CN112321764B - Temperature-resistant salt-resistant viscoelastic particle oil displacement agent and preparation method and application thereof - Google Patents

Temperature-resistant salt-resistant viscoelastic particle oil displacement agent and preparation method and application thereof Download PDF

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CN112321764B
CN112321764B CN202110000619.2A CN202110000619A CN112321764B CN 112321764 B CN112321764 B CN 112321764B CN 202110000619 A CN202110000619 A CN 202110000619A CN 112321764 B CN112321764 B CN 112321764B
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temperature
reaction
displacement agent
oil displacement
resistant
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CN112321764A (en
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齐书磊
李慎伟
姜祖明
杨姗
陈海燕
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Shandong Juxing Petroleum Technology Co.,Ltd.
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Dongying Juxing Petroleum Technology Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/04—Acids; Metal salts or ammonium salts thereof
    • C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F4/00—Polymerisation catalysts
    • C08F4/42—Metals; Metal hydrides; Metallo-organic compounds; Use thereof as catalyst precursors
    • C08F4/72—Metals; Metal hydrides; Metallo-organic compounds; Use thereof as catalyst precursors selected from metals not provided for in group C08F4/44
    • C08F4/74—Metals; Metal hydrides; Metallo-organic compounds; Use thereof as catalyst precursors selected from metals not provided for in group C08F4/44 selected from refractory metals
    • C08F4/78—Metals; Metal hydrides; Metallo-organic compounds; Use thereof as catalyst precursors selected from metals not provided for in group C08F4/44 selected from refractory metals selected from chromium, molybdenum or tungsten
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F8/00—Chemical modification by after-treatment
    • C08F8/12—Hydrolysis
    • 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
    • C09K8/58—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids
    • C09K8/584—Compositions for enhanced recovery methods for obtaining hydrocarbons, i.e. for improving the mobility of the oil, e.g. displacing fluids characterised by the use of specific surfactants
    • 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
    • C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
    • C09K2208/30—Viscoelastic surfactants [VES]

Abstract

The invention provides a temperature-resistant salt-resistant viscoelastic particle oil displacement agent, and a preparation method and application thereof, and belongs to the technical field of oil exploitation, transportation and chemical engineering. The viscoelastic particle oil displacement agent provided by the invention is prepared by polymerizing acrylic acid, 2-acrylamide-2-methylpropanesulfonic acid and acrylamide as monomer molecules step by step, and can effectively control the polymerization reaction speed, so that a branched chain at the tail end of a polymer network is more stretched, and the polymer has higher viscosity and better temperature and salt resistance. The viscoelastic particle oil displacement agent provided by the invention is applied to higher temperature and mineralization degree, has good elastic modulus of a water dispersion system, median value of particle size after swelling, network structure content and viscosity of the water dispersion system, and can realize excellent viscoelastic property and migration property. In addition, under the temperature of 90 ℃ and the mineralization degree of 32868mg/L, the polymer flooding oil deposit, the high-temperature high-salinity oil deposit and the serious heterogeneous oil deposit can still deeply enter the polymer flooding oil deposit to play the roles of plugging and profile control, the swept range is expanded, and the recovery ratio is improved.

Description

Temperature-resistant salt-resistant viscoelastic particle oil displacement agent and preparation method and application thereof
Technical Field
The invention belongs to the technical field of oil exploitation, transportation and chemical engineering, and relates to a temperature-resistant salt-resistant viscoelastic particle oil displacement agent, and a preparation method and application thereof.
Background
Most of old oil fields in the east of China enter the middle and later exploitation stages, after long-term development of secondary oil recovery and tertiary oil recovery, the recovery rate of crude oil is greatly reduced, and in addition, the severe oil reservoir conditions such as high temperature and high salinity and the like cause that 60-70% of crude oil in the underground is still difficult to effectively exploit. The method for improving the recovery ratio after polymer flooding at the present stage is difficult to meet the requirement of further and greatly improving the recovery ratio. Therefore, the brand-new oil displacement agent for effectively exploiting a large amount of residual oil in old oil fields is created, and the brand-new oil displacement agent becomes an urgent task for guaranteeing the continuous supply of crude oil in China.
Patent application CN111635748A discloses a viscoelastic particle oil displacement agent with a water shutoff function, wherein cross-linking agents of the viscoelastic particle oil displacement agent are bis-azo (N, N' -dimethylene isobutyramide) dihydrochloride and bis-azo (2-amidinopropane) dihydrochloride, organic chlorine is easily introduced into the synthesized viscoelastic particle oil displacement agent, and the requirement of 0% of the organic chlorine content in the technical requirement Q/SH 102023742020 on the viscoelastic particle oil displacement agent is not met. Patent application CN101775275A discloses a novel viscoelastic particle oil displacement agent and a preparation method thereof, wherein the synthetic raw material of the novel viscoelastic particle oil displacement agent is only acrylamide, no branched chain is introduced into the terminal of the main chain network of the synthesized novel viscoelastic particle oil displacement agent, the temperature resistance, salt resistance, jelly strength and tackifying effect are poor, and the expansion time is short. Therefore, the viscoelastic particle oil displacement agent which has stronger plugging capability, better polymer tackifying effect, better temperature resistance and salt resistance, better stability, easy injection, easy driving and dynamic profile control has important significance for improving the recovery ratio of the oil deposit after polymer flooding, the high-temperature high-salt oil deposit and the severe heterogeneous oil deposit in the victory oil field.
