfonic modified cationic polyacrylamide with the weight-average molecular weight of 750 × 104(ii) a After the plugging agent after high-temperature treatment is placed at 130 ℃ for 16 hours, the petroleum resin is still stably dispersed, and no coalescence phenomenon occurs, which indicates that when the dosage of the surfactant is within the range of the invention, the dosage of the surfactant is increased, and the stability of the petroleum resin under high temperature and high salt conditions can be improved.
Example 3
A high-temperature resistant petroleum resin dispersoid plugging agent is prepared from the following raw materials in percentage by weight: 10% of C9 petroleum resin, 0.3% of octadecyl dimethyl ammonium oxide, 0.1% of cationic polyacrylamide, 0.2% of triethanolamine, 0.2% of sodium bisulfite, 1.1% of silicon dioxide nano particles, 0.3% of sodium hydroxide and the balance of water; the sum of the mass percentages of the raw materials is 100 percent.
The preparation method of the high-temperature resistant petroleum resin dispersion plugging agent is consistent with the example 1, except that: the amount of the surfactant, octadecyl dimethyl ammonium oxide, was 0.3g, and other steps and conditions were the same as in example 1.
Simulating the conditions of a high-temperature oil reservoir and an oil well, namely stirring the obtained petroleum resin dispersoid plugging agent for 5 hours at the temperature of 90 ℃ to obtain the plugging agent after high-temperature treatment, wherein in the plugging agent, cationic polyacrylamide is subjected to modification reaction to generate sulfonic modified cationic polyacrylamide with the weight-average molecular weight of 750 × 104(ii) a After the plugging agent after high-temperature treatment is placed at 130 ℃ for 17 hours, the petroleum resin is still stably dispersed, and no coalescence phenomenon occurs, which indicates that when the dosage of the surfactant is within the range of the invention, the dosage of the surfactant is increased, and the stability of the petroleum resin under high temperature and high salt conditions can be improved.
Example 4
A high-temperature resistant petroleum resin dispersoid plugging agent is prepared from the following raw materials in percentage by weight: 10% of C9 petroleum resin, 0.2% of octadecyl dimethyl ammonium oxide, 0.15% of cationic polyacrylamide, 0.2% of triethanolamine, 0.2% of sodium bisulfite, 1.1% of silicon dioxide nano particles, 0.3% of sodium hydroxide and the balance of water; the sum of the mass percentages of the raw materials is 100 percent.
The preparation method of the high-temperature resistant petroleum resin dispersion plugging agent is consistent with the example 1, except that: 50g of a 0.3% by mass aqueous solution of cationic polyacrylamide was added, and the other steps and conditions were the same as in example 1.
Simulating the conditions of a high-temperature oil reservoir and an oil well, namely stirring the obtained petroleum resin dispersoid plugging agent for 5 hours at the temperature of 90 ℃ to obtain the plugging agent after high-temperature treatment, wherein in the plugging agent, cationic polyacrylamide is subjected to modification reaction to generate sulfonic modified cationic polyacrylamide with the weight-average molecular weight of 750 × 104(ii) a After the plugging agent after high-temperature treatment is placed at 130 ℃ for 18 hours, the petroleum resin is still stably dispersed, and no coalescence phenomenon occurs, which indicates that when the dosage of the cationic polyacrylamide is within the range of the invention, the dosage is increased, and the stability of the petroleum resin under high temperature and high salt conditions can be improved.
Example 5
A high-temperature resistant petroleum resin dispersoid plugging agent is prepared from the following raw materials in percentage by weight: 10% of C9 petroleum resin, 0.25% of octadecyl dimethyl ammonium oxide, 0.3% of cationic polyacrylamide, 0.2% of triethanolamine, 0.2% of sodium bisulfite, 1.1% of silicon dioxide nano particles, 0.3% of sodium hydroxide and the balance of water; the sum of the mass percentages of the raw materials is 100 percent.
The preparation method of the high-temperature resistant petroleum resin dispersion plugging agent is consistent with the example 2, except that: 50g of a 0.6% by mass aqueous solution of cationic polyacrylamide was added, and the other steps and conditions were the same as in example 2.
Simulating the conditions of a high-temperature oil reservoir and an oil well, namely stirring the obtained petroleum resin dispersoid plugging agent for 5 hours at the temperature of 90 ℃ to obtain the plugging agent after high-temperature treatment, wherein in the plugging agent, cationic polyacrylamide is subjected to modification reaction to generate sulfonic modified cationic polyacrylamide with the weight-average molecular weight of 750 × 104(ii) a After the plugging agent after high-temperature treatment is placed at 130 ℃ for 22 hours, the petroleum resin is still stably dispersed, and no coalescence phenomenon occurs, which indicates that when the dosage of the cationic polyacrylamide is within the range of the invention, the dosage is increased, and the stability of the petroleum resin under high temperature and high salt conditions can be improved.
