KR101872020B1 - Manufacturing method of silica nanofluid and enhanced oil recovery using the same - Google Patents
Manufacturing method of silica nanofluid and enhanced oil recovery using the same Download PDFInfo
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- KR101872020B1 KR101872020B1 KR1020180012174A KR20180012174A KR101872020B1 KR 101872020 B1 KR101872020 B1 KR 101872020B1 KR 1020180012174 A KR1020180012174 A KR 1020180012174A KR 20180012174 A KR20180012174 A KR 20180012174A KR 101872020 B1 KR101872020 B1 KR 101872020B1
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- C—CHEMISTRY; METALLURGY
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
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- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/28—Compounds of silicon
- C09C1/30—Silicic acid
- C09C1/3081—Treatment with organo-silicon compounds
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- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
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- C09K8/02—Well-drilling compositions
- C09K8/04—Aqueous well-drilling compositions
- C09K8/05—Aqueous well-drilling compositions containing inorganic compounds only, e.g. mixtures of clay and salt
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- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/62—Compositions for forming crevices or fractures
- C09K8/66—Compositions based on water or polar solvents
- C09K8/665—Compositions based on water or polar solvents containing inorganic compounds
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- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/84—Compositions based on water or polar solvents
- C09K8/845—Compositions based on water or polar solvents containing inorganic compounds
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- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/92—Compositions for stimulating production by acting on the underground formation characterised by their form or by the form of their components, e.g. encapsulated material
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- E—FIXED CONSTRUCTIONS
- E21—EARTH DRILLING; MINING
- E21B—EARTH DRILLING, e.g. DEEP DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
- E21B43/00—Methods or apparatus for obtaining oil, gas, water, soluble or meltable materials or a slurry of minerals from wells
- E21B43/25—Methods for stimulating production
Abstract
(A) dispersing silica sol in deionized water; (b) introducing a silane coupling agent and performing a silane reaction to modify the surface of the silica nanoparticles; (c) filtering and dialyzing the distilled water to obtain silica nanoparticles; And (d) dispersing the silica nanoparticles in saline.
Therefore, it is possible to increase the oil recovery by increasing the dispersion stability under the high salt condition of the large carbonate reservoir and by using it as the injection fluid of the oil recovery enhancement method.
Description
The present invention relates to a method for producing a surface-modified silica nanofluid and a method for enhancing the recovery of oil using the same.
The process of recovering crude oil from the oil field provides a primary recovery process of crude oil which is pumped through the well and natural pressure or a driving force that can flow the crude oil after the first recovery There is a second recovery process to recover crude oil.
After the first and second recovery processes, a considerable amount of crude oil remains in the dielectric layer, and an enhanced oil recovery (EOR) method is used to recover the crude oil. Particularly, some of the heavy crude oil is difficult to produce without using crude oil recovery promotion method.
Enhanced Oil Recovery (EOR) is a tertiary recovery process. After the second recovery process, surfactant is injected in order to further improve the recovery of crude oil. By doing so, crude oil trapped in the capillary It is a method of increasing the sweep efficiency of crude oil by increasing the viscosity of the water that is pulled out or injected with polymer to push the crude oil.
The global oil recovery (EOR) market is expected to expand from approximately US $ 22.9 billion in 2016 to US $ 30.4 billion by 2021 and a CAGR of 5.9%.
Polymer flooding, which is one of the methods to improve the recovery of crude oil, is a method of recovering crude oil by injecting polymer. It controls the mobility ratio between petroleum and water by injecting a highly viscous polymer aqueous solution into the reservoir It is possible to improve the recovery of oil by lowering the heterogeneity of the fluid permeability of the reservoir layer.
This is advantageous in that it can be applied to various dielectric materials at a low cost. However, since the injection rate of the polymer is low, high-pressure injection equipment is required. If the injection pressure is too high, cracks may occur in the injection gas. The polymer particles are finely crushed and the molecular weight of the polymer is lowered and the efficiency of the polymer injection method is lowered.
Particularly, there is a problem that it is difficult to use the pulimer injection method due to the characteristics of a large carbonate reservoir layer.
In the case of the carbonate reservoir layer, it shows lipophilicity and it is very difficult to recover the oil using water.
Therefore, it is very urgent to develop a new nanofluid that can be effectively used for the recovery of oil even under high temperature and high salt conditions of the carbonate reservoir.
