CN111909679B - Preparation method and application of composition for reducing minimum miscible pressure of carbon dioxide and crude oil based on aerosol surfactant - Google Patents
Preparation method and application of composition for reducing minimum miscible pressure of carbon dioxide and crude oil based on aerosol surfactant Download PDFInfo
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Abstract
本发明涉及一种基于气溶性表面活性剂降低二氧化碳与原油最小混相压力的组合物制备方法及应用，所述组合物的制备方法为：将气溶性表面活性剂与无水乙醇按重量份比1：(10‑20)的比例混合均匀，配制得到气溶性表面活性剂的乙醇溶液待用；将步骤(1)配制的气溶性表面活性剂的乙醇溶液与液态二氧化碳按质量百分比为10‑25％的比例混合均匀制得组合物；上述组合物应用于二氧化碳驱油，有效降低二氧化碳与原油最小混相压力。
The invention relates to a preparation method and application of a composition for reducing the minimum miscible pressure of carbon dioxide and crude oil based on an aerosol surfactant. : the ratio of (10-20) is evenly mixed, and the ethanol solution of the aerosol surfactant is prepared for use; the ethanol solution of the aerosol surfactant prepared in step (1) and the liquid carbon dioxide are 10-25% by mass percentage The above composition is used in carbon dioxide flooding oil, and effectively reduces the minimum miscibility pressure of carbon dioxide and crude oil.
Description
Technical Field
The invention relates to a preparation method and an application method of a composition of an aerosol surfactant for reducing minimum miscible pressure of carbon dioxide and crude oil, and belongs to the technical field of carbon dioxide oil displacement additives.
Background
With the increasing demand for energy, the exploration and development of unconventional oil reservoirs becomes more and more important, especially for very low permeability tight oil resources (permeability: 0.01X 10)-3μm2-0.1×10-3μm2). The use of waterflooding in tight reservoirs is challenging due to lower permeability and poor injectivity. Compared with water injection, carbon dioxide has lower viscosity and better injectability, so that carbon dioxide injection for flooding is a promising method for improving the recovery ratio of the tight oil reservoir. Furthermore, the minimum miscible pressure of carbon dioxide with crude oil is much lower than that of other gases (e.g., nitrogen or methane), which means that miscible flooding is easier to achieve when injecting carbon dioxide into the reservoir. A large number of theories and practices prove that the oil displacement efficiency of carbon dioxide miscible flooding is far higher than that of non-miscible flooding. The Minimum Miscible Pressure (MMP) of carbon dioxide Miscible flooding refers to that under certain Pressure and temperature, when the interfacial tension between oil and gas phases is zero (namely the interfacial tension disappears), the oil and gas phases are Miscible, and the Pressure at the moment is the Minimum Miscible Pressure of the carbon dioxide Miscible flooding.
At present, methods for reducing miscible pressure are mainly classified into an oil-soluble surfactant method, a miscible solvent method, and a supercritical carbon dioxide microemulsion method, depending on the type of the agent used.
(1) The oil-soluble surfactant method generally refers to that an oil-soluble surfactant is injected into a stratum, and the surfactant is dissolved and reduced in viscosity in crude oil so as to reduce the miscible pressure of subsequently injected carbon dioxide and the crude oil. The common construction scheme corresponding to the method is as follows: the method comprises the steps of firstly injecting a surfactant slug into an oil well, and then injecting a carbon dioxide slug after the surfactant slug of the slug is dissolved in the crude oil in the stratum. However, when the method is actually applied in a mine, as shown in fig. 1, the injected surfactant slug is difficult to effectively contact with the crude oil, so that the surfactant slug cannot be efficiently dissolved in the crude oil, and particularly when the method is applied to a stratum with relatively severe heterogeneity (fig. 2), the injected surfactant slug and the carbon dioxide slug have a bottleneck that the carbon dioxide slug and the surfactant slug cannot effectively contact with each other due to factors such as gravity difference and stratum permeability difference, so that the oil-soluble surfactant method has the phenomena of large injection amount of the medicament, low action efficiency, high cost and poor effect when being actually applied in the mine.