Disclosure of Invention
The invention provides a temperature-resistant salt-resistant viscoelastic particle oil displacement agent, a preparation method and application thereof, wherein the viscoelastic particle oil displacement agent adopts acrylic acid, 2-acrylamide-2-methylpropanesulfonic acid and acrylamide as reaction raw materials, and is matched with the reaction raw materials by an optimal process, so that the excellent blocking effect and liquid flow diversion effect can be realized, and the oil displacement agent can really realize the oil displacement function due to easy injection, easy driving, easy deformation, difficult sedimentation and good temperature resistance and salt resistance.
In order to achieve the aim, the invention provides a preparation method of a temperature-resistant salt-tolerant viscoelastic particle oil displacement agent, which comprises the following steps:
adding deionized water and acrylic acid into a reaction kettle, adding 2-acrylamide-2-methylpropanesulfonic acid into a reaction system after the deionized water and the acrylic acid are completely dissolved, keeping the reaction system at 10-15 ℃, and stirring the mixture until the mixture is fully and uniformly mixed;
adding a cross-linking agent N, N-dimethylacrylamide into the reaction system, fully and uniformly mixing, adjusting the pH value in the reaction kettle under the protection of nitrogen, slowly adding a molybdenum polyoxometallate-polyol initiation system into the reaction system, sealing the reaction kettle, and reacting for 3-4 hours to initiate the prepolymerization of the aqueous solution;
after the prepolymerization reaction is finished, adding the prepolymerization product into acrylamide, and continuing to react for 2-3 h at the final reaction temperature of 40 +/-1 ℃;
and (3) introducing steam into a steam heater of the reaction kettle to raise the temperature, raising the temperature of the colloid in the kettle to 75-80 ℃ to perform hydrolysis reaction for 4-6 hours, taking out the polymerization sample after the reaction is finished, grinding and granulating, drying and screening to obtain the temperature-resistant salt-resistant viscoelastic particle oil displacement agent.
Preferably, the mass ratio of the added acrylic acid, 2-acrylamide-2-methylpropanesulfonic acid, acrylamide and deionized water is (0.1-0.3): (0.01-0.05): (0.15-0.5): 1. it is understood that the mass ratio of the added acrylic acid, 2-acrylamido-2-methylpropanesulfonic acid, acrylamide and deionized water may be adjusted within the above range according to the actual circumstances, and may be, for example, 0.1:0.01:0.15:1, 0.1:0.05:0.5:1, 0.2:0.03:0.325:1, 0.3:0.01:0.15:1, 0.3:0.05:0.5:1, 0.3:0.05:0.15:1, 0.2:0.02:0.3:1, 0.2:0.03:0.2:1, 0.2:0.04:0.4:1, 0.1:0.02:0.2:1, 0.3:0.04:0.2: 1.
Preferably, the mass of the added crosslinking agent N, N-dimethylacrylamide accounts for 1% -3% of the total mass of the reaction system.
Preferably, the pH value in the reaction kettle is adjusted to 8-10. It can be understood that the proper pH value of the solution can effectively adjust the crosslinking degree and the branching degree of the viscoelastic particle oil-displacing agent, if the pH value is too high, the reaction rate is higher, which means that the concentration of active free radicals in the solution is increased, the monomer molecules of the viscoelastic particle oil-displacing agent are rapidly crosslinked, and the branching effect is poor; if the pH value is too low, the initiation rate of the monomer molecules is reduced, and the chain length of the molecular main chain of the viscoelastic particle oil displacement agent is shortened.
Preferably, the ratio of polyoxometallate of molybdenum in the initiating system: the mass ratio of the polyhydric alcohol is (0.05-0.1): 1, and the initiating system accounts for 0.1-0.3% of the total mass of the reaction system. It is understood that the mass ratio of the polyoxometalate of molybdenum and the polyol can be adjusted within the above range according to practical circumstances, and for example, can also be 0.05:1, 0.06:1, 0.07:1, 0.08:1, 0.09:1 or any ratio within the above range. In addition, the initiation system may also be present in an amount of 0.1, 0.15, 0.2, 0.25, 0.3% or any value within the above range, based on the total mass of the reaction system.
Preferably, the multimetal heteropolyacid salt of molybdenum in the initiating system is selected from, but not limited to, [ Bmim ]]4[SiMo12O40]、[Hmim]4[SiMo12O40]、[Hmim]3[PMo12O40]、[Dhmim]3[AsMo12O40]One or more of them.
Preferably, the polyol in the initiation system is at least one selected from the group consisting of ethylene glycol, glycerol, and pentaerythritol.
The invention provides a temperature-resistant salt-resistant viscoelastic particle oil displacement agent prepared by the preparation method according to any one of the technical schemes.
The invention provides an application of the temperature-resistant salt-tolerant viscoelastic particle oil displacement agent according to the technical scheme in oilfield exploitation at the temperature of less than or equal to 90 ℃ and the mineralization degree of less than or equal to 32868mg/L (wherein the total amount of calcium ions and magnesium ions is 874 mg/L).
Preferably, the elastic modulus of the aqueous dispersion is more than or equal to 41.6Pa at the temperature of 35 ℃ and the mineralization degree of 32868 mg/L; under room temperature and mineralization degree of 32868mg/L, the median of the particle size after swelling is more than or equal to 761 μm; at the high temperature of 90 ℃ and the mineralization degree of 32868mg/L, the content of the network structure is more than or equal to 65.7 percent, and the viscosity of the water dispersion system is more than or equal to 157.2 mPa.s.
