CN111413401B - Method for in-situ determination of low-mineralization-degree water flooding process on molecular scale - Google Patents
Method for in-situ determination of low-mineralization-degree water flooding process on molecular scale Download PDFInfo
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Abstract
The invention discloses a method for in-situ on-line simulation of a low-salinity water flooding process on a molecular scale by using a dissipative quartz crystal microbalance (QCM-D). Different model compounds are selected to modify and modify the commercial QCM-D chip so as to simulate the rock surface with different wettability. Representative model compounds such as C5Pe and Bisa were selected to simulate polar components in crude oil that tend to adhere to rock surfaces. The liquid environment is provided by aqueous solutions of different ionic species and concentrations. The invention can realize in-situ on-line simulation of the low-salinity water flooding process on a microscopic level through the simulation system, thereby providing theoretical support for actual low-salinity water flooding work. In addition, by comparing the adsorption and desorption behaviors of the crude oil simulant on surfaces with different wettabilities, the micro mechanism and the low mineralization effect of the low mineralization water flooding can be further analyzed and discussed.
Description
Technical Field
The invention belongs to the application of a quartz crystal microbalance technology, and particularly relates to a method for constructing an oil/water/rock three-phase system model by using a dissipative quartz crystal microbalance (QCM-D) technology and simulating a low-salinity water flooding process in situ on a molecular scale by using the model.
Background
Quartz Crystal Microbalances (QCMs), essentially a balance suitable for weighing a small mass of substance, can measure even the mass variations on the nanogram scale. Besides high measurement precision, the device can monitor the change of the mass in real time by monitoring the change of the vibration frequency and the dissipation of the chip, and can sharply catch the change and weak change no matter the mass is increased or reduced. Since the invention, it has been widely used in the fields of surface science, material science, life science, and the like. We have found that changes in mass can be used to confirm the occurrence of an interaction. Taking the adhesion of a surface as an example, if no increase in mass is detected, no interaction is considered to occur, i.e. no molecules adhere to the surface, and vice versa. QCM is therefore a more qualitative and quantitative method of studying the interaction between molecules and surfaces by monitoring the real-time changes in surface quality.
Research shows that reservoir structures are quite complex and heterogeneous, a complex oil/water/rock three-phase system is formed after low-salinity water is injected, and the complex interaction between the reservoir structures and the low-salinity water directly influences the actual recovery ratio. The key to improving the recovery of crude oil is to strip off more crude oil adhered to the surface of rock by various technical means. After decades of development, the low-mineralization water flooding technology has become a widely accepted and widely adopted oil displacement means. However, the oil displacement mechanism behind the method is still not uniformly known, mainly because the traditional macroscopic experiment can hardly detect the microscopic adsorption/desorption behaviors of crude oil on the rock surface in the low-salinity water flooding process, the establishment of the method capable of simulating the low-salinity water flooding process in situ from the microscopic level is very important.
Disclosure of Invention
The invention aims to provide a simple and direct method which is suitable for various oil/water/rock three-phase systems and can simulate a low-salinity water flooding process on a molecular scale in situ and on line.
The invention provides a method for simulating a low-mineralization-degree water flooding process in situ on a molecular scale, which comprises the following steps of: simulating an oil phase by using a solution of polar components in crude oil; injecting salt water solution consisting of different ions to provide a liquid environment and simulate a water phase; adopting a modified substrate as a simulated rock phase; mixing the oil phase, the water phase and the rock phase to obtain an oil/water/rock three-phase system; the variation curve of frequency (delta f) along with time under different salt solution concentrations is measured by using a dissipative quartz crystal microbalance, so that the in-situ on-line simulation of the low-salinity water flooding process on a molecular scale is realized.
In the method, the polar component is selected from asphalt model compounds C5Pe (shown in formula I), Bisa (shown in formula II), TP (shown in formula III) and PAP (shown in formula IV), which are the most representative polar components in the crude oil.
The solvent in the solution of the polar component may be ethanol; the concentration of polar molecules in the solution of the polar component may be 10 mM.
The ion can be sodium, chloride, magnesium, aluminum, sulfate, or calcium. In particular, the aqueous salt solution may be a sodium chloride solution, and the concentration may be 10mM to 100 mM.
The substrate can be a commercial QCM-D SiO2 chip; other coated chips, such as Au-coated chips, can also be selected according to different modification methods.