Example 6
A high-temperature resistant petroleum resin dispersoid plugging agent is prepared from the following raw materials in percentage by weight: 10% of C9 petroleum resin, 0.3% of octadecyl dimethyl ammonium oxide, 0.15% of cationic polyacrylamide, 0.2% of triethanolamine, 0.2% of sodium bisulfite, 1.1% of silicon dioxide nano particles, 0.3% of sodium hydroxide and the balance of water; the sum of the mass percentages of the raw materials is 100 percent.
The preparation method of the high-temperature resistant petroleum resin dispersion plugging agent is consistent with the embodiment 3, except that: 50g of a 0.3% by mass aqueous solution of cationic polyacrylamide was added, and the other steps and conditions were the same as in example 3.
Simulating the conditions of the high-temperature oil reservoir oil well: stirring the petroleum resin dispersoid plugging agent obtained above at 90 ℃ for 5h to obtain the plugging agent after high-temperature treatment.In the plugging agent, cationic polyacrylamide is subjected to modification reaction to generate sulfonic group modified cationic polyacrylamide with the weight average molecular weight of 750 × 104(ii) a After the plugging agent after high-temperature treatment is placed at 130 ℃ for 18 hours, the petroleum resin is still stably dispersed, and no coalescence phenomenon occurs, which indicates that when the dosage of the cationic polyacrylamide is within the range of the invention, the dosage is increased, and the stability of the petroleum resin under high temperature and high salt conditions can be improved.
Comparative example 1
A method of making a blocking agent, as described in example 1, except that: no sodium hydroxide was added and the other steps and conditions were identical to those of example 1.
Simulating the conditions of the high-temperature oil reservoir oil well: and stirring the obtained plugging agent for 5 hours at 90 ℃ to obtain the plugging agent after high-temperature treatment. After the plugging agent subjected to high-temperature treatment is placed at 130 ℃ for 3 hours, the petroleum resin is subjected to a coalescence phenomenon, which shows that the modified cationic polyacrylamide can effectively improve the stability of the petroleum resin at high temperature and high salt.
The plugging agent prepared by the comparative example has short stabilization time, can not be injected into the deep part of an oil reservoir and an oil well, and can plug a near wellbore zone due to premature coalescence.
Comparative example 2
Adding 0.05g of resorcinol and 0.1g of urotropin into 50g of tap water, stirring uniformly to fully dissolve or disperse, mixing 50g of an anionic polyacrylamide solution with a mass concentration of 15% and a hydrolysis degree of 20% prepared by using tap water with the solution, stirring uniformly, placing the obtained gel-forming liquid into an ampoule bottle, and sealing. Then placing the mixture in an oven at 130 ℃, respectively standing for 20 days, 60 days and 90 days, and calculating the dehydration rate of the jelly in the ampoule bottle.
TABLE 1 Water-based jelly dehydration Rate
In the comparative example, the gel is seriously dehydrated, so that the plugging capability of the gel in the stratum is influenced, and the plugging capability of the gel is greatly reduced.
Application example
Investigation of plugging capability:
the plugging agents obtained in examples 1 to 6 after the high-temperature treatment were used as the subjects of the study, and the plugging ability of the petroleum resin dispersion provided by the present invention was examined. The gel-forming liquid obtained in comparative example 2 was used as a research object to examine the blocking ability of the polyacrylamide blocking agent and was used as a comparison. The specific simulation experiment process is as follows: filling quartz sand into seven sand filling pipes with the inner diameter of 2.5cm and the length of 20cm to obtain simulated cores respectively marked as 1#, 2#, 3#, 4#, 5#, 6# and 7#, and driving water until the pressure is stable to obtain the original permeability k1Then, the plugging agent after the high-temperature treatment in "examples 1 to 6" and the gelling solution obtained in "comparative example 2" were reversely injected into the seven sand-packed pipes, respectively, with a volume of 0.25PV (core pore volume), then 0.25PV water was injected for replacement (the purpose of injection was to replace the plugging agent into the middle of the sand-packed pipe and to inject into the deep part of the formation under the simulated formation conditions), then the seven sand-packed pipes were placed in an oven at 130 ℃ for aging for 30 days and 80 days, respectively, and finally water was driven until the pressure was stable, and the post-plugging permeability k of the simulated core was measured2And according to the formula E ═ k1-k2)/k1And calculating the core plugging rate E by 100%, wherein the experimental result is shown in the following table.
Table 2 plugging capability test data
The above experimental results show that: the petroleum resin dispersion plugging agent provided by the invention has excellent plugging performance at a high temperature of 130 ℃, and compared with comparative example 2, the plugging effect of the petroleum resin dispersion plugging agent is not as good as that of the petroleum resin dispersion plugging agent after 20 days or 90 days, and the petroleum resin dispersion plugging agent has a long-term stable plugging effect.