Compared with the prior art, the invention has the advantages and positive effects that:
1. the viscoelastic particle oil displacement agent provided by the invention is prepared by polymerizing acrylic acid, 2-acrylamide-2-methylpropanesulfonic acid and acrylamide as monomer molecules step by step, and can effectively control the polymerization reaction speed, so that a branched chain at the tail end of a polymer network is more stretched, the viscosity of the polymer is higher, the temperature resistance and salt resistance performance are better, and the chain length shortening and viscosity reduction of linear polymers caused by implosion are avoided.
2. In the initiation system provided by the invention, on one hand, the polymetallic heteropoly acid salt of molybdenum can form a plurality of free radical active points with Keggin three-dimensional structures on a polymer chain; on the other hand, the structure of the heteropolyanion has adjustability, and the central atom and the coordination atom can be changed through the adjustability, so that the aims of the multiple oxidability and reducibility of the heteropolyanion are fulfilled. The two factors act together to excite the ortho-carbon of each hydroxyl of the polyhydric alcohol, initiate free radical polymerization to form a branched chain, terminate coupling through partial chain end free radicals to form space effective crosslinking, and the uncrosslinked partial chain end free radicals form a long-chain branched structure.
3. The viscoelastic particle oil displacement agent provided by the invention has good elastic modulus of a water dispersion system, median value of particle size after swelling, content of network structure and viscosity of the water dispersion system at higher temperature and higher mineralization degree, and can realize excellent viscoelastic property and migration property.
4. The viscoelastic particle oil displacement agent provided by the invention can still go deep into an oil reservoir after polymer flooding, a high-temperature high-salt oil reservoir and a severe heterogeneous oil reservoir to play the roles of plugging, profile control and flooding at the temperature of 90 ℃ and the mineralization degree of 32868mg/L, so that the sweep range is expanded, and the recovery ratio is improved.
Detailed Description
In order to more clearly and specifically describe the synthesis and application of the viscoelastic particle oil displacement agent provided in the embodiment of the present invention, the technical solutions in the embodiment of the present invention will be clearly and completely described below, and it is obvious that the described embodiment is only a part of the embodiment of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Preparing simulated saline water:
placing a 5L narrow-necked flask on a 10kg balance, adding 4831.8g of distilled water to the narrow-necked flask, placing it on a magnetic stirrer after adding the magnetic stirrer, starting the stirrer to swirl the solution, and adding the following substances in the order listed: 9.716g of anhydrous calcium chloride, 7.344g of magnesium chloride hexahydrate and 151.19g of sodium chloride. Each reagent is added until it is completely dissolved before the other reagent is added. Stirring with magnetic stirrer for 15 min. The total mineralization of the obtained solution is 32868mg/L, wherein the total amount of calcium ions and magnesium ions is 874 mg/L.
The method for measuring the product performance comprises the following steps:
1 solid content
1.1 weigh clean and dried to constant weight bottle mass to an accuracy of 0.0001g, recorded as m1。
1.2 Add about 2g viscoelastic particle displacement agent sample into constant weight weighing bottle, make sample evenly spread in weighing bottle, accurate to 0.0001g, mark as m2。
1.3 placing the weighing bottle with the sample in the 1.2 into a constant temperature drying box, and drying for 2 hours at the constant temperature of (105 +/-2) DEG C.
1.4 taking out the weighing bottle, putting the weighing bottle into a dryer, cooling for 30min, weighing until the weight is accurate to 0.0001g, and recording as m3。
1.5 three replicates of one sample were taken and the arithmetic mean was used as the measurement. When the individual values deviate from the arithmetic mean by more than 0.5%, a resampling measurement is required.
1.6 the solids S is calculated as follows:
S=(m3-m1/m2-m1)×100%… (1)
in the formula:
s-solid content,%;
m1-weighing the bottle mass, g;
m2-sample mass before drying, g;
m3-sample mass after drying, g.
2 content of network structure
2.1 accurately weighing 1 g-1.5 g of viscoelastic particle oil displacement agent B-PPG sample to be accurate to 0.0001g, and recording the sample as m1。
2.2 weighing a certain amount of simulated saline (degree of mineralization 32868 mg/L) into a 150 mL beaker, starting a constant speed stirrer, slowly adding a sample along the vortex wall for 30 s at the speed of (400 +/-20) r/min, and then stirring for 15-30 min at the speed of (500 +/-20) r/min until the particles are uniformly dispersed.
2.3 transferring the prepared solution into a 1000 mL measuring cylinder, washing the beaker with a small amount of water for several times, and adding standard prepared brine into the measuring cylinder to ensure that the liquid level is maintained at a distance of about 5-10 cm from the upper opening end.
2.4 to prevent the particles from being entrained by the dissolved air bubbles in the water, the mixture was gently stirred with a glass rod every 10 min and repeated three times.
2.5 precipitation for about 5-6 h. During pouring the solution, attention is paid to the interface between the B-PPG network structure and the aqueous solution at the moment, and the interface reaches a position 5 cm away from the outlet end and stops.
2.6 repeat steps 2.4, 2.5 three times.
