CN106590599B - A kind of nano combined nucleocapsid particles oil displacement agent and its preparation method and application - Google Patents
A kind of nano combined nucleocapsid particles oil displacement agent and its preparation method and application Download PDFInfo
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- 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
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Abstract
The present invention provides a kind of nano combined nucleocapsid particles oil displacement agent and its preparation method and application.The preparation method of nano combined nucleocapsid particles oil displacement agent of the invention includes the following steps: 1) to mix acrylamide monomer with deionized water, crosslinking agent is then added, and stirring obtains acrylamide aqueous phase system；2) emulsifier is mixed with organic solvent, with the phyllosilicate of back loading oil displacement surfactant, stirring obtains oil-based system；3) under protective atmosphere and stirring, the oil-based system is slowly added into the acrylamide aqueous phase system, the subsequent initiator that is added carries out polymerization reaction, and after reaction, demulsification, filtering, drying obtain nano combined nucleocapsid particles oil displacement agent.Nano combined nucleocapsid particles oil displacement agent of the invention can form ultralow interfacial tension with crude oil, and the recovery ratio of petroleum is not only greatly improved, furthermore is not easy to be adsorbed in oil displacement process, elute, the loss of surfactant is low, advantageously reduces cost for oil production.
Description
Technical field
The invention belongs to technical field of petroleum extraction, and in particular to a kind of nano combined nucleocapsid particles oil displacement agent and its preparation
Methods and applications.
Background technique
Oil exploitation is generally divided into primary oil recovery and secondary oil recovery.Primary oil recovery is to make oily spray using oil field pressure itself
Out, 20% of original oil in place or so can be produced.As strata pressure reduces, the decline of primary oil recovery yield can adopt at this time
With secondary oil recovery, i.e., is filled the water to stratum and improve pressure to improve oil production, secondary oil recovery can further produce 20% left side of reserves
It is right.It is above-mentioned routine oil recovery technique overall recovery efficiency be only 40% or so, and 60% or so crude oil still residually under.
Currently, the large oilfields such as China's grand celebration, triumph, Central Plains, North China and huge port have entered the water flooding recovery middle and later periods, it is more
Number produced liquid in oil well moisture content is up to 90%.On the other hand, China's oil consumption average growth rate per annum is up to 17% or more, country's hair
Exhibition and reform committee's research report show that the year two thousand twenty China's oil demand will be at 4.5 hundred million -6.1 hundred million tons, and importation dependence will
Up to 60%-70%.
Tertiary oil recovery or intensified oil reduction (Enhanced Oil recovery, EOR) technology be after secondary oil recovery again
Mining novel technology.Tertiary oil recovery technology further increases recovery ratio using technologies such as physics, chemistry and biologies, and reduces residual oil
Saturation degree.Tertiary oil recovery technology includes chemical flooding, gas drive, heating power drive and microorganism drive etc.；Wherein, chemical flooding passes through injection chemistry
Agent improves recovery ratio, including polymer flooding, surfactant flooding, caustic waterflooding and ternary composite driving etc.；Gas drive include mixed phase or
CO2 drive, nitrogen flooding, natural gas drive and flue gas flooding of part mixed phase etc.；It includes steam drive, steam soak, hot water flooding that heating power, which drives,
With combustion in situ etc.；Microbe oil production includes microbial profile control or microbial oil displacement etc..
Surfactant flooding can make interfacial tension reach lower value, therefore can increase substantially the recovery ratio of petroleum.
However, surfactant usage amount is big, and adsorption loss is big in the earth formation, to improve cost for oil production, economic benefit is low.
Summary of the invention
The present invention provides a kind of nano combined nucleocapsid particles oil displacement agent and its preparation method and application, which can be with
Crude oil forms ultralow interfacial tension, so that the recovery ratio of petroleum be greatly improved；In addition, the oil displacement agent in oil displacement process not
It is easily adsorbed, elutes, the loss of surfactant is low, to advantageously reduce cost for oil production.
The first aspect of the present invention provides a kind of preparation method of phyllosilicate for loading oil displacement surfactant, including
Following steps:
Phyllosilicate is mixed with water, forms swelling system；
Intercalator is added into the swelling system, is reacted under stiring, then to the displacement of reservoir oil is added in reaction system
Surfactant, the reaction was continued；
After reaction, it is demulsified, filters, is dry, obtaining the phyllosilicate of load oil displacement surfactant.
Oil displacement surfactant is supported in phyllosilicate by the present invention, utilizes the stratiform of load oil displacement surfactant
Silicate can generate removing dispersion and form removing lamella when preparing polymer, which can generate in the polymer
Nucleation is conducive to the thermo-salt resistance for improving polymer to form core-shell structure；In addition, the removing lamella is surface height
Active nanoparticle, can strong adsorption surfactant to crude oil formed ultralow interfacial tension, increase substantially
The recovery ratio of petroleum, and the removing lamella be able to suppress surfactant in displacement process by duct and adsorption by clay,
Elution, to advantageously reduce the loss of surfactant.
It is 2-4nm it is possible to further control the interlamellar spacing of the phyllosilicate of the load oil displacement surfactant.Tool
There is the phyllosilicate of the interlamellar spacing range to be easy to generate removing dispersion when preparing polymer and form removing lamella, and then shape
At the polymer with core-shell structure.
