CN110872505B - Organic porous nano-particle/surfactant composite oil displacement system and preparation method thereof - Google Patents
Organic porous nano-particle/surfactant composite oil displacement system and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an organic porous nanoparticle/surfactant complex oil displacement system and a preparation method thereof, wherein the complex oil displacement system comprises organic porous nanoparticles and a surfactant, and the preparation method comprises the following steps: uniformly dissolving a surfactant in water to form a surfactant solution; and adding organic porous nano particles into the surfactant solution according to the proportion, and then performing ultrasonic dispersion to obtain the organic porous nano particle/surfactant composite oil displacement system. The preparation method is simple and low in cost; through the interaction of the organic porous nanoparticles and the surfactant, two effects of reducing the adsorption loss of the surfactant and enhancing the oil displacement effect of the surfactant can be realized simultaneously; in addition, the compound oil displacement system has good temperature and salt resistance, can be used as an oil displacement agent to improve the crude oil recovery rate in the oil field environment under the conditions of wide mineralization degree from low mineralization degree to high mineralization degree and wide temperature from low temperature to high temperature, and has wide application prospect.
Description
Technical Field
The invention relates to the technical field of oilfield chemistry in the technology of improving the recovery ratio of crude oil, in particular to an organic porous nanoparticle/surfactant composite oil displacement system and a preparation method thereof.
Background
The crude oil recovery ratio of most oil fields in China after water injection development is generally not more than 40%, and most crude oil still remains in the stratum and is not developed. In order to further improve the crude oil recovery efficiency and realize the yield increase and the stable yield of old oil fields, the chemical flooding technology is widely applied in China and obtains better industrial application effect. The surfactant flooding technology is an important chemical flooding technology, and can realize the remarkable improvement of the crude oil recovery rate by reducing the oil-water interfacial tension, improving the rock surface wettability, emulsifying oil and water and other action mechanisms.
However, in industrial application, the surfactant flooding usually has the defects of large dosage, high cost and the like, and greatly limits the further popularization and application of the technology. One of the main reasons for the high surfactant displacement and cost is the loss of surfactant adsorption to the formation rock. The surfactant molecules can be adsorbed on the rock surface of the near-wellbore zone through various physical force effects such as charge force, van der waals force, hydrogen bond and the like, so that the surfactant amount which can enter the deep part of the stratum to react with crude oil is greatly reduced, and the adsorption loss of the part greatly increases the dosage of the surfactant and the corresponding use cost.
Currently, injection of a sacrificial agent into a formation is the most dominant means of reducing surfactant adsorption loss, and the sacrificial agent may preferentially adsorb on the formation rock surfaces, thereby reducing surfactant adsorption loss on the rock. Chinese patent CN104073231A discloses a sacrificial agent consisting of a biological compound and sodium phosphate, which can reduce the adsorption quantity of surfactant sodium alkyl benzene sulfonate on rocks by 30-50%. Chinese patent CN109403932A discloses an oil displacement method for reducing adsorption loss, the sacrificial agent adopted in the method is at least one of a small molecular compound containing carboxyl, a polymer with the molecular weight of 1000-500000 and an alkaline compound, and the sacrificial agent can reduce the adsorption capacity of a surfactant in an oil displacement fluid by 30-70%.
However, the injection amount of the sacrificial agent is usually large, and the sacrificial agent does not have an obvious surfactant synergistic oil displacement effect, so the use cost of the sacrificial agent can still reduce the economy of surfactant flooding to a certain extent; in addition, the injection process of the sacrificial agent requires a long construction period, which also increases the operation cost of the project in the actual construction process.
Disclosure of Invention
In order to solve the problems, the invention aims to provide an organic porous nanoparticle/surfactant composite oil displacement system and a preparation method thereof, which reduce the adsorption loss of a surfactant and enhance the oil displacement effect of the surfactant through organic porous nanoparticles.
The technical scheme of the invention is as follows:
in one aspect, an organic porous nanoparticle/surfactant complex oil displacement system is provided, which comprises organic porous nanoparticles and a surfactant.