The invention selects different compounds to be used for commercial QCM-D SiO2Modifying the chip to form hydrophilic substrate with Si-OH bonds on the surface, or modifying the chip to form surface with-CH3Hydrophobic substrate) to simulate rock surfaces with different wettabilities.
The monomolecular adsorption layer is formed by silanization reaction by using Si-OH bonds on the surface of a commercial QCM-D SiO2 chip and selected modified molecules.
The specific modification method for the QCM-D SiO2 chip is as follows:
mixing QCM-D SiO2Washing the chip with ethanol and tertiary water for 3 times respectively, and performing plasmaa, processing to obtain a hydrophilic substrate with a surface rich in-OH; soaking the hydrophilic substrate in 5 wt% octadecyl trichlorosilane chloroform solution for 2-3h, taking out, ultrasonically cleaning with chloroform for 15-30min, and blow-drying to obtain the hydrophilic substrate with-CH on the surface3The hydrophobic substrate of (1).
The invention belongs to a method for simulating a low-mineralization-degree water flooding process in situ on a molecular scale by utilizing a dissipative quartz crystal microbalance (QCM-D) technology. The invention selects the polar components with the strongest polarity and the largest molecular weight in the crude oil, namely asphaltene model compounds C5Pe, Bisa and the like, to simulate the oil phase. By using modified commercial QCM-D SiO2The chip as a substrate simulates the rock phase. The liquid environment was provided by the injection of aqueous solutions of different ions, simulating the aqueous phase. Thereby realizing in-situ on-line simulation of the low-salinity water flooding process on the molecular scale. The invention can realize in-situ on-line simulation of the low-salinity water flooding process on a microscopic level through the simulation system, thereby providing theoretical support for actual low-salinity water flooding work. In addition, by comparing the adsorption and desorption behaviors of the crude oil simulant on surfaces with different wettabilities, the micro mechanism and the low mineralization effect of the low mineralization water flooding can be further analyzed and discussed.
Drawings
FIG. 1 is a contact angle test of substrates with different wettabilities modified as in example 1.
FIG. 2 is an in situ simulation of the low salinity waterflood process of example 1 using C5Pe as the oil phase.
Figure 3 is an in situ simulation of the low salinity waterflooding process of example 2 using Bisa as the oil phase.
FIG. 4 is an in situ simulation of the low salinity waterflooding process using TP as the oil phase in example 3.
FIG. 5 is an in situ simulation of the low salinity waterflooding process of example 4 using PAP as the oil phase.
Detailed Description
The present invention is described below with reference to specific embodiments, but the present invention is not limited thereto, and any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
The experimental procedures used in the following examples are all conventional procedures unless otherwise specified.
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
Example 1
Preparation of injection aqueous solution:
0.58g of sodium chloride was dissolved in 100mL of water, and the solution was dissolved with stirring to prepare a 100mM aqueous solution (Highsalanity, HS). 10mL of 100mM NaCl solution was diluted to 100mL to obtain 10mM (LS) sodium chloride solution.
Crude oil model compounds:
asphaltenes are the most polar components of the crude oil with the highest polarity and molecular weight, and are also the main cause of adhesion of the crude oil on rock surfaces. Therefore, an asphaltene model compound C5Pe (structural formula shown in formula I) is selected as a simulant, and an ethanol solution with the concentration of 10mM is used for simulating an oil phase.
Preparation of rock phase substrate:
mixing QCM-D SiO2After the chip is washed by ethanol and water for 3 times respectively, oxygen is introduced into the chip for 10min by a plasma cleaner, and a hydrophilic substrate with a rich-OH surface is obtained. Soaking the hydrophilic substrate in 5 wt% octadecyl trichlorosilane chloroform solution for 2-3h, taking out, ultrasonically cleaning with chloroform for 15-30min, and blow-drying to obtain the hydrophilic substrate with-CH on the surface3The hydrophobic substrate of (1). The contact angle values for different surfaces are shown in figure 1, for example.
As shown in FIG. 2, C5Pe simulated oil phase, NaCl aqueous solution as water phase, and modified SiO were measured using a dissipative quartz crystal microbalance2The chip is a time-varying curve of the frequency (delta f) of a rock phase three-phase system under different salt solution concentrations, namely the adsorption and desorption behaviors of crude oil in the low-salinity water drive process. The whole process is divided into two parts, one is that crude oil is on the surfaceThe adsorption process comprises the steps of introducing ethanol as a background solution, introducing a crude oil model compound solution for adsorption, and introducing ethanol again to wash off molecules with weak surface adsorption; and the other is simulating the low-mineralization-degree water flooding process, which comprises the steps of sequentially introducing solutions with different mineralization degrees and observing the change of the frequency along with time. Wherein, the change of the frequency (delta f) curve to the negative direction represents the adsorption of the crude oil on the surface, and the change of the curve to the positive direction represents the desorption of the crude oil from the surface in the water flooding process.