In the present invention, right as long as can make the phyllosilicate for loading oil displacement surfactant that there is above-mentioned interlamellar spacing
Preparation method is without stringent limitation.Specifically, the mass ratio that can control layered silicate and water is 1:(10-30)；Institute
The additional amount for stating intercalator and oil displacement surfactant can be the 5-20% of layered silicate quality；The reaction can be with
It is carried out under conditions of 70-80 DEG C, 30-35Hz, the reaction time can be 6-10h；It is described that the reaction was continued that the time can be 4-6h.
It is easy to make the interlamellar spacing 2-4nm of the phyllosilicate of load oil displacement surfactant obtained under the above conditions.
The present invention does not limit the specific type of used phyllosilicate, intercalator and oil displacement surfactant strictly
System, can reasonably select according to actual needs.For example, layered silicate can select it is conventional have layered crystal structure and
The silicates mineral of sheet crystal form can specifically be selected from montmorillonite, hydrotalcite, kaolin, attapulgite, sepiolite, silicon ash
One of stone, chlorite and stratiform silica are a variety of；The intercalator is used to form intercalation system, specifically can be with
Selected from one of cetyl trimethylammonium bromide, hexadecyltrimethylammonium chloride and dodecyl sodium sulfate or a variety of；
The oil displacement surfactant can be selected from 3- sulfopropyl Cetyl dimethyl betaine, petroleum sodium sulfonate and detergent alkylate
One of sodium sulfonate is a variety of.
In the present invention, the demulsifier progress of this field routine can be used in described be demulsified, and demulsifier for example can be anhydrous
Ethyl alcohol, acetone etc.；Further, after the drying, the phyllosilicate of load oil displacement surfactant can also be ground,
Screening, to obtain the laminar silicic acid salt powder of load oil displacement surfactant.
The present invention also provides a kind of load oil displacement surfactants being prepared using any of the above-described preparation method
Phyllosilicate.Further, the interlamellar spacing of the phyllosilicate of the load oil displacement surfactant is 2-4nm.
Another aspect of the present invention provides a kind of preparation method of nano combined nucleocapsid particles oil displacement agent, including walks as follows
It is rapid:
1) acrylamide monomer is mixed with deionized water, crosslinking agent is then added, stirred, obtain acrylamide water phase body
System；
2) emulsifier is mixed with organic solvent, the load displacement of reservoir oil by any of the above-described preparation method preparation is then added
The phyllosilicate of surfactant, stirring, obtains oil-based system；
3) under protective atmosphere and stirring, the oil-based system is slowly added into the acrylamide aqueous phase system,
Initiator is then added and carries out polymerization reaction, after reaction, demulsification filters, is dry, obtains the nano combined nucleocapsid particles displacement of reservoir oil
Agent.
The present invention by acrylamide aqueous phase system with containing above-mentioned load oil displacement surfactant phyllosilicate oil
In-situ polymerization synthetic high polymer oil displacement agent is utilized under the conditions of phase system is existing for the initiator；Wherein, oil-displacement surface is loaded
The phyllosilicate of activating agent reacts to form high polymer nano complex nucleus with the aggregated intercalation synthesis of crystal type acrylamide monomer
Shell particle, the phyllosilicate for loading oil displacement surfactant can be achieved evenly dispersed in polyacrylamide matrix, be conducive to
Improve oil displacement efficiency；In addition, the nano combined nucleocapsid particles oil displacement agent can inhibit surfactant in displacement process by duct
With adsorption by clay, elution, to reduce the loss of surfactant, displacement of reservoir oil cost is reduced.
Specifically, in step 1), the mass ratio that can control the acrylamide monomer and deionized water is 1:(1.5-
3)；The additional amount of the crosslinking agent can be the 0.5-3.5% of acrylamide monomer quality；The frequency of the stirring can be
30-35Hz, mixing time can be 30min or more；The crosslinking agent can be diethylenetriamines or N, N- di-2-ethylhexylphosphine oxide third
Acrylamide.
Further, in step 2), the mass ratio that can control the emulsifier and organic solvent is 1:(60-80)；Institute
The additional amount for stating the phyllosilicate of load oil displacement surfactant can be the 1-5% of acrylamide monomer quality；It is described to stir
The frequency mixed can be 30-35Hz, and mixing time is 30min or more；The emulsifier can selected from OP 2, TX 10, OP 10,
One of polysorbas20, polysorbate60, Tween 80, AEO 3, SP 20, SP 60, SP 80, T 152 and T 154 or a variety of；It is described
Organic solvent can be hexamethylene etc..Further, it is also possible to substitute the organic solvent using diesel oil or aviation kerosine to prepare oil
Phase system.
Further, in step 3), the frequency that can control the stirring is 40-60Hz；The additional amount of the initiator
It can be the 0.5-5% of acrylamide monomer quality；The initiator can be selected from ammonium persulfate, potassium peroxydisulfate, bisulfite
One of sodium, sodium sulfite, azodiisobutyronitrile and benzoyl peroxide are a variety of.