Preferably, the mass ratio of the organic porous nanoparticles to the surfactant is 1: 10-2: 1.
Preferably, the organic porous nanoparticles are prepared according to the following steps:
dropwise adding a mixed solution of styrene and divinylbenzene into deionized water dissolved with sodium dodecyl sulfate, stirring and emulsifying simultaneously, continuing to stir and emulsify for 0.5-1 hour after the dropwise addition of the mixed solution of styrene and divinylbenzene is completed, introducing nitrogen to remove oxygen for 15-30 minutes after the emulsification is completed, heating the emulsion to 75-80 ℃, adding a potassium persulfate aqueous solution to initiate a reaction for 8-18 hours, keeping stirring in the reaction process, adding ethanol or a demulsifier into the emulsion after the reaction is completed, performing centrifugal separation to obtain crosslinked polystyrene nano-microspheres, and then washing and drying for multiple times to obtain crosslinked polystyrene nano-microsphere dry powder;
dispersing the crosslinked polystyrene nano microsphere dry powder in 1, 2-dichloroethane to expand for 3-12 hours, sequentially adding formaldehyde-dimethyl acetal and anhydrous ferric trichloride, heating to 70-90 ℃ to react for 16-20 hours, cooling to room temperature after the reaction is finished, washing, purifying and drying to obtain the organic porous nano particles.
Preferably, the mass ratio of the styrene to the divinylbenzene is 9: 1-4.9: 1; the volume ratio of the mixed solution of styrene and divinylbenzene to the deionized water dissolved with sodium dodecyl sulfate is 1: 10-3: 10; the mass ratio of the sodium dodecyl sulfate to the mixed solution of styrene and divinylbenzene is 1: 100-1: 12.5; the mass ratio of the potassium persulfate to the mixed solution of styrene and divinylbenzene is 1: 100-1: 50.
Preferably, the mass ratio of the crosslinked polystyrene nano microsphere dry powder to formaldehyde glycol is 1: 0.8-1: 2.2, and the mass ratio of the crosslinked polystyrene nano microsphere dry powder to anhydrous ferric chloride is 1: 1.6-1: 9.
Preferably, the stirring speed in the emulsification process and the reaction process is 200-400 rpm.
Preferably, the crosslinked polystyrene nano-microspheres are washed by ethanol, and the product obtained by adding formaldehyde acetal and anhydrous ferric chloride and reacting is washed by methanol.
Preferably, after the formaldehyde acetal and the anhydrous ferric chloride are added, the temperature is firstly increased to 40-50 ℃ for reaction for 4-6 hours, and then the temperature is increased to 70-90 ℃ for reaction for 16-20 hours.
In another aspect, a method for preparing any one of the organic porous nanoparticle/surfactant complex oil displacement systems comprises the following steps:
uniformly dissolving a surfactant in water to form a surfactant solution;
and adding organic porous nano particles into the surfactant solution according to the proportion, and then performing ultrasonic dispersion to obtain the organic porous nano particle/surfactant composite oil displacement system.
Preferably, the ultrasonic dispersion time is 0.5-1 h.
The action mechanism of the invention is as follows:
the composite oil displacement system comprises organic porous nano particles and a surfactant, wherein surfactant molecules can act in pores of the organic porous nano particles through a physical force taking a hydrophobic effect as a main part to generate adsorption, and the organic porous nano particles can greatly reduce the adsorption of the surfactant molecules on the surface of rock because the interaction of the physical force between the surfactant molecules and the organic porous nano particles is larger than that between the surfactant molecules and the surface of the rock; when the composite oil displacement system contacts crude oil, the physical force interaction between the surfactant molecules and the organic porous nano particles is smaller than the interaction between the surfactant molecules and the crude oil, and the surfactant is desorbed from the organic porous nano particles and then is adsorbed to an oil-water interface, so that the 'intelligent' release of the surfactant molecules is realized, and the adsorption loss of the surfactant on rocks is effectively reduced. When the molecules of the surfactant are desorbed from the organic porous nanoparticles, the hydrophobic property of the organic porous nanoparticles is gradually enhanced, and the organic porous nanoparticles are gradually aggregated among the particles, so that the blocking effect on the roar of rock is generated, the liquid flow diversion effect can be generated, the sweep efficiency of the surfactant is improved, and the composite oil displacement system can simultaneously realize two effects of reducing the adsorption loss of the surfactant and enhancing the oil displacement effect of the surfactant.