Prior art related to this is disclosed in Korean Patent No. 1591426 (Publication Date: 2016.02.03), there are nanoparticles, a method for producing the same, and a petroleum enhanced recovery method using the same.
Accordingly, it is an object of the present invention to provide a silica nanofluid whose surface has been modified to improve dispersion stability even under high temperature and high salt conditions, and to provide a method for recovering oil in a carbonate reservoir.
The problems to be solved by the present invention are not limited to the above-mentioned problem (s), and another problem (s) not mentioned can be understood by those skilled in the art from the following description.
In order to solve the above-mentioned problems, the present invention provides a process for producing a silica sol comprising the steps of: (a) dispersing silica sol in deionized water; (b) introducing a silane coupling agent and performing a silane reaction to modify the surface of the silica nanoparticles; (c) filtering and dialyzing the distilled water to obtain silica nanoparticles; And (d) dispersing the silica nanoparticles in saline.
The silica sol may also be colloidal silica.
The silane coupling agent may also be (3-glycidyloxypropyl) trimethoxysilane.
The (3-glycidyloxypropyl) trimethoxysilane may be in a concentration of 0.05 to 5 mmol / g.
The silane reaction may be carried out at 65 to 75 ° C for 24 to 26 hours to attach a methoxy group to the silica nanoparticles.
The silica nanoparticles may also have an average particle size of from 35 to 55 nm.
The brine may also contain 5 to 20 wt% of salt.
The silica nanofluid also has a particle concentration of 0.05 to 3 wt%.
Also, the silica nanofluid can maintain the dispersion stability of the silica nanoparticles at a temperature of 25 to 90 ° C.
According to another aspect of the present invention, there is provided a method for enhancing oil recovery using a nanofluid, comprising: (i) identifying a carbonate reservoir layer and generating an injection reservoir in the carbonate reservoir; (ii) dispersing the silica sol in deionized water; (iii) introducing a silane coupling agent and performing a silane reaction to modify the surface of the silica nanoparticles; (iv) filtering and dialyzing the distilled water to obtain silica nanoparticles; (v) dispersing the silica nanoparticles in a water layer to produce a silica nanofluid; And (vi) injecting silica nanofluid into the spaces between the rocks through the injection well to recover petroleum in the rock.
Further, in the step (ii), the silane coupling agent may be (3-glycidyloxypropyl) trimethoxysilane at a concentration of 0.05 to 5 mmol / g (3-glycidyloxypropyl) trimethoxysilane.
Also, in the step (iii), the silane reaction may be carried out at 65 to 75 ° C for 24 to 26 hours to attach silane to the silica nanoparticles.
Also, in the step (vi), the silica nanofluid has a particle concentration of 0.5 to 2 wt% and can increase the hydrophilicity of the carbonate reservoir layer.
Also, in the step (v), the silica nanofluid produced may maintain the dispersion stability of the silica nanoparticles at a temperature of 25 to 90 ° C.
According to the present invention, the surface of silica nanoparticles can be modified to produce silica nanoparticles having structural stability, and nanofluids containing the same can be prepared.
Silica nanoparticles can be modified by confirming the optimal silane reaction conditions in which the silica nanoparticles exhibit colloidal stability at high temperatures and high temperatures.
It is possible to provide a silane feed concentration capable of optimizing the stability of the silica nanoparticles particularly at high temperature.
The prepared nanofluid greatly increases the dispersion stability of the nanoparticles under the high salt condition, so that aggregation or precipitation does not occur even when the nanoparticles are added to the carbonate reservoir due to the accumulation of nanoparticles.
In addition, when the prepared silica nanofluid is injected into the pores of the carbonate reservoir, the hydrophilicity of the oil between the rocks increases and the efficiency of the oil recovery enhancement method can be greatly increased.
1 is a flow chart showing a process sequence of a method of manufacturing a silica nanofluid according to an embodiment of the present invention.
FIG. 2 is a flow chart showing a process sequence of a method for enhancing a petroleum recovery using a silica nanofluid according to another embodiment of the present invention.
3 is a graph showing the average particle size of the silica nanofluid according to the supply amount of the silane in the method of manufacturing the silica nanofluid according to the embodiment of the present invention.
FIG. 4 is a scanning electron microscope (SEM) image of silica nanoparticles according to a change in silane concentration in a method for producing a silica nanofluid according to an embodiment of the present invention.