In the present invention, the polymerization reaction requires to implement in oxygen-free environment, can be by elder generation into polymerization reaction kettle
It introduces inert gas and forms oxygen-free environment, nitrogen etc. can be used in inert gas；Specifically, can first continue logical to polymerization reaction kettle
Enter nitrogen 10-20min, to remove the air in polymerization reaction kettle, the nitrogen gas purity used can be 98.99-99.99%, pressure
It can be 20-30m that power, which can be 0.50-0.55MPa, flow,3/h。
In addition, the oil-based system is slowly added into the acrylamide aqueous phase system in step 3), can be formed steady
Fixed anti-phase suspension liquid system；When polymerization reaction generates high polymer nano compound nucleocapsid particles, there are a heatings for reaction system
Process, reaction temperature system temperature after rising to maximum temperature can remain stable.Specifically, initiator is added and carries out polymerization reaction
Afterwards, reaction a period of time, the temperature of reaction system can be risen, no longer be risen after system temperature is raised to peak, at this time
Isothermal holding can be carried out to reaction system, soaking time can be 2-3h, and isothermal holding is beneficial to prevent system temperature reduction, from
And it is more conducive to complete polymerization reaction.
Further, the temperature of the drying can control at 60-70 DEG C, and ± 5 DEG C of fluctuation may be present；In addition, also
Nano combined nucleocapsid particles oil displacement agent can be ground, be sieved, such as cross 200 meshes, to obtain nano combined nucleocapsid
Particle oil displacement agent powder, average grain diameter can be controlled in 10-20 μm.
In the present invention, various reagents can pass through common commercially available acquisition.
The present invention also provides a kind of nano combined nucleocapsid particles oil displacement agents, according to any of the above-described preparation method system
?.
Interfacial tension between nano combined nucleocapsid particles oil displacement agent of the invention and crude oil is 10-2The mN/m order of magnitude is left
The right side, concretely 9 × 10-3mN/m-7×10-2MN/m, which can form ultralow interfacial tension with crude oil, thus favorably
In the recovery ratio for increasing substantially petroleum；Continue in particular, the nano combined nucleocapsid particles oil displacement agent has in displacement process
Stability, can still be maintained 10 with the interfacial tension of crude oil after displacement-2MN/m order of magnitude or so, concretely 3 ×
10-2mN/m-9×10-2Thus mN/m illustrates that the nano combined nucleocapsid particles oil displacement agent is able to maintain surface in oil displacement process
Activating agent does not lose or less loss, to advantageously reduce displacement of reservoir oil cost.
The present invention also provides application of the above-mentioned nano combined nucleocapsid particles oil displacement agent in oil exploitation.Specifically, this is received
Meter Fu He nucleocapsid particle oil displacement agent can be used in tertiary oil recovery or intensified oil reduction.
The present invention also provides a kind of oil production methods, after water drive, are carried out using above-mentioned nano combined nucleocapsid particles oil displacement agent
The displacement of reservoir oil.
Implementation of the invention, at least has the advantage that
1, removing dispersion can be generated when the phyllosilicate of load oil displacement surfactant of the invention prepares polymer
And removing lamella is formed, which can generate nucleation in the polymer to form core-shell structure, be conducive to mention
The thermo-salt resistance of high polymer.
2, the interfacial tension between nano combined nucleocapsid particles oil displacement agent and crude oil of the invention is 10-2The mN/m order of magnitude,
Oil recovery can be increased substantially；In addition, the nano combined nucleocapsid particles oil displacement agent can inhibit surfactant in displacement
In the process by duct and adsorption by clay, elution, to advantageously reduce the loss of surfactant, displacement of reservoir oil cost is reduced.
3, nano combined nucleocapsid particles oil displacement agent of the invention can carry out the displacement of reservoir oil in neutral conditions, in the displacement of reservoir oil
Seal-off effect is good, high to the oil displacement efficiency of petroleum, and the increase rate of oil recovery especially can be used for multiple up to 20% or more
The oil recovery of miscellaneous reservoir, can protect the permeability, lasting effect and high efficiency of reservoir, and strong applicability has wide range of applications.
Detailed description of the invention
Fig. 1 is the X ray diffracting spectrum of each material of a, b, c, d, in which: a is the montmorillonite raw material of embodiment 1；B is to implement
The phyllosilicate of load oil displacement surfactant prepared by example 1；C is polyacrylamide microsphere oil displacement agent prepared by comparative example 1；
D is nano combined nucleocapsid particles oil displacement agent prepared by embodiment 7；
Fig. 2 is the infared spectrum of each material of a, b, c, d, in which: a is the montmorillonite raw material of embodiment 1；B is the system of embodiment 1
The phyllosilicate of standby load oil displacement surfactant；C is polyacrylamide microsphere oil displacement agent prepared by comparative example 1；D is real
Apply the nano combined nucleocapsid particles oil displacement agent of the preparation of example 7；
Fig. 3 is the grain size distribution of the oil displacement agent of embodiment 7 and comparative example 1；
Fig. 4 is the scanning electron microscope (SEM) photograph of nano combined nucleocapsid particles oil displacement agent prepared by embodiment 7；
Fig. 5 is the transmission electron microscope picture of nano combined nucleocapsid particles oil displacement agent prepared by embodiment 7.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with attached drawing of the invention and implementation
Example, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is the present invention
A part of the embodiment, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not having
Every other embodiment obtained under the premise of creative work is made, shall fall within the protection scope of the present invention.