Compared with the prior art, the invention has the following advantages:
the composite oil displacement system has the advantages of simple preparation method, wide raw material source and low cost, and can simultaneously realize two effects of reducing the adsorption loss of the surfactant and enhancing the oil displacement effect of the surfactant. After being compounded with the surfactant, the organic porous nano particles can be uniformly dispersed in water, and the compound oil displacement system is easy to pump; compared with the conventional inorganic hydrophobic nanoparticles, the organic porous nanoparticles have a deformable and breakable skeleton structure, and cannot block stratum pores to cause reservoir damage after aggregation; the compound oil displacement system has good temperature and salt resistance, and can be used as an oil displacement agent in an oil field environment under the conditions of wide mineralization degree from low mineralization degree to high mineralization degree and wide temperature from low temperature to high temperature to improve the crude oil recovery rate.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a microscopic morphology of the organic porous nanoparticles of example 1;
FIG. 2 is a performance diagram of enhanced oil recovery of the organic porous nanoparticle/surfactant complex flooding system of the present invention.
Detailed Description
The invention is further illustrated with reference to the following figures and examples. It should be noted that, in the present application, the embodiments and the technical features of the embodiments may be combined with each other without conflict.
On one hand, the invention provides an organic porous nanoparticle/surfactant composite oil displacement system which comprises organic porous nanoparticles and a surfactant, wherein the mass ratio of the organic porous nanoparticles to the surfactant is 1: 10-2: 1.
Optionally, the surfactant is any one of an anionic surfactant, a nonionic surfactant, an anionic-nonionic surfactant, and an amphoteric surfactant.
In a specific embodiment, the organic porous nanoparticles are prepared according to the following steps:
dropwise adding a mixed solution of styrene and divinylbenzene into deionized water dissolved with sodium dodecyl sulfate, stirring and emulsifying simultaneously, continuing to stir and emulsify for 0.5-1 hour after the dropwise addition of the mixed solution of styrene and divinylbenzene is completed, introducing nitrogen to remove oxygen for 15-30 minutes after the emulsification is completed, heating the emulsion to 75-80 ℃, adding a potassium persulfate aqueous solution to initiate a reaction for 8-18 hours, keeping stirring in the reaction process, adding ethanol or a demulsifier into the emulsion after the reaction is completed, demulsifying, centrifuging to obtain crosslinked polystyrene nano-microspheres, washing and drying for multiple times to obtain crosslinked polystyrene nano-microsphere dry powder, wherein the mass ratio of styrene to divinylbenzene is 9: 1-4.9: 1; the volume ratio of the mixed solution of styrene and divinylbenzene to the deionized water dissolved with sodium dodecyl sulfate is 1: 10-3: 10; the mass ratio of the sodium dodecyl sulfate to the mixed solution of styrene and divinylbenzene is 1: 100-1: 12.5; the mass ratio of the potassium persulfate to the mixed solution of styrene and divinylbenzene is 1: 100-1: 50.
Dispersing the crosslinked polystyrene nano microsphere dry powder in 1, 2-dichloroethane to expand for 3-12 hours, sequentially adding formaldehyde acetal and anhydrous ferric trichloride, heating to 70-90 ℃ to react for 16-20 hours, cooling to room temperature after the reaction is finished, washing, purifying and drying to obtain the organic porous nano particles, wherein the mass ratio of the crosslinked polystyrene nano microsphere dry powder to formaldehyde acetal diol is 1: 0.8-1: 2.2, and the mass ratio of the crosslinked polystyrene nano microsphere dry powder to the anhydrous ferric trichloride is 1: 1.6-1: 9.
In the preparation process, the stirring speed in the emulsification process and the reaction process is 200-400 r/min.