2.7 taking the precipitate below the interface, washing with absolute ethyl alcohol to obtain a white insoluble substance, repeatedly washing with absolute ethyl alcohol for 2 times, standing for a little, transferring the insoluble substance to a surface dish, placing in a constant-temperature drying oven, and drying at 90 ℃ for 2 h.
2.8 taking out the insoluble substances, putting into a dryer, cooling for 30min, weighing to the accuracy of 0.0001g, recording as m2。
2.9 network structure N is calculated as:
Figure 242092DEST_PATH_IMAGE001
in the formula:
n-network structure content,%;
m1-initial sample mass, g;
m2-sample mass after washing the pellet, g.
3 median particle diameter after swelling
3.1 accurately weighing (5/S) g of viscoelastic particle oil displacement agent sample (S is solid content) to be accurate to 0.0001 g. Weighing (1000-5/S) g of simulated saline in a 1000 mL wide-mouth bottle, starting a constant speed stirrer to slowly add a sample along the vortex wall for 30S at (400 +/-20) r/min, and then stirring for 2h at the stirring speed of (500 +/-20) r/min to obtain a solution with the concentration of 5000 mg/L.
3.2 taking a proper amount of the test solution prepared in the step 3.1, and measuring the median particle size (D50) on a laser particle distribution measuring instrument according to the operation steps.
4 modulus of elasticity of aqueous dispersion
4.1 taking a proper amount of simulated saline for testing the viscoelastic particle oil displacement agent.
4.2 starting up and setting conditions according to the rheometer operating instruction, setting the measuring temperature to be 35 ℃, selecting a flat plate mode and a rotor model PP60Ti, taking a proper amount of test solution on the flat plate, setting the gap to be 200 mu m, descending the machine head to the set gap, and wiping off redundant test solution. And (4) determining the elastic modulus of the viscoelastic particle oil-displacing agent water dispersion system with the concentration of 5000mg/L according to the operation instruction of a rheometer.
4.3 Each sample should be processed into 3 parallel samples according to 4.1-4.2, the relative error of each measured value and the arithmetic mean value is not more than 10%, and the arithmetic mean value is taken as the measured result.
5 viscosity of aqueous Dispersion
5.1 taking proper amount of simulated saline for viscoelastic particle oil displacement agent experiments.
5.2 starting up and setting conditions according to the rheometer operation instruction, setting the measurement temperature to be 90 ℃, moving the solution to be measured into a measuring cylinder, keeping the temperature for 3min, selecting a coaxial cylinder mode, setting the rotor model number CC27 and the shear rate to be 7.34s-1And measuring the viscosity of the dispersion system with the concentration of 5000mg/L within 1min according to the operation instruction of the rheometer, and taking the average value of the viscosity to obtain the viscosity of the dispersion system.
5.3 each sample should be processed into 3 parallel samples according to 5.1-5.2, the relative error of each measured value and the arithmetic mean value is not more than 10%, and the arithmetic mean value is taken as the measured result.
Example 1
Adding 100Kg of deionized water into a reaction kettle, adding 10Kg of Acrylic Acid (AA), adding 1Kg of AMPS into the reaction system after completely dissolving, simultaneously keeping the temperature of the reaction system at 10 ℃, stirring for 1h, and finally fully stirring and uniformly mixing. Adding 1.26Kg of N, N-Dimethylacrylamide (DMAM) into the reaction system, and after the N, N-Dimethylacrylamide (DMAM) is dissolved and uniformly mixed, introducing nitrogen into the reaction liquid for 30min at a nitrogen port at the bottom of the reaction kettle so as to be convenient for fully removing oxygen in the reaction system. Adjusting the pH value in the reaction kettle, and slowly adding 0.006Kg of [ Bmim ] into the reaction system under the protection of nitrogen]4[SiMo12O40]And 0.12Kg of an aqueous ethylene glycol-initiated system was prepolymerized. The reaction kettle is sealed, and the reaction time is 3 hours.
After the prepolymerization was completed, the prepolymerization product was added to 15Kg AM, and the reaction was continued for 2 hours at a final reaction temperature of about 40 ℃ and the temperature change during the reaction was recorded. And (3) introducing steam into a steam heater in the reaction kettle to raise the temperature, so that the temperature of colloid in the kettle is raised to 75 ℃, starting hydrolysis reaction, wherein the hydrolysis reaction period is 4h, taking out a polymerization sample after the hydrolysis reaction is finished, grinding and granulating, drying in a vacuum drying oven at 105 ℃, and screening by a standard screen to obtain the viscoelastic particle oil displacement agent JX-1.
Example 2
Adding 100Kg of deionized water into a reaction kettle, adding 10Kg of Acrylic Acid (AA), adding 5Kg of AMPS into the reaction system after completely dissolving, simultaneously keeping the temperature of the reaction system at 15 ℃, stirring for 1h, and finally fully stirring and uniformly mixing. 4.95Kg of N, N-Dimethylacrylamide (DMAM) is added into the reaction system, and after the N, N-dimethylacrylamide is dissolved and uniformly mixed, nitrogen is introduced into the reaction liquid for 30min from a nitrogen port at the bottom of the reaction kettle, so that oxygen in the reaction system can be removed sufficiently. Adjusting the pH value in the reaction kettle, and slowly adding 0.045Kg [ Hmim ] into the reaction system under the protection of nitrogen]4[SiMo12O40]And 0.45Kg of an aqueous pentaerythritol initiating system. The reaction kettle is sealed, and the reaction time is 4 hours.