Embodiment 1 loads the preparation of the phyllosilicate of oil displacement surfactant
A. montmorillonite is mixed with water by mass parts 1:20 in a kettle, stirs 30min at room temperature, form swelling
System；
B. above-mentioned swelling system is warming up to 80 DEG C, 20% cetyl trimethyl bromine is added in the quality based on montmorillonite
Change ammonium, sets stirring unit frequency as 30Hz, be stirred to react 6h；
C. based on the quality of montmorillonite, 20% 3- sulfopropyl etradecyldimethylamine is added into above-mentioned gained reaction system
Base glycine betaine (industrial products), the reaction was continued 4h obtain the phyllosilicate slurries of load oil displacement surfactant；
D. above-mentioned slurries filtered, dried, be ground up, sieved, obtain the laminar silicic acid of load oil displacement surfactant
Salt powder, for use.
Small-angle diffraction measurement, Cu are carried out using sample of the German Bruker D8-Advance type X-ray diffractometer to preparation
Target KαRadiation, tube current 40mA, tube voltage 40kV, scanning speed are 0.1 °/s, and step width is 0.02 °, 2 θ of scanning range=
1.3-10°；Interlamellar spacing d001 is calculated according to Bragg formula.
2d sin θ=n λ
In above formula, λ is Cu KαThe wavelength (λ=0.154nm) of radiant light；D is the interplanar distance of diffraction (nm)；2 θ are
The angle of diffraction (°).
The result shows that: gained loads the laminated silicate interlayer of oil displacement surfactant away from for 2.27nm.
In addition, the X-ray of the phyllosilicate of montmorillonite raw material and the load oil displacement surfactant of above-mentioned preparation is spread out
It penetrates map and infared spectrum is shown in Fig. 1 and Fig. 2 respectively.
Embodiment 2 loads the preparation of the phyllosilicate of oil displacement surfactant
A. montmorillonite is mixed with water by mass parts 1:20 in a kettle, stirs 30min at room temperature, form swelling
System；
B. above-mentioned swelling system is warming up to 80 DEG C, 20% cetyl trimethyl chlorine is added in the quality based on montmorillonite
Change ammonium, sets stirring unit frequency as 30Hz, be stirred to react 6h；
C. based on the quality of montmorillonite, 20% 3- sulfopropyl etradecyldimethylamine is added into above-mentioned gained reaction system
Base glycine betaine (industrial products), the reaction was continued 4h obtain the phyllosilicate slurries of load oil displacement surfactant；
D. above-mentioned slurries filtered, dried, be ground up, sieved, obtain the laminar silicic acid of load oil displacement surfactant
Salt powder, for use.
Through detecting, gained loads the laminated silicate interlayer of oil displacement surfactant away from for 2.10nm.
Embodiment 3 loads the preparation of the phyllosilicate of oil displacement surfactant
A. kaolin is mixed with water by mass parts 1:20 in a kettle, stirs 30min at room temperature, form swelling
System；
B. above-mentioned swelling system is warming up to 80 DEG C, 20% cetyl trimethyl bromine is added based on kaolinic quality
Change ammonium, sets stirring unit frequency as 30Hz, be stirred to react 8h；
C. it is based on kaolinic quality, 20% 3- sulfopropyl etradecyldimethylamine is added into above-mentioned gained reaction system
Base glycine betaine (industrial products), the reaction was continued 6h obtain the phyllosilicate slurries of load oil displacement surfactant；
D. above-mentioned slurries filtered, dried, be ground up, sieved, obtain the laminar silicic acid of load oil displacement surfactant
Salt powder, for use.
Through detecting, gained loads the laminated silicate interlayer of oil displacement surfactant away from for 2.17nm.
Embodiment 4 loads the preparation of the phyllosilicate of oil displacement surfactant
A. stratiform silica is mixed with water by mass parts 1:30 in a kettle, stirs 30min, shape at room temperature
At swelling system；
B. above-mentioned swelling system is warming up to 80 DEG C, 20% cetyl three is added in the quality based on stratiform silica
Ammonio methacrylate sets stirring unit frequency as 30Hz, is stirred to react 6h；
C. 20% 3- sulfopropyl hexadecane is added into above-mentioned gained reaction system for the quality based on stratiform silica
Base dimethyl betaine (industrial products), the reaction was continued 4h obtain the phyllosilicate slurries of load oil displacement surfactant；
D. above-mentioned slurries filtered, dried, be ground up, sieved, obtain the laminar silicic acid of load oil displacement surfactant
Salt powder, for use.
Through detecting, gained loads the laminated silicate interlayer of oil displacement surfactant away from for 2.07nm.
Embodiment 5 loads the preparation of the phyllosilicate of oil displacement surfactant
A. montmorillonite is mixed with water by mass parts 1:20 in a kettle, stirs 30min at room temperature, form swelling
System；
B. above-mentioned swelling system is warming up to 80 DEG C, 20% cetyl trimethyl bromine is added in the quality based on montmorillonite
Change ammonium, sets stirring unit frequency as 30Hz, be stirred to react 8h；
C. based on the quality of montmorillonite, 10% 3- sulfopropyl etradecyldimethylamine is added into above-mentioned gained reaction system
Base glycine betaine (industrial products), the reaction was continued 6h obtain the phyllosilicate slurries of load oil displacement surfactant；
D. above-mentioned slurries filtered, dried, be ground up, sieved, obtain the laminar silicic acid of load oil displacement surfactant
Salt powder, for use.
Through detecting, gained loads the laminated silicate interlayer of oil displacement surfactant away from for 2.13nm.