In view of the above problems, improved oil-soluble surfactant methods have been developed, such as one proposed in chinese patent CN102337874A for miscible flooding CO reduction2The method is characterized in that the method is also an injected oil-soluble surfactant, but the screened oil-soluble surfactant has a certain carbon dioxide affinity and can be dissolved in supercritical carbon dioxide under a certain temperature and pressure condition, so that when the injected carbon dioxide is converted into a supercritical state under a formation temperature and pressure condition during the injection of a carbon dioxide slug, the injected oil-soluble surfactant slug can be solubilized, the carbon dioxide can carry the surfactant to contact with the crude oil, and the effect of reducing the miscible pressure is realized. Although the method can improve the contact efficiency of the carbon dioxide, the surfactant and the crude oil, the solubilization efficiency of the carbon dioxide on the surfactant in the contact process is low and the effect of reducing the miscible pressure is not very obvious because the contact area of the carbon dioxide slug injected subsequently and the surfactant slug injected in the preamble in the formation pore is small and the gravity floating effect in the contact process still exists. And the methodThe premise of the method application is still that the surfactant slug needs to be injected into the stratum, so that if the method is applied to oil reservoirs with low permeability, such as ultra-low permeability oil reservoirs, compact oil reservoirs and the like, the oil-soluble surfactant has the problems of high injection pressure and incapability of injection, and the method cannot be applied.
(2) The miscible solvent method generally means that low molecular weight hydrocarbons and low carbon alcohols are utilized, and the low molecular weight hydrocarbons are generally gaseous hydrocarbons and can be mixed with carbon dioxide for injection, and the low molecular weight hydrocarbons and crude oil react for many times in a stratum to form a miscible phase; the low-carbon alcohols are commonly used as methanol, ethanol, butanol, pentanol and the like, and can be mixed with carbon dioxide under certain temperature and pressure conditions, so that the mixture is injected into a stratum together, and can form a mixed phase through multiple actions with crude oil. Chinese patent CN105422066A proposes a method for reducing the minimum miscible pressure of carbon dioxide flooding by using lower alcohol miscible solvents such as methanol and ethanol, and the method proves that after 3-5% of alcohol mixture is added into crude oil, the minimum miscible pressure between carbon dioxide and crude oil can be reduced by 9.21%, which shows that the system miscible pressure can be reduced by adding a small amount of mixed alcohol into a carbon dioxide/crude oil system. However, in the application process of the method, because the different alcohols and the carbon dioxide have different mixing and dissolving capacities, the pressure conditions required for mixing and dissolving the alcohols and the carbon dioxide are different, so that the carbon dioxide and the low-carbon alcohol medicaments are easily separated step by step in the injection process and the stratum flowing process, the carbon dioxide and the low-carbon alcohol medicaments cannot be synchronously moved when flowing in the stratum, and further cannot simultaneously interact with the crude oil, so that part of the low-carbon alcohol medicaments form ineffective injection, and the mixed phase pressure capacity of the low-carbon alcohol medicaments is reduced.
(3) The supercritical carbon dioxide microemulsion method combines the supercritical technology and the microemulsion technology, utilizes the nano-scale aggregate formed by dispersing surfactant molecules in the supercritical carbon dioxide, takes the supercritical carbon dioxide as a continuous phase and the surfactant as a dispersed phase, and water molecules are dissolved in an inner core formed by polar heads of the surfactant, so that the minimum miscible phase pressure is reduced through the solubilization. Chinese patent CN104194762A proposes a supercritical carbon dioxide microemulsionThe method for reducing the miscible pressure of carbon dioxide and crude oil is to select the supercritical carbon dioxide microemulsion formed by the surface active agents such as homologues of sodium di- (1-ethyl-2-methyl-1-pentyl) sulfosuccinate and the alcohol auxiliary agents to reduce the miscible pressure of the carbon dioxide and the crude oil, and the reduction amplitude can reach 10%. However, the current supercritical carbon dioxide microemulsion method has limited capability of reducing miscible pressure, and the presence of water in the system is not favorable for reducing the miscible pressure. Chinese patent CN104610953A and Chinese literature fatty alcohol polyoxypropylene Ether to CO2The method for reducing the mixed phase pressure by using the supercritical carbon dioxide microemulsion is also proposed in the influence of the minimum mixed phase pressure, preferably selects fatty alcohol polyoxyethylene polyoxypropylene ether and alkylphenol