FIG. 5 is a photograph showing the change of the prepared silica nanofluid with time according to the dispersion time in the production method of the silica nanofluid according to the embodiment of the present invention. FIG.
FIG. 6 is a graph showing the average particle size of the silica nanoparticles according to the salt concentration in the method of manufacturing the silica nanofluid according to the embodiment of the present invention.
FIG. 7 is a photograph showing changes in salt concentration and dispersion time of the produced silica nanofluid in the method for producing silica nanofluid according to an embodiment of the present invention. FIG.
FIG. 8 is a scanning electron microscope (SEM) image of silica nanoparticles according to a change in salinity of salt water in a method for producing silica nanofluid according to an embodiment of the present invention.
9 is a graph showing the average particle size of the silica nanoparticles according to the concentration of the silica nanoparticles in the method of manufacturing the silica nanofluid according to the embodiment of the present invention.
10 is a photograph showing changes in particle concentration and dispersion time of the produced silica nanofluid in the method for producing silica nanofluid according to an embodiment of the present invention.
11 is a scanning electron micrograph of the particle concentration of the prepared silica nanofluid in the method of producing a silica nanofluid according to an embodiment of the present invention.
FIG. 12 is a graph showing the contact angle according to the concentration of silica nanoparticles in a lime stone sample in a method for enhancing the recovery of oil using a silica nanofluid according to another embodiment of the present invention. FIG.
13 is a photograph showing a change in the contact angle according to the concentration of the silica nanoparticles relative to the lime stone sample in the oil recovery enhancement method using the silica nanofluid according to another embodiment of the present invention.
14 is a graph showing a contact angle according to the concentration of silica nanoparticles in a dolomite sample in a petroleum recovery enhancement method using a silica nanofluid according to another embodiment of the present invention.
FIG. 15 is a photograph showing the change in the contact angle according to the concentration of silica nanoparticles relative to the dolomite sample in the oil recovery enhancement method using the silica nanofluid according to another embodiment of the present invention. FIG.
Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS The advantages and features of the present invention and the manner of achieving it will become apparent with reference to the embodiments described in detail below with reference to the accompanying drawings.
The present invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art. To fully disclose the scope of the invention to those skilled in the art, and the invention is only defined by the scope of the claims.
In the following description, well-known functions or constructions are not described in detail since they would obscure the invention in unnecessary detail.
A method for preparing a silica nanofluid according to the present invention comprises the steps of: (a) dispersing silica sol in deionized water; (b) introducing a silane coupling agent and performing a silane reaction to modify the surface of the silica nanoparticles; (c) filtering and dialyzing the distilled water to obtain silica nanoparticles; And (d) dispersing the silica nanoparticles in saline.
1 is a flow chart showing a process sequence of a method of manufacturing a silica nanofluid according to an embodiment of the present invention.
Referring to FIG. 1, silica sol is dispersed in deionized water (S10).
The silica may be a means of SiO 2, and remedies typically colloidal silica (colloidal silica).
The silica has a powder form, in which silicon atoms and oxygen atoms form a siloxane bond (Si-O-Si), and the surface has a large number of OH groups.
The colloidal silica may be dispersed in deionized water to form a sol form.
In an organic solvent other than the deionized water, a problem may occur that the polymer is not dispersed depending on the polarity.
The surface of the silica nanoparticles is modified by introducing a silane coupling agent and performing a silane reaction (S20).
The silane coupling agent may be (3-glycidyloxypropyl) trimethoxysilane] (3-glycidyloxypropyl) trimethoxysilane.
The (3-glycidyloxypropyl) trimethoxysilane has a methoxy group as a reactor.
When the methoxy group is present, it may be chemically bonded to the inorganic material.
The inorganic material and the organic material can be combined through the silane coupling agent.
The (3-glycidyloxypropyl) trimethoxysilane may be in a concentration of 0.05 to 5 mmol / g.
The silica nanofluid can maintain its stability under the high concentration of saline under the above concentration range to prevent agglomeration between the nanoparticles and prevent agglomeration and precipitation of the silica nanoparticles.
The silane reaction is carried out at 65 to 75 ° C for 24 to 26 hours to graft silane on the surface of the silica nanoparticles.
The surface of the silica nanoparticles can be modified by attaching silane to the surface of the silica nanoparticles by hydrolysis of the silane at the above temperature and time range.