Embodiment 6 loads the preparation of the phyllosilicate of oil displacement surfactant
A. montmorillonite is mixed with water by mass parts 1:20 in a kettle, stirs 30min at room temperature, form swelling
System；
B. above-mentioned swelling system is warming up to 80 DEG C, 10% cetyl trimethyl chlorine is added in the quality based on montmorillonite
Change ammonium, sets stirring unit frequency as 30Hz, be stirred to react 6h；
C. based on the quality of montmorillonite, 10% 3- sulfopropyl etradecyldimethylamine is added into above-mentioned gained reaction system
Base glycine betaine (industrial products), the reaction was continued 4h obtain the phyllosilicate slurries of load oil displacement surfactant；
D. above-mentioned slurries filtered, dried, be ground up, sieved, obtain the laminar silicic acid of load oil displacement surfactant
Salt powder, for use.
Through detecting, gained loads the laminated silicate interlayer of oil displacement surfactant away from for 1.85nm.
The preparation of the nano combined nucleocapsid particles oil displacement agent of embodiment 7
A. the ratio of acrylamide monomer and deionized water 1:2 in mass ratio are mixed, the matter based on acrylamide monomer
0.5% crosslinking agent diethylenetriamines is added in amount, and the frequency for controlling stirring is 30Hz, stirs 30min or more, forms acryloyl
Aqueous amine phase system；
B. polyoxyethylene nonylphenol ether 2 is mixed with the organic solvent ratio of 1:60 in mass ratio, the quality based on acrylamide monomer
The phyllosilicate for loading oil displacement surfactant prepared by 1% embodiment 1 is added, is stirred under being 30Hz in stirring frequency
30min or more forms oil-based system；
C. above-mentioned acrylamide aqueous phase system is transferred to polymerization reaction kettle, under nitrogen atmosphere, control stirring frequency is
Oil-based system is slowly dropped in acrylamide aqueous phase system by 40Hz, anti-phase suspension liquid is formed, based on acrylamide monomer
The initiator ammonium persulfate that quality is added 0.5% carries out polymerization reaction, when temperature of reaction system no longer increases in reaction process, protects
Temperature maintains 3h, obtains nano combined nucleocapsid particles system；
D. above-mentioned nano combined nucleocapsid particles system be demulsified, filtered, is dry, be ground up, sieved, obtaining nano combined nucleocapsid
Particle oil displacement agent.
The yield of the nano combined nucleocapsid particles oil displacement agent of gained is shown in table 1；X ray diffracting spectrum, infared spectrum are shown in respectively
Fig. 1 to Fig. 2, particle diameter distribution are shown in that Fig. 3, scanning electron microscope (SEM) photograph (SEM figure) and transmission electron microscope picture (TEM figure) are shown in Fig. 4 to Fig. 5；Average grain
Diameter result is shown in table 1.
As shown in Figure 1, the X-ray diffraction curve of the nano combined nucleocapsid particles oil displacement agent of gained is a smooth curve,
Strong diffraction maximum do not occur, be indicated above: the montmorillonite for loading oil displacement surfactant is removed well, polymer chain insertion
To the interlayer of montmorillonite.
As shown in Figure 2, the nano combined nucleocapsid particles oil displacement agent of gained is in 3630cm-1There is absorption peak, it is corresponding to be
Al-OH and Si-OH key absorption peak in montmorillonite illustrates de- containing the illiteracy after load in nano combined nucleocapsid particles oil displacement agent
Soil.
As shown in Figure 4, the pattern of the nano combined nucleocapsid particles oil displacement agent of gained is spheroidal, and sphericity is high, while
Intergranular soilless sticking phenomenon.
There are many black lines for representing montmorillonite layer in the nano combined nucleocapsid particles oil displacement agent of Fig. 5 display gained,
And there is free Distribution Phenomena in these black lines majorities, the montmorillonite for being indicated above load oil displacement surfactant is poly- in preparation
Removing dispersion can be generated when closing object and forms removing lamella, which generates nucleation in the polymer to be formed
Core-shell structure.
In addition, rotating drop ultralow interfacial tension instrument using XZD-5 type, the nano combined nucleocapsid particles displacement of reservoir oil agent solution is measured
With crude oil interfacial tension, it the results are shown in Table 2.
The preparation of the nano combined nucleocapsid particles oil displacement agent of embodiment 8
A. the ratio of acrylamide monomer and deionized water 1:2 in mass ratio are mixed, the matter based on acrylamide monomer
2% crosslinking agent N, N- methylene-bisacrylamide is added in amount, and control stirring frequency is 30Hz, stirs 30min or more, forms third
Acrylamide aqueous phase system；
B. emulsifier tween 20 is mixed with the organic solvent ratio of 1:60 in mass ratio, the matter based on acrylamide monomer
The phyllosilicate of load oil displacement surfactant prepared by the embodiment 2 that amount is added 1%, is stirred at stirring frequency 30Hz
30min or more forms oil-based system；
C. above-mentioned acrylamide aqueous phase system is transferred to polymerization reaction kettle, under nitrogen atmosphere, control stirring frequency is
Oil-based system is slowly dropped in acrylamide aqueous phase system by 40Hz, anti-phase suspension liquid is formed, based on acrylamide monomer
The initiator potassium persulfate that quality is added 1.0% carries out polymerization reaction, when temperature of reaction system no longer increases in reaction process, protects
Temperature maintains 2-3h, obtains nano combined nucleocapsid particles system；
D. above-mentioned nano combined nucleocapsid particles system be demulsified, filtered, is dry, be ground up, sieved, obtaining nano combined nucleocapsid
Particle oil displacement agent；Its yield and average grain diameter the results are shown in Table 1, and interfacial tension the results are shown in Table 2.