After the prepolymerization was completed, the prepolymerization product was added to 50Kg AM, and the reaction was continued for 3 hours at a final reaction temperature of about 40 ℃ and the temperature change during the reaction was recorded. And (3) introducing steam into a steam heater in the reaction kettle to raise the temperature, raising the temperature of the gel in the kettle to 80 ℃, starting hydrolysis reaction, wherein the hydrolysis reaction period is 6 hours, taking out the polymerization sample after the hydrolysis reaction is finished, grinding and granulating, drying in a vacuum drying oven at 105 ℃, and screening by a standard sieve to obtain the viscoelastic particle oil-displacing agent JX-2.
Example 3
Adding 100Kg of deionized water into a reaction kettle, adding 20Kg of Acrylic Acid (AA), adding 3Kg of AMPS into the reaction system after completely dissolving, simultaneously keeping the temperature of the reaction system at 12 ℃, stirring for 1h, and finally fully stirring and uniformly mixing. To the direction of3.11Kg of N, N-Dimethylacrylamide (DMAM) is added into the reaction system, after the N, N-dimethylacrylamide is dissolved and mixed fully and uniformly, nitrogen is introduced into the reaction liquid for 30min from a nitrogen port at the bottom of the reaction kettle, so that oxygen in the reaction system can be removed fully. Adjusting the pH value in the reaction kettle, and slowly adding 0.0217Kg of [ Hpy ] into the reaction system under the protection of nitrogen]4[GeMo12O40]And 0.2893Kg of glycerol as an aqueous initiation system. The reaction kettle is sealed, and the reaction time is 3.5 h.
After the prepolymerization was completed, the prepolymerization product was added to 32.5Kg AM and the reaction was continued for 2.5 hours at a final reaction temperature of about 40 ℃ and the temperature change during the course was recorded. And (3) introducing steam into a steam heater in the reaction kettle to raise the temperature, raising the temperature of the gel in the kettle to 78 ℃, starting hydrolysis reaction, wherein the hydrolysis reaction period is 5 hours, taking out the polymerization sample after the hydrolysis reaction is finished, grinding and granulating, drying in a vacuum drying oven at 105 ℃, and screening by a standard sieve to obtain the viscoelastic particle oil-displacing agent JX-3.
Example 4
Adding 100Kg of deionized water into a reaction kettle, adding 30Kg of Acrylic Acid (AA), adding 1Kg of AMPS into the reaction system after completely dissolving, simultaneously keeping the temperature of the reaction system at 10 ℃, stirring for 1h, and finally fully stirring and uniformly mixing. Adding 1.45Kg of N, N-Dimethylacrylamide (DMAM) into the reaction system, and after the N, N-Dimethylacrylamide (DMAM) is dissolved and uniformly mixed, introducing nitrogen into the reaction liquid for 30min at a nitrogen port at the bottom of the reaction kettle so as to be convenient for fully removing oxygen in the reaction system. Adjusting the pH value in the reaction kettle, and slowly adding 0.0069Kg of Dhmim into the reaction system under the protection of nitrogen]3[AsMo12O40]And 0.1381Kg of glycerol as an aqueous initiation system. The reaction kettle is sealed, and the reaction time is 3 hours.
After the prepolymerization was completed, the prepolymerization product was added to 15Kg AM, and the reaction was continued for 2 hours at a final reaction temperature of about 40 ℃ and the temperature change during the reaction was recorded. And (3) introducing steam into a steam heater in the reaction kettle to raise the temperature, so that the temperature of colloid in the kettle is raised to 75 ℃, starting hydrolysis reaction, wherein the hydrolysis reaction period is 4h, taking out a polymerization sample after the hydrolysis reaction is finished, grinding and granulating, drying in a vacuum drying oven at 105 ℃, and screening by a standard screen to obtain the viscoelastic particle oil displacement agent JX-4.
Example 5
Adding 100Kg of deionized water into a reaction kettle, adding 30Kg of Acrylic Acid (AA), adding 5Kg of AMPS into the reaction system after completely dissolving, simultaneously keeping the temperature of the reaction system at 15 ℃, stirring for 1h, and finally fully stirring and uniformly mixing. Adding 5.55Kg of N, N-Dimethylacrylamide (DMAM) into the reaction system, and after the N, N-Dimethylacrylamide (DMAM) is dissolved and uniformly mixed, introducing nitrogen into the reaction liquid for 30min at a nitrogen port at the bottom of the reaction kettle so as to be convenient for fully removing oxygen in the reaction system. Adjusting the pH value in the reaction kettle, and slowly adding 0.0505Kg of Hmim into the reaction system under the protection of nitrogen]3[PMo12O40]And 0.5045Kg of ethylene glycol as an aqueous initiating system. The reaction kettle is sealed, and the reaction time is 4 hours.
After the prepolymerization was completed, the prepolymerization product was added to 50Kg AM, and the reaction was continued for 3 hours at a final reaction temperature of about 40 ℃ and the temperature change during the reaction was recorded. And (3) introducing steam into a steam heater in the reaction kettle to raise the temperature, raising the temperature of the gel in the kettle to 80 ℃, starting hydrolysis reaction, wherein the hydrolysis reaction period is 6 hours, taking out the polymerization sample after the hydrolysis reaction is finished, grinding and granulating, drying in a vacuum drying oven at 105 ℃, and screening by a standard sieve to obtain the viscoelastic particle oil-displacing agent JX-5.