Example 2
Preparation of injection aqueous solution:
0.58g of sodium chloride was dissolved in 100mL of water, and the solution was dissolved with stirring to prepare a 100mM aqueous solution (Highsalanity, HS). 10mL of 100mM NaCl solution was diluted to 100mL to obtain 10mM sodium chloride solution (Lowsalinity, LS).
Crude oil model compounds:
asphaltenes are the most polar components of the crude oil with the highest polarity and molecular weight, and are also the main cause of adhesion of the crude oil on rock surfaces. Therefore, an asphaltene model compound Bisa (structural formula shown in formula II) is selected as a simulant, and an ethanol solution with the concentration of 10mM is used for simulating an oil phase.
Preparation of rock phase substrate:
mixing QCM-D SiO2After the chip is washed by ethanol and water for 3 times respectively, oxygen is introduced into the chip for 10min by a plasma cleaner, and a hydrophilic substrate with a rich-OH surface is obtained. Soaking the hydrophilic substrate in 5 wt% octadecyl trichlorosilane chloroform solution for 2-3h, taking out, ultrasonically cleaning with chloroform for 15-30min, and blow-drying to obtain the hydrophilic substrate with-CH on the surface3The hydrophobic substrate of (1). The contact angle values for different surfaces are shown in figure 2.
As shown in FIG. 3, the modified SiO is prepared by using Bisa simulated oil phase and NaCl aqueous solution as water phase2The frequency (delta f) of a three-phase system with a chip as a rock phase changes along with time under different salt solution concentrations, namely the low mineralization degreeAnd (3) crude oil adsorption and desorption in the water drive process. The whole process is divided into two parts, wherein one part is the adsorption process of the crude oil on the surface, and the adsorption process comprises the steps of introducing ethanol as a background solution, introducing a crude oil model compound solution for adsorption, and introducing ethanol again to wash off molecules with weak surface adsorption; and the other is simulating the low-mineralization-degree water flooding process, which comprises the steps of sequentially introducing solutions with different mineralization degrees and observing the change of the frequency along with time.
Example 3
Preparation of injection aqueous solution:
0.58g of sodium chloride was dissolved in 100mL of water, and the solution was dissolved with stirring to prepare a 100mM aqueous solution (Highsalanity, HS). 10mL of 100mM NaCl solution was diluted to 100mL to obtain 10mM sodium chloride solution (Lowsalinity, LS).
Crude oil model compounds:
asphaltenes are the most polar components of the crude oil with the highest polarity and molecular weight, and are also the main cause of adhesion of the crude oil on rock surfaces. Therefore, an asphaltene model compound TP (structural formula shown in formula III) is selected as a simulant, and an ethanol solution with the concentration of 10mM is used for simulating an oil phase.
Preparation of rock phase substrate:
mixing QCM-D SiO2After the chip is washed by ethanol and water for 3 times respectively, oxygen is introduced into the chip for 10min by a plasma cleaner, and a hydrophilic substrate with a rich-OH surface is obtained. Soaking the hydrophilic substrate in 5 wt% octadecyl trichlorosilane chloroform solution for 2-3h, taking out, ultrasonically cleaning with chloroform for 15-30min, and blow-drying to obtain the hydrophilic substrate with-CH on the surface3The hydrophobic substrate of (1). The contact angle values for different surfaces are shown in figure 2.
As shown in FIG. 4, the oil phase was simulated using TP, the aqueous NaCl solution was used as the aqueous phase, and the modified SiO was obtained2The chip is a time-varying curve of the frequency (delta f) of a rock phase three-phase system under different salt solution concentrations, namely the adsorption and desorption behaviors of crude oil in the low-salinity water drive process. All overThe process is divided into two parts, wherein one part is the adsorption process of the crude oil on the surface, and the adsorption process comprises the steps of introducing ethanol as a background solution, introducing a crude oil model compound solution for adsorption, and introducing ethanol again to wash off molecules with weak surface adsorption; and the other is simulating the low-mineralization-degree water flooding process, which comprises the steps of sequentially introducing solutions with different mineralization degrees and observing the change of the frequency along with time.