The preparation of the nano combined nucleocapsid particles oil displacement agent of embodiment 9
A. the ratio of acrylamide monomer and deionized water 1:2 in mass ratio are mixed, the matter based on acrylamide monomer
2% crosslinking agent diethylenetriamines is added in amount, and control stirring frequency is 30Hz, stirs 30min or more, forms acryloyl aqueous amine
Phase system；
B. emulsifier SP 20 is mixed with the organic solvent ratio of 1:60 in mass ratio, the matter based on acrylamide monomer
The phyllosilicate of load oil displacement surfactant prepared by the embodiment 3 that amount is added 3% is stirred in the case where stirring frequency is 30Hz
30min or more forms oil-based system；
C. above-mentioned acrylamide aqueous phase system is transferred to polymerization reaction kettle, under nitrogen atmosphere, control stirring frequency is
Oil-based system is slowly dropped in acrylamide aqueous phase system by 40Hz, anti-phase suspension liquid is formed, based on acrylamide monomer
The initiator benzoyl peroxide that quality is added 1.0% carries out polymerization reaction, when temperature of reaction system no longer rises in reaction process
Height, heat preservation maintain 3h, obtain nano combined nucleocapsid particles system；
D. above-mentioned nano combined nucleocapsid particles system be demulsified, filtered, is dry, be ground up, sieved, obtaining nano combined nucleocapsid
Particle oil displacement agent；Its yield and average grain diameter the results are shown in Table 1, and interfacial tension the results are shown in Table 2.
The preparation of the nano combined nucleocapsid particles oil displacement agent of embodiment 10
A. the ratio of acrylamide monomer and deionized water 1:2 in mass ratio are mixed, the matter based on acrylamide monomer
2% crosslinking agent diethylenetriamines is added in amount, and control stirring frequency is 30Hz, stirs 30min or more, forms acryloyl aqueous amine
Phase system；
B. emulsifier T 152 is mixed with the organic solvent ratio of 1:60 in mass ratio, the matter based on acrylamide monomer
The phyllosilicate of load oil displacement surfactant prepared by the embodiment 4 that amount is added 5% is stirred in the case where stirring frequency is 30Hz
30min or more becomes oil-based system；
C. above-mentioned acrylamide aqueous phase system is transferred to polymerization reaction kettle, under nitrogen atmosphere, control stirring frequency is
Oil-based system is slowly dropped in acrylamide aqueous phase system by 40Hz, anti-phase suspension liquid is formed, based on acrylamide monomer
The initiator sodium hydrogensulfite that quality is added 2.0% carries out polymerization reaction, when temperature of reaction system no longer increases in reaction process,
Heat preservation maintains 3h, obtains nano combined nucleocapsid particles system；
D. above-mentioned nano combined nucleocapsid particles system be demulsified, filtered, is dry, be ground up, sieved, obtaining nano combined nucleocapsid
Particle oil displacement agent；Its yield and average grain diameter the results are shown in Table 1, and interfacial tension the results are shown in Table 2.
The preparation of the nano combined nucleocapsid particles oil displacement agent of embodiment 11
A. the ratio of acrylamide monomer and deionized water 1:2 in mass ratio are mixed, the matter based on acrylamide monomer
3% crosslinking agent N, N- methylene-bisacrylamide is added in amount, and control stirring frequency is 30Hz, stirs 30min or more, forms third
Acrylamide aqueous phase system；
B. emulsifier TX 10 is mixed with the organic solvent ratio of 1:60 in mass ratio, the matter based on acrylamide monomer
The phyllosilicate of load oil displacement surfactant prepared by the embodiment 5 that amount is added 5% is stirred in the case where stirring frequency is 30Hz
30min or more forms oil-based system；
C. above-mentioned acrylamide aqueous phase system is transferred to polymerization reaction kettle, under nitrogen atmosphere, control stirring frequency is
Oil-based system is slowly dropped in acrylamide aqueous phase system by 40Hz, anti-phase suspension liquid is formed, based on acrylamide monomer
The initiator sodium sulfite that quality is added 2.5% carries out polymerization reaction, when temperature of reaction system no longer increases in reaction process, protects
Temperature maintains 3h, obtains nano combined nucleocapsid particles system；
D. above-mentioned nano combined nucleocapsid particles system be demulsified, filtered, is dry, be ground up, sieved, obtaining nano combined nucleocapsid
Particle oil displacement agent；Its yield and average grain diameter the results are shown in Table 1, and interfacial tension the results are shown in Table 2.