polyoxyethylene polyoxypropylene ether, and respectively compounds one or more of low-carbon alcohols (methanol, ethanol, propanol, butanol and the like) to form the supercritical carbon dioxide microemulsion so as to reduce the mixed phase pressure. As described in the patent, the lower alcohol co-solvent is added in a small amount, and the polymerization degree of oxyethylene and oxypropylene in the preferred surfactant is low, so that the solubility of the preferred surfactant in supercritical carbon dioxide is low, which is not beneficial to the long-distance migration of the surfactant carried by the supercritical carbon dioxide in a dissolving way in a porous medium. Chinese patent CN103867169A discloses a method for controlling the mobility of carbon dioxide flooding by using an aerosol surfactant, in which the preferred aerosol surfactants are fatty alcohol polyoxyethylene polyoxypropylene ether and alkylphenol polyoxyethylene polyoxypropylene ether, however, because the main purpose of the invention is to control the mobility of carbon dioxide by using supercritical carbon dioxide to dissolve the aerosol surfactant and bring it into the formation to contact with formation water to form foam, the preferred surfactant dosage is lower, and no auxiliary agent is added to improve the solubility of the surfactant in carbon dioxide. Therefore, there is a need to develop a new system for reducing miscible pressure surfactant to a certain extent, which can be dissolved in supercritical carbon dioxide, and injected into the formation by supercritical carbon dioxide, so as to improve the injection capability and increase the action efficiency, thereby achieving a large miscible pressure of carbon dioxide and crude oilThe degree decreases.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method and application of a composition for reducing the minimum miscible pressure of carbon dioxide and crude oil based on a gas-soluble surfactant. The technology can further promote the large-scale application of the carbon dioxide flooding technology in China, realize miscible flooding in the carbon dioxide flooding process, improve the flooding effect, and lay a foundation for realizing win-win of carbon dioxide emission reduction and utilization.
The technical scheme of the invention is as follows:
a method for preparing a composition for reducing the minimum miscible pressure of carbon dioxide and crude oil based on an aerosol surfactant comprises the following steps:
(1) mixing an aerosol surfactant and absolute ethyl alcohol according to a weight ratio of 1: (10-20) mixing uniformly according to the proportion to prepare an ethanol solution of the aerosol surfactant for later use;
(2) and (2) uniformly mixing the ethanol solution of the aerosol surfactant prepared in the step (1) and liquid carbon dioxide according to the mass percentage of 10-25% to prepare the composition.
Preferably, according to the invention, the aerosol surfactant described in step (1) is a dehydrated powder.
Preferably, according to the present invention, the aerosol surfactant described in step (1) is an aerosol surfactant containing a carbon dioxide-philic group.
Further preferably, the carbon dioxide-philic group is a polyoxyethylene group or a polyoxypropylene group.
More preferably, the aerosol surfactant is fatty alcohol polyoxyethylene polyoxypropylene ether or nonylphenol polyoxyethylene ether, wherein the polymerization degree of the oxyethylene is 9-12.
More preferably, the aerosol surfactant is fatty alcohol polyoxyethylene polyoxypropylene ether or nonylphenol polyoxyethylene ether, wherein the polymerization degree of the oxyethylene is 9.
According to the invention, preferably, in the step (1), the ratio of the aerosol surfactant to the absolute ethyl alcohol is 1: 10, and preparing an ethanol solution of the aerosol surfactant for later use.
Further preferably, the ethanol solution of the aerosol surfactant prepared in the step (1) and the liquid carbon dioxide are uniformly mixed according to the mass percentage of 20% to prepare the composition.
The solubility of the gas soluble surfactant in the supercritical carbon dioxide under the conditions of the temperature of 40-90 ℃ and the pressure of 10-30 MPa is 0.05-0.35 wt%, and when the supercritical carbon dioxide contains 10-25 wt% of absolute ethyl alcohol, the solubility of the gas soluble surfactant in the supercritical carbon dioxide can be improved to 0.5-2.5 wt% under the same temperature and pressure conditions.
The composition is applied to carbon dioxide flooding, and the minimum miscible pressure of carbon dioxide and crude oil is reduced.
According to the invention, the application method of the composition comprises the following steps:
when the oil reservoir is shallow in buried depth and reaches an oil displacement layer, the composition cannot be converted into a supercritical state, and the composition is directly injected in a supercritical carbon dioxide mode to displace oil.
Further preferably, the reservoir burial depth is less than 1500 m.
Further preferably, the composition is prepared by uniformly mixing the ethanol solution of the air-soluble surfactant and liquid carbon dioxide according to the mass percentage of 10-20%.