Example 4
Preparation of injection aqueous solution:
0.58g of sodium chloride was dissolved in 100mL of water, and the solution was dissolved with stirring to prepare a 100mM aqueous solution (HS). 10mL of NaCl 100mM solution was diluted to 100mL to obtain 10mM sodium chloride solution (Low saline, LS).
Crude oil model compounds:
asphaltenes are the most polar components of the crude oil with the highest polarity and molecular weight, and are also the main cause of adhesion of the crude oil on rock surfaces. Therefore, an asphaltene model compound PAP (structural formula shown in formula IV) is selected as a simulant, and an ethanol solution with the concentration of 10mM is used for simulating an oil phase.
Preparation of rock phase substrate:
mixing QCM-D SiO2After the chip is washed by ethanol and water for 3 times respectively, oxygen is introduced into the chip for 10min by a plasma cleaner, and a hydrophilic substrate with a rich-OH surface is obtained. Soaking the hydrophilic substrate in 5% chloroform solution of octadecyl trichlorosilane for 2-3h, taking out, ultrasonically cleaning with chloroform for 15-30min, and blow-drying to obtain the hydrophilic substrate with-CH on the surface3The hydrophobic substrate of (1). The contact angle values for different surfaces are shown in figure 2.
As shown in FIG. 5, PAP simulated oil phase and NaCl aqueous solution were used as water phase, and modified SiO was used2The chip is a time-varying curve of the frequency (delta f) of a rock phase three-phase system under different salt solution concentrations, namely the adsorption and desorption behaviors of crude oil in the low-salinity water drive process. The whole process is divided into two parts, one is the adsorption process of the crude oil on the surface,introducing ethanol as a background solution, introducing a crude oil model compound solution for adsorption, and introducing ethanol again to wash off molecules with weak surface adsorption; and the other is simulating the low-mineralization-degree water flooding process, which comprises the steps of sequentially introducing solutions with different mineralization degrees and observing the change of the frequency along with time.
Claims (1)
1. A method for simulating a low salinity water flooding process in situ on a molecular scale, comprising the steps of: simulating an oil phase by using a solution of polar components in crude oil; injecting water solution composed of different ions to provide liquid environment and simulate water phase; adopting a modified substrate as a simulated rock phase; mixing the oil phase, the water phase and the rock phase to obtain an oil/water/rock three-phase system; measuring a change curve of frequency (delta f) along with time under different salt solution concentrations by using a dissipative quartz crystal microbalance, and realizing in-situ on-line simulation of a low-salinity water flooding process on a molecular scale;
the polar component in the crude oil is selected from compounds represented by any one of the following formulas I-IV:
the solvent in the polar component solution is ethanol; the concentration of polar molecules in the solution of the polar component is 10 mM;
the substrate is commercial QCM-D SiO2A chip;
for the QCM-D SiO2Modifying the chip to form Si-OH on the surface of the chip to form a hydrophilic substrate; or modifying the QCM-D SiO2 chip to enable the surface of the QCM-D SiO2 chip to have hydrophobic groups to form a hydrophobic substrate;
the ions of the aqueous solution are selected from at least one of: sodium ion, chloride ion, magnesium ion, aluminum ion, sulfate ion, or calcium ion.
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| CN108508239A (en) * | 2018-04-04 | 2018-09-07 | 中国科学院化学研究所 | A kind of analogy method directly measuring oil/water/rock three-phase intermolecular interaction |
| CN108876055A (en) * | 2018-07-09 | 2018-11-23 | 中国石油大学(华东) | A kind of extra-low permeability oil reservoirs low mineralization water drive prediction of result method |
| CN109296347A (en) * | 2018-06-13 | 2019-02-01 | 西南石油大学 | A kind of direct observation simulator and method of low mineralization water drive |
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| CN108508239A (en) * | 2018-04-04 | 2018-09-07 | 中国科学院化学研究所 | A kind of analogy method directly measuring oil/water/rock three-phase intermolecular interaction |
| CN109296347A (en) * | 2018-06-13 | 2019-02-01 | 西南石油大学 | A kind of direct observation simulator and method of low mineralization water drive |
| CN108876055A (en) * | 2018-07-09 | 2018-11-23 | 中国石油大学(华东) | A kind of extra-low permeability oil reservoirs low mineralization water drive prediction of result method |
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