The preparation of the nano combined nucleocapsid particles oil displacement agent of embodiment 12
A. the ratio of acrylamide monomer and deionized water 1:2 in mass ratio are mixed, the matter based on acrylamide monomer
0.5% crosslinking agent diethylenetriamines is added in amount, and the frequency for controlling stirring is 30Hz, stirs 30min or more, forms acryloyl
Aqueous amine phase system；
B. polyoxyethylene nonylphenol ether 2 is mixed with the organic solvent ratio of 1:60 in mass ratio, the quality based on acrylamide monomer
The phyllosilicate for loading oil displacement surfactant prepared by 1% embodiment 6 is added, is stirred under being 30Hz in stirring frequency
30min or more forms oil-based system；
C. above-mentioned acrylamide aqueous phase system is transferred to polymerization reaction kettle, under nitrogen atmosphere, control stirring frequency is
Oil-based system is slowly dropped in acrylamide aqueous phase system by 40Hz, anti-phase suspension liquid is formed, based on acrylamide monomer
The initiator ammonium persulfate that quality is added 0.5% carries out polymerization reaction, when temperature of reaction system no longer increases in reaction process, protects
Temperature maintains 3h, obtains nano combined nucleocapsid particles system；
D. above-mentioned nano combined nucleocapsid particles system be demulsified, filtered, is dry, be ground up, sieved, obtaining nano combined nucleocapsid
Particle oil displacement agent；Its yield and average grain diameter the results are shown in Table 1, and interfacial tension the results are shown in Table 2.
The preparation of 1 polyacrylamide microsphere oil displacement agent of comparative example
A. the ratio of acrylamide monomer and deionized water 1:2 in mass ratio are mixed, the matter based on acrylamide monomer
2% crosslinking agent diethylenetriamines is added in amount, and the frequency for controlling stirring is 30Hz, stirs 30min or more, forms acrylamide
Aqueous phase system；
B. polyoxyethylene nonylphenol ether 2 is mixed with the organic solvent ratio of 1:60 in mass ratio, is stirred in the case where stirring frequency is 30Hz
30min or more forms oil-based system；
C. above-mentioned acrylamide aqueous phase system is transferred to polymerization reaction kettle, under nitrogen atmosphere, control stirring frequency is
Oil-based system is slowly dropped in acrylamide aqueous phase system by 40Hz, anti-phase suspension liquid is formed, based on acrylamide monomer
The initiator ammonium persulfate that quality is added 1.0% carries out polymerization reaction, when temperature of reaction system no longer increases in reaction process, protects
Temperature maintains 3h, obtains polyacrylamide microsphere system；
D. above-mentioned polyacrylamide microsphere system be demulsified, filtered, is dry, be ground up, sieved, obtaining polyacrylamide microsphere
Oil displacement agent；Its X ray diffracting spectrum and infared spectrum are shown in Fig. 1 and Fig. 2 respectively, and particle diameter distribution is shown in Fig. 3；In addition, average grain diameter knot
Fruit is shown in table 1, and interfacial tension the results are shown in Table 2.
The yield and average grain diameter of each oil displacement agent of table 1
| Nano combined nucleocapsid particles oil displacement agent | Average grain diameter (μm) | Yield (%) |
| Embodiment 7 | 12.05 | 90.53 |
| Embodiment 8 | 10.58 | 98.24 |
| Embodiment 9 | 15.36 | 93.56 |
| Embodiment 10 | 20.57 | 93.47 |
| Embodiment 11 | 21.56 | 91.25 |
| Embodiment 12 | 24.89 | 90.33 |
Table 1 the result shows that:
The yield of the nano combined nucleocapsid particles oil displacement agent of various embodiments of the present invention reaches 90% or more, and average grain diameter exists
In the range of 10-25 μm.
The interfacial tension of each oil displacement agent of table 2
Table 2 the result shows that:
1, the interfacial tension between the nano combined nucleocapsid particles oil displacement agent and crude oil of various embodiments of the present invention is 10-2mN/m
Order of magnitude or so, which can form ultralow interfacial tension with crude oil, to be conducive to increase substantially the harvesting of petroleum
Rate；In particular, the nano combined nucleocapsid particles oil displacement agent in displacement process have lasting stability, after displacement with original
The interfacial tension of oil can still be maintained 10-2Thus mN/m order of magnitude or so illustrates that the nano combined nucleocapsid particles oil displacement agent exists
It is able to maintain surfactant in oil displacement process not lose or less loss, to advantageously reduce displacement of reservoir oil cost.
2, in addition, when controlling the interlamellar spacing for loading the phyllosilicate of oil displacement surfactant for 2-4nm, relative to
Interlamellar spacing is less than 2nm, can obtain the nano combined nucleocapsid particles oil displacement agent with more low interfacial tension, more conducively oil recovery
The raising of rate and the reduction of displacement of reservoir oil cost.
3, the interfacial tension relatively, between the polyacrylamide microsphere oil displacement agent and crude oil of comparative example 1 is relatively large,
The usage amount of meeting enlarged surface activating agent；In addition, the polyacrylamide microsphere oil displacement agent is significantly reduced in displacement rear surface tension,
Illustrate that its adsorption loss in the earth formation is big, to improve cost for oil production, economic benefit is low.
Test example 1 blocks test
7 blocks of rock cores are taken, number 1-7 injects nano combined nucleocapsid prepared by above-described embodiment 7-12 to rock core 1-7 respectively
Polyacrylamide microsphere oil displacement agent prepared by grain oil displacement agent and comparative example 1 carries out closure test；The permeability of each rock core is measured,
And sealing ratiod is calculated, it as a result see the table below 3.