According to the invention, the application method of the composition comprises the following steps:
when the oil reservoir is deeply buried, the composition reaches an oil displacement layer and is converted into a supercritical state, and the composition is injected in a liquid form to displace oil.
Further preferably, the reservoir burial depth is more than 1500 m.
Further preferably, the composition is prepared by uniformly mixing the ethanol solution of the air-soluble surfactant and liquid carbon dioxide according to the mass percentage of 15-25%.
According to the invention, the composition is preferably used, wherein the ratio of the aerosol surfactant to the absolute ethyl alcohol is 1: 10 are mixed uniformly.
Further preferably, the composition is prepared by uniformly mixing an ethanol solution of the aerosol surfactant and liquid carbon dioxide according to the mass percentage of 20%.
The technical scheme of the invention has the beneficial effects
1. The method applies the gas soluble surfactant to reduce the miscible pressure of the carbon dioxide and the crude oil for the first time, and uniformly mixes the ethanol solution of the gas soluble surfactant with the liquid carbon dioxide and injects the mixture into the stratum, or directly pressurizes and heats the mixture on the ground to a supercritical state after uniform mixing and injects the mixture into the stratum; in addition, the problem that the conventional miscible pressure reducing agent and the carbon dioxide cannot be effectively mixed due to the gravity separation effect of the two agents (as shown in figure 3) is avoided, and when the agent flows to the heterogeneous formation, the aerosol surfactant can still be dissolved in the supercritical carbon dioxide and can be transported together with the supercritical carbon dioxide to contact with the crude oil to exert the effect of reducing the miscible pressure (as shown in figure 4).
2. The preferred gas-soluble surfactant is an ethanol solution of the gas-soluble surfactant, which is prepared by dehydrated surfactant powder and absolute ethanol according to a certain mass ratio, and the system does not contain water, so that the dependence on water phase injection in the construction process of reducing miscible phase pressure by the existing supercritical carbon dioxide microemulsion method is avoided, the injection capability of the system selected by the invention in oil reservoirs with lower permeability such as compact oil reservoirs is greatly improved, and the application range of the system is expanded.
3. The addition amount (10 wt% -25 wt%) of the preferred auxiliary agent ethanol is greatly improved compared with the addition amount (less than 5 wt%) of the conventional method, so that the method is favorable for remarkably improving the solubility of the surfactant in the supercritical carbon dioxide, is convenient for the supercritical carbon dioxide to dissolve and carry the surfactant to be remotely moved in a porous medium, and is favorable for deep mass transfer to reduce the miscible phase pressure; on the other hand, the distribution coefficient of the surfactant between the supercritical carbon dioxide and the crude oil can be adjusted by adjusting the addition amount of the auxiliary agent ethanol (the distribution coefficient refers to the ratio of the solubility of the surfactant in the supercritical carbon dioxide to the solubility of the surfactant in the crude oil when the supercritical carbon dioxide carrying the surfactant is fully mixed with the crude oil and before the mixing phase and the two are separated again), the balance relationship between the surfactant and the parent crude oil can be optimized by adjusting the parameter, and the interface effect of the surfactant on the interface between the carbon dioxide and the crude oil is exerted to the maximum.
Drawings
FIG. 1 is a schematic diagram of a period of time during which a soluble surfactant is injected to reduce miscible pressure and the plug is injected to cause carbon dioxide to be out of contact with crude oil;
FIG. 2 is a schematic illustration of the gravity differentiation of a heterogeneous formation during the injection of a soluble surfactant;
FIG. 3 is a schematic diagram of miscible flooding of a supercritical carbon dioxide injection formation with an aerosol surfactant;
FIG. 4 is a schematic diagram of miscible flooding of a heterogeneous formation with an aerosol surfactant dissolved in supercritical carbon dioxide;
FIG. 5 is a flow chart of an interfacial tension test experiment;
FIG. 6 is an interfacial tension of carbon dioxide and crude oil system at different pressures;
FIG. 7 is a graph showing the effect of varying degrees of polymerization of ethylene oxide on the reduction of miscible pressure of carbon dioxide and crude oil by an aerosol surfactant;
FIG. 8 is a graph showing the effect of various alcoholic adjuvants on the reduction of the miscible pressure of carbon dioxide and crude oil by an aerosol surfactant;
FIG. 9 is a flow chart of a long core displacement experiment;
FIG. 10 is a graph of the cumulative recovery of carbon dioxide displaced crude at different pressures;
FIG. 11 is a control flow diagram of a method for reducing minimum miscible pressure of carbon dioxide and crude oil based on a gas-soluble surfactant as described in example 1;
in the figure: 1. a liquid carbon dioxide tanker; 2. a high pressure storage tank; 3. a high-pressure stirring tank; 4. ground pumping equipment; 5. a warming device; 6. an injection well; 7. ground pumping equipment; 8. an injection well; 9. a shallow reservoir; 10. deep reservoir.