Comparative example 1
Adding 100Kg of deionized water into a reaction kettle, adding 10Kg of Acrylamide (AM), adding 1Kg of AMPS into the reaction system after completely dissolving, simultaneously keeping the temperature of the reaction system at 10 ℃, stirring for 1h, and finally fully stirring and uniformly mixing. Adding 1.26Kg of N, N-Dimethylacrylamide (DMAM) into the reaction system, and after the N, N-Dimethylacrylamide (DMAM) is dissolved and uniformly mixed, introducing nitrogen into the reaction liquid for 30min at a nitrogen port at the bottom of the reaction kettle so as to be convenient for fully removing oxygen in the reaction system. Adjusting the pH value in the reaction kettle, and slowly adding 0.006Kg of [ Bmim ] into the reaction system under the protection of nitrogen]4[SiMo12O40]And 0.12Kg of an aqueous ethylene glycol-initiated system was prepolymerized. The reaction kettle is sealed, and the reaction time is 3 hours.
After the prepolymerization was completed, the prepolymerization product was added to 15Kg of AA and the reaction was continued for 2 hours at a final reaction temperature of about 35 ℃ and the temperature change during the reaction was recorded. And (3) introducing steam into a steam heater in the reaction kettle to raise the temperature, so that the temperature of colloid in the kettle is raised to 75 ℃, starting hydrolysis reaction, wherein the hydrolysis reaction period is 4h, taking out a polymerization sample after the hydrolysis reaction is finished, grinding and granulating, drying in a vacuum drying oven at 105 ℃, and screening by a standard screen to obtain the viscoelastic particle oil displacement agent JX-6.
Comparative example 2
Adding 100Kg of deionized water into a reaction kettle, adding 20Kg of Acrylic Acid (AA), adding 3Kg of AMPS into the reaction system after completely dissolving, simultaneously keeping the temperature of the reaction system at 12 ℃, stirring for 1h, and finally fully stirring and uniformly mixing. Adding 3.11Kg of N, N-Dimethylacrylamide (DMAM) into the reaction system, and after the N, N-Dimethylacrylamide (DMAM) is dissolved and uniformly mixed, introducing nitrogen into the reaction liquid for 30min at a nitrogen port at the bottom of the reaction kettle, so as to be convenient for fully removing oxygen in the reaction system. Adjusting the pH value in the reaction kettle, and slowly adding 0.0217Kg of [ Hpy ] into the reaction system under the protection of nitrogen]3[GeMo12O40]And 0.2893Kg of glycerol as an aqueous initiation system. The reaction kettle is sealed, the reaction time is 3.5h, the final reaction temperature is about 30 ℃, and the temperature change in the process is recorded.
And (3) introducing steam into a steam heater in the reaction kettle to raise the temperature, raising the temperature of the gel in the kettle to 78 ℃, starting hydrolysis reaction, wherein the hydrolysis reaction period is 5 hours, taking out the polymerization sample after the hydrolysis reaction is finished, grinding and granulating, drying in a vacuum drying oven at 105 ℃, and screening by a standard sieve to obtain the viscoelastic particle oil-displacing agent JX-7.
Comparative example 3
Adding 100Kg of deionized water into a reaction kettle, adding 30Kg of Acrylic Acid (AA), adding 1Kg of AMPS into the reaction system after completely dissolving, simultaneously keeping the temperature of the reaction system at 10 ℃, stirring for 1h, and finally fully stirring and uniformly mixing. Adding 1.45Kg of N, N-Dimethylacrylamide (DMAM) into the reaction system, and after the N, N-Dimethylacrylamide (DMAM) is dissolved and uniformly mixed, introducing nitrogen into the reaction liquid for 30min at a nitrogen port at the bottom of the reaction kettle so as to be convenient for fully removing oxygen in the reaction system. Adjusting the pH value in the reaction kettle, and slowly adding 0.0069Kg of Dhmim into the reaction system under the protection of nitrogen] ReO4And 0.1381Kg of glycerol as an aqueous initiation system. The reaction kettle is sealed, and the reaction time is 3 hours.
After the prepolymerization was completed, the prepolymerization product was added to 15Kg AM, and the reaction was continued for 2 hours at a final reaction temperature of about 40 ℃ and the temperature change during the reaction was recorded. And (3) introducing steam into a steam heater in the reaction kettle to raise the temperature, so that the temperature of colloid in the kettle is raised to 75 ℃, starting hydrolysis reaction, wherein the hydrolysis reaction period is 4h, taking out a polymerization sample after the hydrolysis reaction is finished, grinding and granulating, drying in a vacuum drying oven at 105 ℃, and screening by a standard screen to obtain the viscoelastic particle oil displacement agent JX-8.
Comparative example 4
Adding 100Kg of deionized water into a reaction kettle, adding 30Kg of Acrylic Acid (AA), adding 5Kg of AMPS into the reaction system after completely dissolving, simultaneously keeping the temperature of the reaction system at 15 ℃, stirring for 1h, and finally fully stirring and uniformly mixing. Adding 5.55Kg of N, N-Dimethylacrylamide (DMAM) into the reaction system, and after the N, N-Dimethylacrylamide (DMAM) is dissolved and uniformly mixed, introducing nitrogen into the reaction liquid for 30min at a nitrogen port at the bottom of the reaction kettle so as to be convenient for fully removing oxygen in the reaction system. Adjusting the pH value in the reaction kettle, and slowly adding 0.0505Kg of Hmim into the reaction system under the protection of nitrogen]4[Mo8O26]And 0.5045Kg of ethylene glycol as an aqueous initiating system. The reaction kettle is sealed, and the reaction time is 4 hours.