Surface modified silica nanoparticles have greatly increased structural stability under high salt conditions.
When a silane coupling agent is supplied at a concentration of 0.2 mmol / g at a room temperature of 25 ° C, a silane coupling agent is preferably added at a concentration of 1 to 0.5 mmol / g at 90 ° C under a high temperature condition since the stability of the silica nanoparticles can be optimized. The stability of the silica nanoparticles can be optimally maintained.
Filtered through distilled water and dialyzed to obtain silica nanoparticles (S30).
Through the dialysis, the unreacted (3-glycidyloxypropyl) trimethoxysilane can be removed.
The silica nanoparticles may have an average particle size of 35 to 55 nm.
The size of the silica nanoparticles is maintained in a colloidal form, and the particles can be homogeneously distributed.
The silica nanoparticles are dispersed in saline to produce a silica nanofluid (S40).
The salt water may contain 5 to 20 wt% of salt.
The salinity corresponds to the high saltiness condition of the carbonate reservoir, and the silica nanoparticles maintain the dispersion stability in the above range of saline water.
The silica nanofluid has a particle concentration of 0.05 to 3 wt%.
The surface-modified silica nanoparticles at the above particle concentration do not affect the dispersion stability in the nanofluid.
According to another aspect of the present invention, there is provided a method for enhancing oil recovery using a nanofluid, comprising: (i) identifying a carbonate reservoir layer and generating an injection reservoir in the carbonate reservoir; (ii) dispersing the silica sol in deionized water; (iii) introducing a silane coupling agent and performing a silane reaction to modify the surface of the silica nanoparticles; (iv) filtering and dialyzing the distilled water to obtain silica nanoparticles; (v) dispersing the silica nanoparticles in a water layer to produce a silica nanofluid; And (vi) injecting silica nanofluid into the spaces between the rocks through the injection well to recover petroleum in the rock.
FIG. 2 is a flow chart showing a process sequence of a method for enhancing a petroleum recovery using a silica nanofluid according to another embodiment of the present invention.
Referring to FIG. 2, a carbonate reservoir layer is identified and an injection tablet is formed in the rock of the carbonate reservoir (S100).
The carbonate reservoir may be at high salt and high temperature conditions.
It is difficult to maintain the dispersion stability of the silica nanoparticles when the carbonate reservoir is in a high salt and high temperature condition.
The silica sol is dispersed in deionized water (S200).
The colloidal silica can be prepared by dispersing silica using deionized water to form a sol.
In an organic solvent other than the deionized water, a problem may occur that the polymer is not dispersed depending on the polarity.
A silane coupling agent is added and a silane reaction is carried out to modify the surface of the silica nanoparticles (S300).
The silane coupling agent may be 0.05 to 5 mmol / g (3-glycidyloxypropyl) trimethoxysilane.
The (3-glycidyloxypropyl) trimethoxysilane has a methoxy group as a reactor.
The silica nanofluid can maintain its stability under the high concentration of saline under the above concentration range to prevent agglomeration between the nanoparticles and prevent agglomeration and precipitation of the silica nanoparticles.
The silane reaction is carried out at 65 to 75 ° C for 24 to 26 hours to attach silane to the silica nanoparticles.
The surface of the silica nanoparticles can be modified by attaching silane to the surface of the silica nanoparticles by hydrolysis of the silane at the above temperature and time range.
Filtered through distilled water and dialyzed to obtain silica nanoparticles (S400).
Unreacted (3-glycidyloxypropyl) trimethoxysilane can be removed through the dialysis.
The silica nanofluid is injected between the pores of the rock through the injection well to recover the oil in the rock (S500).
The silica nanofluid has a particle concentration of 0.05 to 3 wt% and can increase the hydrophilicity of the petroleum in the rock.
Therefore, the silica nanofluid contains solid colloidal particles as a dispersion medium, and when injected into the carbonate reservoir, the silica nanoparticles penetrate between the rock and the oil to reduce residual oil saturation and improve the wettability of the surface of the rock, It is possible to greatly increase the efficiency of oil recovery enhancement.
Hereinafter, the present invention will be described in more detail with reference to the following examples. However, the scope of the present invention is not limited to the following examples.