Detailed Description
The technical solutions of the present invention are further described below with reference to the drawings and the embodiments of the specification, but the scope of the present invention is not limited thereto.
Source of raw materials
The surfactant used in the invention is obtained by purchase, dried at 60 ℃ to be processed into powder and then used.
Experimental examples 1-4 the 2-ethyl-1-hexanol-polyoxypropylene polyoxyethylene ether is obtained from Shanghai highland barley limited company, the purity is not less than 98.5%, and the structural formula is as follows:
wherein: m is 6-15, and n is 5.
Experimental examples 1-4 the nonylphenol polyoxyethylene ether was obtained from Shanghai Michelin Biochemical technology Ltd, and was chemically pure, and the structural formula was as follows:
wherein: n is 4 to 15.
Experimental example 1
The gas-soluble surfactant reduces the miscible pressure of carbon dioxide/crude oil, and the polymerization degree of ethylene oxide of the gas-soluble surfactant is preferably tested:
the experimental conditions are as follows:
(1) simulating the oil reservoir temperature: 60 ℃;
(2) experimental oil: the technical scheme is applicable to crude oil viscosity of less than 100mPa & s under the oil reservoir condition, and the degassed crude oil in the high 89 blocks of the victory oil field is selected in the experimental example, and belongs to typical compact oil reservoir blocks, wherein the crude oil viscosity is 24mPa & s under the oil reservoir condition;
(3) carbon dioxide: the purity is 99.9 percent, and the product is produced by Qingdao Tianyuan gas manufacturing company Limited;
(4) air-soluble surfactant: 2-Ethyl-1-hexanol-polyoxypropylene Polyoxyethylene Ether (fatty alcohol polyoxyethylene polyoxypropylene Ether) (2 EH-PO)n-EOmN is 5, m is 6, 9, 13, 15), nonylphenol polyoxyethylene ether (NP-m, m is 4, 6, 9, 12, 15).
(5) The absolute ethyl alcohol is a common commercial product
(6) Tracker-H type interfacial tensiometer: manufactured by Teclis, France.
Purpose of the experiment:
simulating the process that the gas-soluble surfactant is contacted with crude oil after being dissolved and carried into a stratum by supercritical carbon dioxide, measuring the change of the interfacial tension of the carbon dioxide and the crude oil under the action of the gas-soluble surfactant by a pendant drop method, obtaining the minimum miscible phase pressure of the carbon dioxide and the crude oil before and after the gas-soluble surfactant is added by utilizing an interfacial tension disappearance method, and evaluating the influence rule of the polymerization degree of the ethylene oxide of the gas-soluble surfactant on the capability of reducing the minimum miscible phase pressure of the carbon dioxide and the crude oil.
Experimental procedure (experimental flow chart shown in fig. 5):
(1) testing the air tightness of the experimental device by using high-pressure nitrogen;
(2) sequentially cleaning the high-temperature high-pressure reaction kettle, the injection syringe and the straight needle by using acetone, absolute ethyl alcohol and distilled water;
(3) installing the syringe and the needle tube filled with the crude oil on a driving system;
(4) uniformly preparing an aerosol surfactant and absolute ethyl alcohol according to a certain mass ratio, and then injecting an ethanol solution of the aerosol surfactant and liquid carbon dioxide into a high-pressure closed container according to a certain mass ratio to uniformly prepare for later use;
(5) adjusting the temperature of the high-temperature high-pressure reaction kettle to 60 ℃, injecting a certain amount of ethanol solution of the gas-soluble surfactant and liquid carbon dioxide into the high-temperature high-pressure reaction kettle, and adjusting the injection amount to reach the required experimental pressure after the temperature is stable;
(6) adjusting the base to enable the needle head to appear in the visual window, and driving the motor to enable the oil drops to form a downward suspension oil drop on the needle point of the syringe;
(7) input of CO in control system2And the oil drop density, the volume of the oil drop and the dynamic interfacial tension are measured in real time through a data image acquisition system;
(8) increasing the pressure, re-extruding oil drops, repeating the experiment, and measuring the interfacial tension of the carbon dioxide and the crude oil under different pressures;
(9) and obtaining the pressure when the interfacial tension is zero according to a linear extrapolation method, namely the minimum miscible pressure of the carbon dioxide and the crude oil.