After the prepolymerization was completed, the prepolymerization product was added to 50Kg AM, and the reaction was continued for 3 hours at a final reaction temperature of about 40 ℃ and the temperature change during the reaction was recorded. And (3) introducing steam into a steam heater in the reaction kettle to raise the temperature, raising the temperature of the gel in the kettle to 80 ℃, starting hydrolysis reaction, wherein the hydrolysis reaction period is 6 hours, taking out the polymerization sample after the hydrolysis reaction is finished, grinding and granulating, drying in a vacuum drying oven at 105 ℃, and screening by a standard screen to obtain the viscoelastic particle oil-displacing agent JX-9.
Performance testing
In order to further verify that the obtained product has good temperature resistance and salt resistance effects, when the viscoelastic particle oil-displacing agent aqueous solution is measured according to a product performance test method, the experiment is carried out based on the existing technical requirement Q/SH 102023742020 of the viscoelastic particle oil-displacing agent, and on the premise that other conditions are not changed, the specified test mineralization degree is increased from 19334mg/L to 32868mg/L by the particle size median value and the network structure content after swelling; the elastic modulus test temperature of the aqueous dispersion is increased from (25 +/-0.5) DEG C to (35 +/-0.5) DEG C, and the test mineralization is increased from 19334mg/L to 32868 mg/L; the viscosity test temperature of the aqueous dispersion is increased from (75 +/-0.5) DEG C to (90 +/-0.5) DEG C, and the test mineralization degree is increased from 19334mg/L to 32868 mg/L. Specific results are shown in table 1.
TABLE 1 Performance test results for various examples/comparative examples
Name (R) Solid content% Median diameter μm after swelling Elastic modulus (5000mg/L) Pa of aqueous dispersion Viscosity (5000mg/L) of aqueous dispersion mPa.s Content of network structure%
JX-1 92.5 765[1]/732[2] 51.6[3]/30.6[4] 187.2[5]/83.4[6] 69.2[7]/60.1[8]
JX-2 93.2 773[1]/741[2] 52.2[3]/31.1[4] 196.5[5]/86.2[6] 65.7[7]/58.3[8]
JX-3 91.7 766[1]/735[2] 53.5[3]/31.6[4] 205.3[5]/90.4[6] 67.4[7]/58.9[8]
JX-4 94.1 784[1]/752[2] 56.1[3]/32.8[4] 216.5[5]/91.6[6] 75.5[7]/62.4[8]
JX-5 90.9 761[1]/727[2] 54.7[3]/31.8[4] 187.8[5]/83.5[6] 66.9[7]/58.5[8]
JX-6 92.5 756[1]/723[2] 50.7[1]/28.9[2] 22.4[5]/9.3[6] 81.3[7]/72.0[8]
JX-7 89.3 752[1]/717[2] 51.2[1]/30.3[2] 21.8[5]/9.7[6] 84.0[7]/73.8[8]
JX-8 91.3 657[1]/625[2] 23.1[1]/11.2[2] 35.4[5]/15.2[6] 42.5[7]/34.6[8]
JX-9 90.1 662[1]/629[2] 25.8[1]/12.5[2] 46.7[5]/21.8[6] 48.7[7]/40.5[8]
Note: [1] the measurement results of the particle size median value after swelling in 6.6 of the technical requirement Q/SH 102023742020 on viscoelastic particle oil displacement agent under room temperature and mineralization degree of 19334 mg/L;
[2] in the product performance measuring method, the median value of the particle size after 3 swelling is measured under the conditions of room temperature and the mineralization degree of 32868 mg/L;
[3] the determination result of the elastic modulus test condition of 6.7.2 water dispersion system in the technical requirement Q/SH 102023742020 of viscoelastic particle oil displacement agent at 25 ℃ and the mineralization degree of 19334 mg/L;
[4] in the product performance measuring method, the 4-water dispersion system elastic modulus test condition is 35 ℃, and the measurement result is under the mineralization degree of 32868 mg/L;
[5] 6.8.2 in the technical requirement Q/SH 102023742020 on viscocity test condition of a water dispersion system of 6.8.2, and a measurement result under the condition of the mineralization degree of 19334 mg/L;
[6] in the product performance measuring method, the viscosity test condition of a 5 water dispersion system is 90 ℃, and the measurement result is under the mineralization degree of 32868 mg/L;
[7] the test condition of 6.5 network structure content in the technical requirement Q/SH 102023742020 on the viscoelastic particle oil displacement agent is 90 ℃, and the result is measured under the mineralization degree of 19334 mg/L;
[8] in the product performance measuring method, the 2-network structure content is measured under the conditions of 90 ℃ and the mineralization degree of 32868 mg/L;
as can be seen from the above table, when the product performance is tested according to the technical requirements specified by the product performance measuring method, the technical indexes JX-1, JX-2, JX-3, JX-4 and JX-5 are obviously higher than the technical requirements specified by the existing standards, and the product performance is also measured under the conditions of increasing the testing temperature and testing the mineralization degree. Different from example 1, the reaction raw materials AM and AA in comparative example 1 are added in the same order, and the reaction raw material AM in the first step in the comparative example reacts with AMPS to generate free radical with large steric hindrance and limited movement capacity, so that the AA is difficult to sufficiently initiate further reaction, the reaction conversion rate is low, the length of a branched chain at the tail end of a polymer network is limited, and the viscosity of the JX-6 aqueous dispersion system is low. In comparative example 2, the two-step reaction in