Example 1: Preparation of silica nanofluid
The silica sol (LUDOX® TMA colloidal silica 34 wt%, SIGMA-ALDRICH, USA), which is a dispersion medium composed of silicon dioxide (SiO 2 ), which is mainly used for improving the recovery of oil, was prepared for the preparation of silica nanofluid. (3-Glycidyloxypropyl) trimethoxysilane, SIGMA-ALDRICH, USA, which is a silane coupling agent; Hereinafter " GPTMS ") was used for surface modification.
The surface modification of the silica was carried out by mixing silica sol at a concentration of 0.05-5 mmol / g of GPTMS, reacting at 65-75 ° C for 24-26 hours and dialyzing in distilled water to remove residual GPTMS.
The surface - modified mixture was again dispersed in saline containing 5, 10, 15 and 20 wt% of salt (
Example 2: Utilizing the method of enhancing the recovery of oil
In order to apply the silica nanofluid of Example 1 to the method of enhancing the oil flow rate, a limestone sample and a dolomite sample were assumed to be carbonate reservoirs, respectively, and silica nanofluids were injected into each sample to confirm hydrophilicity.
Experimental Example 1: Evaluation of silica nanofluid dispersion stability
In order to confirm the dispersion stability of the silica nanofluid, the transparency and the amount of the precipitated silica nanofluid were confirmed.
The size of the nanoparticles was measured using a dynamic light scattering device, and the particle size of the silica nanofluid and the reaction analysis results of the silica nanoparticles were confirmed using a transmission electron microscope.
First, to confirm the dispersion stability of the silica nanofluid according to the changed silane concentration by the addition of the silane coupling agent, the concentration, temperature and dispersion time of the silane were varied as shown in Table 1 to confirm the particle size.
3 is a graph showing the average particle size of the silica nanofluid according to the supply amount of the silane in the method of manufacturing the silica nanofluid according to the embodiment of the present invention.
Referring to FIG. 3, it was confirmed that the stability of the nanofluid was increased when the silane concentration was increased to 0.2 mmol / g or more at a room temperature of 25 ° C.
Particularly, it was confirmed that the dispersion stability was maintained at a concentration of 1 mmol / g to 0.5 mmol / g at 90 ° C, which is a high temperature condition, and the supply amount of silane capable of maintaining dispersion stability even under high temperature conditions was confirmed.
FIG. 4 is a scanning electron microscope (SEM) image of silica nanoparticles according to a change in silane concentration in a method for producing a silica nanofluid according to an embodiment of the present invention.
Referring to FIG. 4, it was confirmed that the average size of the silica nanoparticles in the S1-25 sample (25 ° C., 0.05 mmol / g) was 1 μm or more, and the reaction with the silane was insufficient.
In addition, the average size of the silica nanoparticles was 42 nm in the S5-25 sample (25 ° C, 1 mmol / g), and it was confirmed that the dispersion stability was obtained because the particles were relatively homogeneously distributed.
FIG. 5 is a photograph showing the change of the prepared silica nanofluid with time according to the dispersion time in the production method of the silica nanofluid according to the embodiment of the present invention. FIG.
Referring to FIG. 5, (a) shows a photograph of the dispersion at room temperature of 25.degree. C. for 7 days, and (b) shows a photograph of dispersion at a high temperature of 90.degree. C. for 7 days.
When the concentration of silane was less than 0.2 mmol / g at 25 ° C, the silica nanoparticles remained agglomerated and opaque. However, it was confirmed that the dispersion stability was maintained at 0.2 mmol / g or more, Respectively.
When it was 0.5 mmol / g or more at a high temperature of 90 캜, the dispersion stability was maintained and it was confirmed that it was transparent.
It was confirmed that the stability of colloidal dispersion increases as the feed amount of silane increases.
In order to confirm the dispersion stability of the silica nanofluid according to the salt concentration, the concentration of the saline solution was changed as shown in Table 2 to confirm flocculation or sedimentation.
FIG. 6 is a graph showing the average particle size of the silica nanoparticles according to the salt concentration in the method of manufacturing the silica nanofluid according to the embodiment of the present invention.
Referring to FIG. 6, although the average particle size was increased with increasing salt concentration at 25 ° C, the dispersion stability was maintained, and no aggregation or precipitation of the nanofluid was observed. At 90 ° C, It was confirmed that the particle size greatly increased to 85 nm.
FIG. 7 is a photograph showing changes in salt concentration and dispersion time of the produced silica nanofluid in the method for producing silica nanofluid according to an embodiment of the present invention. FIG.