Optionally, the crosslinked polystyrene nano-microspheres are washed by ethanol, and the product obtained by adding formaldehyde acetal and anhydrous ferric chloride and reacting is washed by methanol.
In another specific embodiment, different from the above embodiments, after adding formaldehyde diethylene glycol and anhydrous ferric trichloride, heating to 40-50 ℃ for reaction for 4-6 hours, and then heating to 70-90 ℃ for reaction for 16-20 hours, the hypercrosslinking effect can be improved to a small extent, and the formed porous nanoparticles have a slightly higher pore volume and specific surface area, which is helpful for enhancing the capability of reducing the adsorption loss of the surfactant.
In another aspect, the invention further provides a method for preparing any one of the organic porous nanoparticle/surfactant composite oil displacement systems, which comprises the following steps:
uniformly dissolving a surfactant in water to form a surfactant solution;
and adding organic porous nano particles into the surfactant solution according to the proportion, and then performing ultrasonic dispersion to obtain the organic porous nano particle/surfactant composite oil displacement system.
In a specific embodiment, the ultrasonic dispersion time is 0.5-1 h.
Example 1
Dropwise adding a mixed solution of 10g of styrene and 0.5g of divinylbenzene into 100g of deionized water in which 0.2g of sodium dodecyl sulfate is dissolved, stirring and emulsifying at the speed of 300 revolutions per minute, continuously stirring and emulsifying for 1 hour after the dropwise addition of the mixed solution of styrene and divinylbenzene is completed, introducing nitrogen to remove oxygen for 15 minutes after the emulsification is completed, heating the emulsion to 80 ℃, adding 5g of potassium persulfate aqueous solution to initiate a reaction, wherein the mass concentration of the potassium persulfate aqueous solution is 3%, the stirring speed is kept at 300 revolutions per minute during the reaction process, and the reaction is completed after 8 hours. And adding ethanol into the reacted emulsion for demulsification, then centrifugally separating the crosslinked polystyrene nano-microspheres, washing the crosslinked polystyrene nano-microspheres for multiple times by using ethanol, and drying to obtain a crosslinked polystyrene nano-microsphere dry powder product.
Dispersing 2.5g of crosslinked polystyrene nano microsphere dry powder in 100mL of 1, 2-dichloroethane for expansion for 6 hours, then adding 3.7g of formaldehyde-dimethyl acetal and 8.6g of anhydrous ferric chloride into the 1, 2-dichloroethane suspension of the crosslinked polystyrene nano particles, heating the mixed system to 45 ℃ for reaction for 6 hours, and then heating to 80 ℃ again for reaction for 18 hours. And after the reaction is finished, cooling to room temperature, washing and purifying the product by using methanol, and drying the product to obtain the organic porous nano-particles. The microscopic morphology of the organic porous nanoparticles is shown in fig. 1, and as can be seen from fig. 1, the organic porous nanoparticles are in a regular spherical shape, and the particle size is in the nanometer level. Performing a nitrogen adsorption test on the organic porous nanoparticles to obtain the BET surface area of 926m2/g。
And adding 0.8g of the organic porous nano particles into 1000g of an alcohol ether carboxylate aqueous solution with the mass concentration of 0.2%, stirring and dispersing uniformly, wherein the mineralization degree of the alcohol ether carboxylate aqueous solution is 8000mg/L, and thus obtaining the organic porous nano particle/surfactant composite oil displacement system.
Example 2
Dropwise adding a mixed solution of 8g of styrene and 0.2g of divinylbenzene into 100g of deionized water in which 0.24g of sodium dodecyl sulfate is dissolved, stirring and emulsifying at the speed of 350 r/min, continuously stirring and emulsifying for 1 hour after the dropwise addition of the mixed solution of styrene and divinylbenzene is completed, introducing nitrogen to remove oxygen for 15 minutes after the emulsification is completed, heating the emulsion to 80 ℃, adding an aqueous solution in which 3.3g of potassium persulfate is added to initiate a reaction, wherein the mass concentration of the aqueous solution of potassium persulfate is 3%, the stirring speed is kept at 350 r/min during the reaction, and the reaction is completed after 8 hours. And adding ethanol into the reacted emulsion for demulsification, then centrifugally separating the crosslinked polystyrene nano-microspheres, washing the crosslinked polystyrene nano-microspheres for multiple times by using ethanol, and drying to obtain a crosslinked polystyrene nano-microsphere dry powder product.