Claims (7)
1. A high-temperature resistant petroleum resin dispersoid plugging agent is prepared from the following raw materials in percentage by weight: 5 to 15 percent of petroleum resin, 0.1 to 0.5 percent of surfactant, 0.05 to 0.4 percent of cationic polyacrylamide, 0.1 to 0.4 percent of triethanolamine, 0.1 to 0.5 percent of sodium bisulfite, 1 to 3 percent of silicon dioxide nano particles, 0.1 to 0.5 percent of pH regulator and the balance of water; the sum of the mass percentages of the raw materials is 100 percent;
the petroleum resin is C5 or C9 petroleum resin, the relative molecular mass is 1000-5000, the softening point is 100-120 ℃, the surfactant is octadecyl dimethyl ammonium oxide, and the weight-average molecular weight of the cationic polyacrylamide is 700 × 104～800×104The cation degree is 20-40%, the particle size of the silicon dioxide nano particles is 10-14nm, the pH regulator is sodium hydroxide, and the water has the mineralization degree of (20-25) × 104mg/L of formation water, wherein Na+The content is (7-8) × 104mg/L、Ca2+The content of the active component is (0.5-1.5) × 104mg/L、Mg2+The content of the active component is (0.1-0.2) × 104mg/L、HCO3 -The content of the extract is (0.01-0.02) × 104mg/L、Cl-The content is (13-14) × 104mg/L。
2. The high-temperature resistant petroleum resin dispersion plugging agent according to claim 1, which is prepared from the following raw materials in percentage by weight: 5 to 10 percent of petroleum resin, 0.1 to 0.3 percent of surfactant, 0.05 to 0.3 percent of cationic polyacrylamide, 0.1 to 0.2 percent of triethanolamine, 0.15 to 0.4 percent of sodium bisulfite, 1 to 2 percent of silicon dioxide nano particles, 0.2 to 0.4 percent of pH regulator and the balance of water; the sum of the mass percentages of the raw materials is 100 percent.
3. The high temperature resistant petroleum resin dispersion plugging agent of claim 1, wherein said water has a degree of mineralization of 22.3 × 104mg/L of formation water, wherein Na+The content is 7.3 × 104mg/L、Ca2+The content is 1.1 × 104mg/L、Mg2+The content is 0.15 × 104mg/L、HCO3 -The content is 0.018 × 104mg/L、Cl-The content is 13.7 × 104mg/L。
4. The method of preparing a high temperature resistant petroleum resin dispersion block agent of any one of claims 1 to 3, comprising the steps of:
dissolving a surfactant in water, adding petroleum resin powder, and fully dispersing to obtain a petroleum resin dispersion liquid; dissolving cationic polyacrylamide, triethanolamine, sodium bisulfite and a pH regulator in water, adding silicon dioxide nanoparticles, and fully dispersing to obtain a mixed solution; and uniformly mixing the mixed solution and the petroleum resin dispersion solution to obtain the petroleum resin dispersion plugging agent.
5. The method for preparing the high temperature resistant petroleum resin dispersion plugging agent according to claim 4, wherein the petroleum resin powder is obtained by crushing petroleum resin into powder with a particle size of 0.5-10 microns by using a freezing and crushing method, namely using liquid nitrogen as a cold source.
6. The method for preparing the high-temperature resistant petroleum resin dispersion plugging agent according to claim 4, wherein the mass concentration of the petroleum resin in the petroleum resin dispersion liquid is 25-30%.
7. The use of the high temperature resistant petroleum resin dispersion plugging agent of any one of claims 1-3 in high temperature reservoir oil wells for profile control and water plugging;
injecting the petroleum resin dispersion plugging agent into a high-temperature oil reservoir oil well, and gradually increasing the temperature from top to bottom in the oil reservoir oil well to obtain sulfonic modified cationic polyacrylamide through sulfonic modification reaction of cationic polyacrylamide in the petroleum resin dispersion plugging agent, triethanolamine and sodium bisulfite, wherein the weight average molecular weight of the sulfonic modified cationic polyacrylamide is 710 × 104～810×104The petroleum resin dispersion plugging agent can effectively disperse and stabilize petroleum resin suspension, and effectively improve the high temperature resistance, salt resistance and stability of the petroleum resin dispersion plugging agent, thereby achieving the purpose of injecting the petroleum resin dispersion plugging agent into the deep part of an oil reservoir oil well without blocking a near well zone and entering the oilThe petroleum resin at the deep part of the oil-storing well begins to soften and become sticky, so that the water flow channel is coalesced and blocked to achieve the purpose of water blocking.
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| CN113088269B (en) * | 2019-12-23 | 2023-01-31 | 中石化南京化工研究院有限公司 | Organic-inorganic composite water shutoff agent |
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| CN101935520A (en) * | 2010-07-19 | 2011-01-05 | 中国海洋石油总公司 | Novel emulsion organic resin selective plugging agent |
| CN106047324A (en) * | 2016-06-30 | 2016-10-26 | 中国石油大学(华东) | Reinforced gel dispersion deep profile control and flooding agent for low-permeability high-temperature high-salt oil reservoirs |
| CN106634906A (en) * | 2016-09-18 | 2017-05-10 | 中国石油大学(华东) | Gel with high temperature resistance |
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| CN101935520A (en) * | 2010-07-19 | 2011-01-05 | 中国海洋石油总公司 | Novel emulsion organic resin selective plugging agent |
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