Referring to FIG. 7 (a), the dispersion stability was not changed according to the change of the salt concentration at the temperature of 25 ° C for 7 days, and it was transparent. It was confirmed that the transparency was slightly lowered Respectively.
FIG. 8 is a scanning electron microscope (SEM) image of silica nanoparticles according to a change in salinity of salt water in a method for producing silica nanofluid according to an embodiment of the present invention.
Referring to FIG. 8, the mean particle size was 42 nm at a sample B2-25 (10 wt%, 25 ° C), the particles were relatively homogeneously distributed, and the average at a sample B4-25 (20 wt% It was confirmed that the particle size was 51 nm and the particles were partially agglomerated.
As the concentration of salt increased, the average particle size increased but the colloidal dispersion stability could be maintained.
In order to confirm the dispersion stability of the silica nanofluid according to the concentration of the silica nanoparticles, the particle size was confirmed by changing the concentration of the silica nanoparticles as shown in Table 3 below.
9 is a graph showing the average particle size of the silica nanoparticles according to the concentration of the silica nanoparticles in the method of manufacturing the silica nanofluid according to the embodiment of the present invention.
Referring to FIG. 9, the average particle size was changed in the range of 30 to 42 nm at a room temperature of 25 ° C, and the average particle size was changed in the range of 44 to 50 nm at a high temperature of 90 ° C.
10 is a photograph showing changes in particle concentration and dispersion time of the produced silica nanofluid in the method for producing silica nanofluid according to an embodiment of the present invention.
Referring to FIG. 10 (a), it was confirmed that when the particle concentration was changed at 25 ° C. for 7 days, the dispersion stability was maintained, and the particle concentration was changed at 90 ° C. It was confirmed that the dispersion stability of the colloid was maintained.
11 is a scanning electron micrograph of the particle concentration of the prepared silica nanofluid in the method of producing a silica nanofluid according to an embodiment of the present invention.
11, the average particle size was 42 nm and relatively homogeneous in the N3-25 sample (particle concentration 0.5 wt%, 25 ° C), and even in the case of the N5-25 sample (
Therefore, it was confirmed that the average particle size did not change sensitively according to the change of the particle concentration.
Experimental Example 2: Analysis of rock-nanofluid reaction
In Experimental Example 1, it was confirmed that the silica-nanofluid having the dispersion stability was confirmed to be able to increase the efficiency of the petroleum recovery enhancement by performing a rock-fluid reaction analysis.
First, a sample for lipophilization was aged.
Five oils of limestone (Limestone, CaCO 3 , 98.52%) and five dolomite [CaMg (CO 3 ) 2, 93.81%] were prepared and aged at 80 ° C for 7 days to prepare oil kerosene , Then washed and dried.
The contact angle before and after the reaction was measured using a contact angle measuring apparatus.
FIG. 12 is a graph showing the contact angle according to the concentration of silica nanoparticles in a lime stone sample in a method for enhancing the recovery of oil using a silica nanofluid according to another embodiment of the present invention. FIG.
Referring to FIG. 12, five limestone samples were reacted with 0.1 to 4 wt% of nanofluids.
It was confirmed that when the concentration of the surface-modified silica nanoparticles was 2% or more, the hydrophilicity was improved.
When the concentration was less than 2%, the change in the wettability was not large and the lipophilic state remained.
13 is a photograph showing a change in the contact angle according to the concentration of the silica nanoparticles relative to the lime stone sample in the oil recovery enhancement method using the silica nanofluid according to another embodiment of the present invention.
13, it was confirmed that the contact angle before the reaction was 146 ° (oil-wet) and the contact angle after the reaction was 56 ° (water-wet).
14 is a graph showing a contact angle according to the concentration of silica nanoparticles in a dolomite sample in a petroleum recovery enhancement method using a silica nanofluid according to another embodiment of the present invention.
Referring to FIG. 14, five dolomite samples were reacted with 0.1 to 4 wt% of nanofluids.
When the concentration of the surface modified silica nanoparticles was more than 0.5%, it was confirmed to be hydrophilic and the adsorption environment of the rock surface was considered to be advantageous compared with the lime stone.
FIG. 15 is a photograph showing the change in the contact angle according to the concentration of silica nanoparticles relative to the dolomite sample in the oil recovery enhancement method using the silica nanofluid according to another embodiment of the present invention. FIG.