example 3 is changed into one-step reaction to directly generate a polymer, the reaction speed is difficult to control, and implosion is easy to occur. In addition, AM does not take part in the polymerization reaction as a raw material, so that the terminal branch of a network structure is short and few, and the two factors act together to cause the low viscosity of the JX-7 aqueous dispersion system. Initiation System of comparative example 4 from [ Hmim ] in example 5]3[PMo12O40]Becomes [ Hmim ]]4[Mo8O26]On one hand, the active points of free radicals are relatively less, and the adjacent carbon of each hydroxyl group of the polyhydric alcohol is difficult to be fully excited to initiate free radical polymerization to form a branched chain and a cross-link; on the other hand, since the structure controllability is relatively weak, it is difficult to sufficiently pass the central atom and the coordinating atom through such a regulation actionThe purpose of various oxidizability and reducibility is achieved by changing. The two factors act together to greatly reduce the median of the particle size after the JX-9 is swelled, the elastic modulus of the water dispersion system, the viscosity of the water dispersion system and the content of the network structure. The initiation system of comparative example 3 consisted of [ Dhmim ] in example 4]3[AsMo12O40]Becomes [ Dhmim ]] ReO4The free radical active sites are fewer, and the self structure has no adjustability, so that the particle size median value after JX-8 swelling, the elastic modulus of the water dispersion system, the viscosity of the water dispersion system and the content of network structures are lower. Therefore, the final performance of the product provided by the invention can be fully exerted only under the formula and the component proportion set by the invention.

Claims (8)

1. The preparation method of the temperature-resistant salt-resistant viscoelastic particle oil displacement agent is characterized by comprising the following steps of:
adding deionized water and acrylic acid into a reaction kettle, adding 2-acrylamide-2-methylpropanesulfonic acid into a reaction system after the deionized water and the acrylic acid are completely dissolved, keeping the reaction system at 10-15 ℃, and stirring the mixture until the mixture is fully and uniformly mixed;
adding a cross-linking agent N, N-dimethylacrylamide into the reaction system, fully and uniformly mixing, adjusting the pH value in the reaction kettle under the protection of nitrogen, slowly adding a molybdenum polyoxometallate-polyol initiation system into the reaction system, sealing the reaction kettle, and reacting for 3-4 hours to initiate the prepolymerization of the aqueous solution;
after the prepolymerization reaction is finished, adding the prepolymerization product into acrylamide, and continuing to react for 2-3 h at the final reaction temperature of 40 +/-1 ℃;
introducing steam into a steam heater of the reaction kettle to raise the temperature, raising the temperature of colloid in the kettle to 75-80 ℃ for hydrolysis reaction for 4-6 h, taking out a polymerization sample after the reaction is finished, grinding and granulating, drying and screening to obtain a temperature-resistant salt-resistant viscoelastic particle oil displacement agent;
the multi-metal heteropolyacid salt of molybdenum in the initiation system: the mass ratio of the polyhydric alcohol is (0.05-0.1): 1, and the initiating system accounts for 0.1-0.3% of the total mass of the reaction system;
poly-gold of molybdenum in the initiating systemThe heteropolyacid salt is selected from [ Bmim ]]3[SiMo12O40]、[Hmim]3[SiMo12O40]、[Dhmim]3[SiMo12O40]At least one of (1).
2. The preparation method according to claim 1, wherein the mass ratio of the added acrylic acid, 2-acrylamide-2-methylpropanesulfonic acid, acrylamide and deionized water is (0.1-0.3): (0.01-0.05): (0.15-0.5): 1.
3. the preparation method of claim 1, wherein the mass of the added crosslinking agent N, N-dimethylacrylamide is 1% -3% of the total mass of the reaction system.
4. The preparation method according to claim 1, wherein the pH in the reaction kettle is adjusted to 8-10.
5. The method according to claim 1, wherein the polyol in the initiation system is at least one selected from the group consisting of ethylene glycol, glycerol, and pentaerythritol.
6. The temperature-resistant salt-tolerant viscoelastic particle oil displacement agent prepared by the preparation method according to any one of claims 1 to 5.
7. The application of the temperature-resistant salt-tolerant viscoelastic particle oil displacement agent according to claim 6 in oilfield exploitation at the temperature of less than or equal to 90 ℃ and the mineralization degree of less than or equal to 32868 mg/L.
8. The use according to claim 7, wherein the elastic modulus of the aqueous dispersion is greater than or equal to 41.6Pa at a temperature of 35 ℃ and a degree of mineralization of 32868 mg/L; under room temperature and mineralization degree of 32868mg/L, the median of the particle size after swelling is more than or equal to 761 μm; at the high temperature of 90 ℃ and the mineralization degree of 32868mg/L, the content of the network structure is more than or equal to 65.7 percent, and the viscosity of the water dispersion system is more than or equal to 157.2 mPa.s.
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