3g of crosslinked polystyrene nano microsphere dry powder is dispersed in 120mL of 1, 2-dichloroethane to be expanded for 6 hours, then 6.5g of formaldehyde-dimethyl acetal and 14g of anhydrous ferric chloride are sequentially added into the 1, 2-dichloroethane suspension of the crosslinked polystyrene nano particles, the mixed system is heated to 45 ℃ to react for 6 hours, and then the temperature is raised to 80 ℃ again to react for 18 hours. And after the reaction is finished, cooling to room temperature, washing and purifying the product by using methanol, and drying the product to obtain the organic porous nano-particles.
Adding 1g of organic porous nano particles into 1000g of petroleum sulfonate aqueous solution with the mass concentration of 0.3%, stirring and dispersing uniformly, wherein the mineralization degree of the petroleum sulfonate aqueous solution is 3000mg/L, and thus obtaining the organic porous nano particle/surfactant composite oil displacement system.
Example 3
The organic porous nanoparticle/surfactant complex oil displacement system prepared in example 1 and a 0.2% alcohol ether carboxylate aqueous solution were used to perform a sand-pack pipe displacement experiment under the same conditions, wherein the sand-pack model in the displacement experiment had an inner diameter of 25mm, a length of 500mm, a porosity of about 30%, and a permeability of about 0.8 μm2The temperature condition is room temperature, the displacement speed is 0.2mL/min, the dynamic adsorption capacity of the surfactant is calculated according to the change of the concentration of the alcohol ether carboxylate in the core produced liquid, the change of the concentration of the alcohol ether carboxylate is measured by adopting an ultraviolet spectrophotometer, and the comparison experiment result shows that compared with a 0.2% alcohol ether carboxylate aqueous solution, the dynamic adsorption capacity of the surfactant of the organic porous nano particle/surfactant composite oil displacement system is reduced by 91.6%, and is far higher than the surfactant adsorption capacity reduced by adopting a sacrificial agent in the prior art.
Example 4
The organic porous nanoparticle/surfactant composite oil displacement system prepared in example 2 and a 0.3% petroleum sulfonate aqueous solution are adopted to respectively perform a sand-packed pipe displacement experiment under the same conditions, wherein the inner diameter of a sand-packed model in the displacement experiment is 25mm, and the length of the sand-packed model is 25mm500mm, a porosity of about 30% and a permeability of about 0.8 μm2The temperature condition is room temperature, the displacement speed is 0.2mL/min, the dynamic adsorption capacity of the surfactant is calculated according to the change of the concentration of the petroleum sulfonate in the core produced fluid, the change of the concentration of the petroleum sulfonate is measured by adopting an ultraviolet spectrophotometer, and the comparison experiment result shows that compared with a 0.3% petroleum sulfonate aqueous solution, the dynamic adsorption capacity of the surfactant of the organic porous nano particle/surfactant composite oil displacement system is reduced by 85.3%, and is far higher than the adsorption capacity of the surfactant reduced by adopting a sacrificial agent in the prior art.