The experimental results are as follows:
as shown in fig. 6, the interfacial tension of pure carbon dioxide and crude oil under different pressures is measured, and then the data points are subjected to piecewise linear fitting, wherein the pressure corresponding to the intersection point of the solid line part and the abscissa obtained by fitting is the Minimum Miscible Pressure (MMP) of carbon dioxide and crude oil in multiple contact, and the pressure corresponding to the intersection point of the dotted line part and the abscissa is the minimum miscible pressure (P) of carbon dioxide and crude oil in one contactmax). MMP was measured to be 16.79MPa, P according to this methodmax＝30.56MPa。
Similarly, MMP after the addition of aerosol surfactants with different degrees of polymerization of ethylene oxide was tested according to this method is shown in FIG. 7.
As can be seen from fig. 7, when the mass ratio of the aerosol surfactant to the auxiliary ethanol is 1: 10, when the addition amount of the ethanol solution of the aerosol surfactant is 20 wt% of the mass of the carbon dioxide, the miscible pressure of the carbon dioxide and the crude oil is firstly reduced and then increased with the increase of the polymerization degree of the ethylene oxide in both the fatty alcohol polyoxyethylene polyoxypropylene ether and the nonylphenol polyoxyethylene ether. The reason for this is mainly because the oxyethylene group has the carbon dioxide affinity, and the solubility of the two types of surfactants in carbon dioxide increases with the increase of the polymerization degree of oxyethylene, but when the polymerization degree of oxyethylene is too high, the increase of the solubility in carbon dioxide becomes slow due to the increase of the molecular weight thereof, and the increase of the molecular weight thereof causes the increase of the lipophilicity thereof, which affects the adsorption thereof at the gas-liquid interface, thereby causing the decrease of the ability thereof to reduce the interfacial tension. From this experimental example, it is preferable that the optimum degree of polymerization of oxyethylene is 9.
Experimental example 2
The type of the alcohol auxiliary agent used by the gas-soluble surfactant for reducing the carbon dioxide/crude oil miscible pressure is preferably tested:
the experimental conditions are as follows:
(1) simulating the oil reservoir temperature: 60 ℃;
(2) experimental oil: the technical scheme is applicable to crude oil viscosity of less than 100mPa & s under the oil reservoir condition, and the degassed crude oil in the high 89 blocks of the victory oil field is selected in the experimental example, and belongs to typical compact oil reservoir blocks, wherein the crude oil viscosity is 24mPa & s under the oil reservoir condition;
(3) carbon dioxide: the purity is 99.9 percent, and the product is produced by Qingdao Tianyuan gas manufacturing company Limited;
(4) air-soluble surfactant: 2-Ethyl-1-hexanol-polyoxypropylene Polyoxyethylene Ether (fatty alcohol polyoxyethylene polyoxypropylene Ether) (2 EH-PO)5-EO9) Nonylphenol polyoxyethylene ether (NP-9).
(5) Methanol and glycol are common commercial products
(6) Tracker-H type interfacial tensiometer: manufactured by Teclis, France.
Purpose of the experiment:
simulating the process that the gas-soluble surfactant is contacted with crude oil after being dissolved and carried into a stratum by supercritical carbon dioxide, measuring the change of the interfacial tension of the carbon dioxide and the crude oil under the action of the gas-soluble surfactant by a pendant drop method, obtaining the minimum miscible phase pressure of the carbon dioxide and the crude oil before and after the gas-soluble surfactant is added by utilizing an interfacial tension disappearance method, and evaluating the influence rule of different alcohol auxiliary agents on the capability of the gas-soluble surfactant for reducing the minimum miscible phase pressure of the carbon dioxide and the crude oil.