Referring to FIG. 15, it was confirmed that the contact angle before the reaction was 140 ° (oil-wet) and the contact angle after the reaction was 83.2 ° (water-wet).
Therefore, it is confirmed that the wettability of the oil after the reaction with the silica nanoparticles is greatly increased with respect to the lime stone sample and the dolomite sample. Therefore, when the oil is used as the injection fluid for the oil recovery enhancement method, Respectively.
Therefore, the method of manufacturing silica nanofluids according to the present invention can manufacture a nanofluid that maintains dispersion stability under high salt and high temperature conditions by modifying the surface by attaching silane to the silica nanoparticles in the nanofluid.
In addition, it was used as an injection fluid to enhance the recovery of petroleum to the carbonate reservoir with high salt and high temperature conditions. The size of nanoparticles in the nanofluid increased as the salinity of the dispersion solvent increased, but EOR could be applied below 100 nm. Respectively.
It was confirmed that the wettability improvement effect of silica nanofluid prepared from limestone and dolomite samples was confirmed. When the concentration of nanoparticles were 2% and 0.5% respectively, the surface of the rock could be hydrophilized. It can be greatly increased.
Although the method for producing the silica nanofluid according to the present invention and the method for enhancing the recovery of oil using the method have been described above, it is apparent that various modifications can be made without departing from the scope of the present invention.
Therefore, the scope of the present invention should not be construed as being limited to the embodiments described, but should be determined by equivalents to the appended claims, as well as the following claims.
It is to be understood that the foregoing embodiments are illustrative and not restrictive in all respects and that the scope of the present invention is indicated by the appended claims rather than the foregoing description, It is intended that all changes and modifications derived from the equivalent concept be included within the scope of the present invention.
Claims (14)
(b) introducing a silane coupling agent and performing a silane reaction to modify the surface of the silica nanoparticles;
(c) filtering and dialyzing the distilled water to obtain silica nanoparticles; And
(d) dispersing the silica nanoparticles in saline containing 5 to 20 wt% of salt, wherein the average particle size of the silica nanoparticles increases as the concentration of the salt increases One is to maintain colloidal dispersion stability,
Wherein the silica nanofluid maintains the dispersion stability of the silica nanoparticles at a temperature of 25 to 90 占 폚.
The silica sol
Wherein the silica nanofluid is a colloidal silica.
The silane coupling agent
(3-glycidyloxypropyl) trimethoxysilane]. The method of claim 1,
The (3-glycidyloxypropyl) trimethoxysilane is
0.0 > mmol / g. ≪ / RTI >
The silane reaction
And reacting at 65 to 75 ° C for 24 to 26 hours to attach silane to the silica nanoparticles.
The silica nanoparticles
Wherein the average particle size is between 35 and 55 nm.
The silica nanofluid
Lt; RTI ID = 0.0 >%< / RTI > to 3 wt%.
(i) identifying a carbonate reservoir layer and creating an injection well in the rock of the carbonate reservoir layer;
(ii) dispersing the silica sol in deionized water;
(iii) introducing a silane coupling agent and performing a silane reaction to modify the surface of the silica nanoparticles;
(iv) filtering and dialyzing the distilled water to obtain silica nanoparticles;
(v) dispersing the silica nanoparticles in a water layer to produce a silica nanofluid; And
(vi) injecting silica nanofluid into the pores of the rock through the injection well to recover petroleum in the rock,
The carbonate reservoir layer contains 5 to 20 wt% of salt, and the average particle size of the silica nanoparticles increases as the concentration of salt increases, but the stability of the colloid dispersion is maintained,
Wherein the prepared silica nanofluid has a dispersion stability of the silica nanoparticles maintained at a temperature of 25 to 90 DEG C in the step (v).
In the step (iii)
Wherein the silane coupling agent is (3-Glycidyloxypropyl) trimethoxysilane at a concentration of 0.05 to 5 mmol / g (3-glycidyloxypropyl) trimethoxysilane.
In the step (iii)
Wherein the silane reaction is carried out at 65 to 75 ° C for 24 to 26 hours to attach silane to the silica nanoparticles.
In the step (vi)
The silica nanofluid has a particle concentration of 0.05 to 3 wt%
And increasing the hydrophilicity of petroleum in the rock.
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