The sealing ratiod of each oil displacement agent of table 3
As seen from the results in Table 3:
Relative to the polyacrylamide microsphere oil displacement agent of comparative example 1, using the nano combined nucleocapsid of various embodiments of the present invention
When particle oil displacement agent carries out the displacement of reservoir oil, the permeability of reservoir can be preferably protected, plugging effect is good, and sealing ratiod is high, strong applicability,
The oil recovery that especially can be used for complicated reservoirs, has wide range of applications.
2 displacement of reservoir oil of test example test
7 blocks of rock cores are taken, number 8-14 injects crude oil to rock core 8-14 respectively.
Firstly, clear water displacement is used to the rock core 8-14 of injection crude oil respectively, by the Mass Calculation water drive for displacing crude oil
Efficiency；Then, on the basis of water drive, be respectively adopted above-described embodiment 7-12 preparation nano combined nucleocapsid particles oil displacement agent with
And polyacrylamide microsphere oil displacement agent prepared by comparative example 1 carries out displacement, each oil displacement agent pair of Mass Calculation by displacing crude oil
The oil displacement efficiency of respective rock core, the results are shown in Table 4.
The oil displacement efficiency of each oil displacement agent of table 4
As seen from the results in Table 4:
Relative to the polyacrylamide microsphere oil displacement agent of comparative example 1, the nano combined nucleocapsid particles of various embodiments of the present invention
Oil displacement agent is high to the oil displacement efficiency of petroleum, and the increase rate of oil recovery is up to 20% or more, to advantageously reduce oil recovery
Cost.
Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations；To the greatest extent
Pipe present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: its according to
So be possible to modify the technical solutions described in the foregoing embodiments, or to some or all of the technical features into
Row equivalent replacement；And these are modified or replaceed, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution
The range of scheme.
Claims (9)
1. a kind of preparation method of nano combined nucleocapsid particles oil displacement agent, which comprises the steps of:
1) acrylamide monomer is mixed with deionized water, crosslinking agent is then added, stirred, obtain acrylamide aqueous phase system；
2) emulsifier is mixed with organic solvent, the phyllosilicate of load oil displacement surfactant is then added, stirring obtains
Oil-based system；
Wherein, the phyllosilicate of the load oil displacement surfactant is prepared as follows:
I) phyllosilicate is mixed with water, form swelling system；
II) into the swelling system intercalator is added, it is reacted under stiring, then to displacement of reservoir oil table is added in reaction system
Face activating agent, the reaction was continued；
III) after reaction, demulsification, filtering, drying obtain the phyllosilicate of load oil displacement surfactant；
3) under protective atmosphere and stirring, the oil-based system is slowly added into the acrylamide aqueous phase system, then
Initiator is added and carries out polymerization reaction, after reaction, demulsification, filtering, drying obtain nano combined nucleocapsid particles oil displacement agent.
2. preparation method according to claim 1, which is characterized in that the laminar silicic acid of the load oil displacement surfactant
The interlamellar spacing of salt is 2-4nm.
3. preparation method according to claim 1, which is characterized in that the mass ratio for controlling layered silicate and water is
1:(10-30)；The additional amount of the intercalator and oil displacement surfactant is the 5-20% of layered silicate quality；It is described
Reaction carries out under conditions of 70-80 DEG C, 30-35Hz, reaction time 6-10h；The reaction was continued time is 4-6h.
4. preparation method according to claim 1 to 3, which is characterized in that layered silicate be selected from montmorillonite,
One of hydrotalcite, kaolin, attapulgite, sepiolite, wollastonite, chlorite and stratiform silica are a variety of；It is described
Intercalator be selected from one of cetyl trimethylammonium bromide, hexadecyltrimethylammonium chloride and dodecyl sodium sulfate or
It is a variety of；The oil displacement surfactant is selected from 3- sulfopropyl Cetyl dimethyl betaine, petroleum sodium sulfonate and dodecyl
One of benzene sulfonic acid sodium salt is a variety of.
5. preparation method according to claim 1-3, which is characterized in that in step 1), control the acryloyl
Amine monomers and the mass ratio of deionized water are 1:(1.5-3)；The additional amount of the crosslinking agent is acrylamide monomer quality
0.5-3.5%；The frequency of the stirring is 30-35Hz, and mixing time is 30min or more；The crosslinking agent is diethylidene three
Amine or N,N methylene bis acrylamide.
6. preparation method according to claim 1-3, which is characterized in that in step 2), control the emulsifier
Mass ratio with organic solvent is 1:(60-80)；The additional amount of the phyllosilicate of the load oil displacement surfactant is third
The 1-5% of acrylamide monomer mass；The frequency of the stirring is 30-35Hz, and mixing time is 30min or more；The emulsifier
Selected from OP 2, TX 10, OP 10, polysorbas20, polysorbate60, Tween 80, AEO 3, SP 20, SP 60, SP 80, T 152 and T
One of 154 or a variety of.
7. preparation method according to claim 1-3, which is characterized in that in step 3), control the stirring
Frequency is 40-60Hz；The additional amount of the initiator is the 0.5-5% of acrylamide monomer quality；The initiator was selected from
One of ammonium sulfate, potassium peroxydisulfate, sodium hydrogensulfite, sodium sulfite, azodiisobutyronitrile and benzoyl peroxide are a variety of.
8. a kind of nano combined nucleocapsid particles oil displacement agent, which is characterized in that according to preparation method as claimed in claim 1 to 7
It is made.
9. application of the nano combined nucleocapsid particles oil displacement agent according to any one of claims 8 in oil exploitation.
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