CN111413401A - 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 realize real-time monitoring of mass change by monitoring the change of chip vibration frequency and dissipation, and can sharply capture 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 quantitative and qualitative 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 point for improving the recovery efficiency of the crude oil is to strip off more crude oil adhered to the surface of the 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 line in situ on a molecular scale.
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 composed 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 method is characterized in that a dissipative quartz crystal microbalance is utilized to measure the change curve of frequency (delta f) along with time under different salt solution concentrations, and 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 crude oil, in-situ on-line simulation of low salinity water flooding is realized on the molecular scale.
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 plasma treatment 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 a molecular scale. The invention can realize in-situ on-line simulation of the low-salinity water drive process on a microscopic level by the simulation system, thereby providing theoretical support for the actual low-salinity water drive 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 hypomineralization effect of the hypomineralization 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 100m L of water, and dissolved by stirring to prepare a 100mM aqueous solution (Highsalanity, HS). A10 m L NaCl100mM solution was diluted to 100m L to obtain a 10mM (L w saline, L S) 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, a plasma cleaner is used for introducing oxygen for treatment for 10min, 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 and modified SiO were used as the aqueous phase in the measurement by 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, 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. Wherein, the change of the frequency (delta f) curve towards the negative direction represents the adsorption of the crude oil on the surface, and the change of the frequency (delta f) curve towards 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 100m L of water, and dissolved with stirring to prepare a 100mM aqueous solution (Highsalanity, HS). A10 mM solution of L of NaCl in 100mM was diluted to 100m L to obtain a 10mM sodium chloride solution (L lowsalanity, L S).
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, a plasma cleaner is used for introducing oxygen for treatment for 10min, 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 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, 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 100m L of water, and dissolved with stirring to prepare a 100mM aqueous solution (Highsalanity, HS). A10 mM solution of L of NaCl in 100mM was diluted to 100m L to obtain a 10mM sodium chloride solution (L lowsalanity, L S).
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, a plasma cleaner is used for introducing oxygen for treatment for 10min, 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. 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 process of water flooding with low mineralization degree, which comprises the steps of sequentially introducing solutions with different mineralization degrees and observing the change of frequency along with time.
Example 4
Preparation of injection aqueous solution:
0.58g of sodium chloride was dissolved in 100m L of water, and dissolved with stirring to prepare a 100mM aqueous solution (Highsalanity, HS). A10 mM solution of L of NaCl in 100mM was diluted to 100m L to obtain a 10mM sodium chloride solution (L lowsalanity, L S).
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, a plasma cleaner is used for introducing oxygen for treatment for 10min, 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 surface3A hydrophobic substrate. 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, 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.
Claims (6)
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; 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.
3. the method according to claim 1 or 2, characterized in that: 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.
4. The method according to any one of claims 1-3, wherein: 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.
5. The method according to any one of claims 1-4, wherein: the substrate is a commercial QCM-D SiO2 chip.
6. The method of claim 5, wherein: modifying the QCM-D SiO2 chip to form Si-OH on the surface of the QCM-D SiO2 chip so as to form a hydrophilic substrate; or modifying the QCM-D SiO2 chip to make the surface thereof carry hydrophobic groups to form a hydrophobic substrate.
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