Example 5
The organic porous nanoparticle/surfactant composite flooding system prepared in example 1 was subjected to a single core displacement experiment in which the core diameter was 38mm, the length was 78mm, the porosity was 20.6%, and the permeability was 0.328 μm2The viscosity of crude oil is 28.3 mPa.s, the initial oil saturation is 68%, the experimental temperature is 60 ℃, the displacement speed is 0.2mL/min, after water is driven to reach 98% of water content, the organic porous nanoparticle/surfactant composite oil displacement system prepared in 0.3PV example 1 is injected, then the subsequent water drive is continuously carried out until the water content reaches 98% again, the crude oil recovery efficiency in the whole crude oil recovery process is as shown in figure 2, and as can be seen from figure 2, the crude oil recovery efficiency is improved by 22.3% after the composite oil displacement system and the subsequent water drive, and the organic porous nanoparticle/surfactant composite oil displacement system has a good effect of improving the crude oil recovery efficiency.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (9)
1. An organic porous nanoparticle/surfactant complex oil displacement system is characterized by comprising organic porous nanoparticles and a surfactant, wherein the organic porous nanoparticles are prepared according to the following steps:
dropwise adding a mixed solution of styrene and divinylbenzene into deionized water dissolved with sodium dodecyl sulfate, stirring and emulsifying simultaneously, continuing to stir and emulsify for 0.5-1 hour after the dropwise addition of the mixed solution of styrene and divinylbenzene is completed, introducing nitrogen to remove oxygen for 15-30 minutes after the emulsification is completed, heating the emulsion to 75-80 ℃, adding a potassium persulfate aqueous solution to initiate a reaction for 8-18 hours, keeping stirring in the reaction process, adding ethanol or a demulsifier into the emulsion after the reaction is completed, performing centrifugal separation to obtain crosslinked polystyrene nano-microspheres, and then washing and drying for multiple times to obtain crosslinked polystyrene nano-microsphere dry powder;
dispersing the crosslinked polystyrene nano microsphere dry powder in 1, 2-dichloroethane to expand for 3-12 hours, sequentially adding formaldehyde-dimethyl acetal and anhydrous ferric trichloride, heating to 70-90 ℃ to react for 16-20 hours, cooling to room temperature after the reaction is finished, washing, purifying and drying to obtain the organic porous nano particles.
2. The organic porous nanoparticle/surfactant complex oil displacement system of claim 1, wherein the mass ratio of the organic porous nanoparticles to the surfactant is 1: 10-2: 1.
3. The organic porous nanoparticle/surfactant complex oil displacement system of claim 1, wherein the mass ratio of styrene to divinylbenzene is 9:1 to 4.9: 1; the volume ratio of the mixed solution of styrene and divinylbenzene to the deionized water dissolved with sodium dodecyl sulfate is 1: 10-3: 10; the mass ratio of the sodium dodecyl sulfate to the mixed solution of styrene and divinylbenzene is 1: 100-1: 12.5; the mass ratio of the potassium persulfate to the mixed solution of styrene and divinylbenzene is 1: 100-1: 50.
4. The organic porous nanoparticle/surfactant complex oil displacement system of claim 1, wherein the mass ratio of the crosslinked polystyrene nanosphere dry powder to formaldehyde glycol is 1: 0.8-1: 2.2, and the mass ratio of the crosslinked polystyrene nanosphere dry powder to anhydrous ferric chloride is 1: 1.6-1: 9.
5. The organic porous nanoparticle/surfactant complex oil displacement system of claim 1, wherein the stirring rate in the emulsification process and the reaction process is 200-400 rpm.
6. The organic porous nanoparticle/surfactant complex oil displacement system of claim 1, wherein the crosslinked polystyrene nanospheres are washed with ethanol, and the product obtained by adding formaldehyde acetal and anhydrous ferric chloride and reacting is washed with methanol.
7. The organic porous nanoparticle/surfactant complex oil displacement system of claim 1, wherein after the formaldehyde acetal and the anhydrous ferric chloride are added, the temperature is raised to 40-50 ℃ for reaction for 4-6 hours, and then the temperature is raised to 70-90 ℃ for reaction for 16-20 hours.
8. A method for preparing the organic porous nanoparticle/surfactant complex oil displacement system of any one of claims 1-7, which comprises the following steps:
uniformly dissolving a surfactant in water to form a surfactant solution;
and adding organic porous nano particles into the surfactant solution according to the proportion, and then performing ultrasonic dispersion to obtain the organic porous nano particle/surfactant composite oil displacement system.
9. The method for preparing the organic porous nanoparticle/surfactant complex oil displacing system according to claim 8, wherein the ultrasonic dispersion time is 0.5-1 h.
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