Experimental procedure (experimental flow chart shown in fig. 5):
(1) testing the air tightness of the experimental device by using high-pressure nitrogen;
(2) sequentially cleaning the high-temperature high-pressure reaction kettle, the injection syringe and the straight needle by using acetone, absolute ethyl alcohol and distilled water;
(3) installing the syringe and the needle tube filled with the crude oil on a driving system;
(4) uniformly preparing an aerosol surfactant and methanol or glycol according to a certain mass ratio (1: 10), and then injecting a methanol or glycol solution of the aerosol surfactant and liquid carbon dioxide into a high-pressure closed container according to a certain mass ratio (1: 5) to uniformly prepare for later use;
(5) adjusting the temperature of the high-temperature high-pressure reaction kettle to 60 ℃, injecting a certain amount of methanol or glycol solution of the gas-soluble surfactant and liquid carbon dioxide into the high-temperature high-pressure reaction kettle, and adjusting the injection amount to reach the required experimental pressure after the temperature is stable;
(6) adjusting the base to enable the needle head to appear in the visual window, and driving the motor to enable the oil drops to form a downward suspension oil drop on the needle point of the syringe;
(7) input of CO in control system2And the oil drop density, the volume of the oil drop and the dynamic interfacial tension are measured in real time through a data image acquisition system;
(8) increasing the pressure, re-extruding oil drops, repeating the experiment, and measuring the interfacial tension of the carbon dioxide and the crude oil under different pressures;
(9) and obtaining the pressure when the interfacial tension is zero according to a linear extrapolation method, namely the minimum miscible pressure of the carbon dioxide and the crude oil.
The experimental results are as follows:
as shown in FIG. 8, the influence of various alcohol-based auxiliary agents on the miscible pressure of carbon dioxide and crude oil was measured when the polymerization degree of oxyethylene was 9. As can be seen from FIG. 8, methanol has little synergistic effect with two surfactants in the three auxiliary agents, which indicates that methanol can hardly help the two surfactants to dissolve in carbon dioxide, and the minimum miscible pressure reduction amplitude of the system is small; the ethanol and the surfactant have the best synergistic effect, can help the air-soluble surfactant to dissolve in carbon dioxide, and can better act on an oil-gas interface; the glycol and the surfactant have a certain synergistic effect, but the effect is not obvious. Only ethanol in the three adjuvants can produce synergistic effect with two surfactants, and the other two adjuvants are not suitable. Thus, the best results of ethanol with both surfactants are demonstrated by this experiment.
Experimental example 3
The amount of the aerosol surfactant and the ethanol auxiliary agent used by the gas soluble surfactant for reducing the carbon dioxide/crude oil miscible phase pressure is preferably tested:
the experimental conditions are as follows:
(1) simulating the oil reservoir temperature: 60 ℃;
(2) experimental oil: the technical scheme is applicable to crude oil viscosity of less than 100mPa & s under the oil reservoir condition, and the degassed crude oil in the high 89 blocks of the victory oil field is selected in the experimental example, and belongs to typical compact oil reservoir blocks, wherein the crude oil viscosity is 24mPa & s under the oil reservoir condition;
(3) carbon dioxide: the purity is 99.9 percent, and the product is produced by Qingdao Tianyuan gas manufacturing company Limited;
(4) air-soluble surfactant: 2-ethyl-1-hexanol-polyoxypropylene polyoxyethylene ether (fatty alcohol polyoxyethylene polyoxypropylene ether), n-5, m-9 (2 EH-PO)5-EO9) Nonylphenol polyoxyethylene ether, n ═ 9 (NP-9);
(5) the absolute ethyl alcohol is a common commercial product;
(6) Tracker-H type interfacial tensiometer: manufactured by Teclis, France;
purpose of the experiment:
simulating the process that the gas-soluble surfactant is contacted with crude oil after being dissolved and carried into a stratum by supercritical carbon dioxide, measuring the change of the interfacial tension of the carbon dioxide and the crude oil under the action of the gas-soluble surfactant by a pendant drop method, obtaining the minimum miscible phase pressure of the carbon dioxide and the crude oil before and after the gas-soluble surfactant is added by utilizing an interfacial tension disappearance method, and evaluating the influence of the dosage of the gas-soluble surfactant and ethanol on the performance of reducing the minimum miscible phase pressure of the carbon dioxide and the crude oil.
Experimental procedure (experimental flow chart shown in fig. 5):
(1) testing the air tightness of the experimental device by using high-pressure nitrogen;
(2) sequentially cleaning the high-temperature high-pressure reaction kettle, the injection syringe and the straight needle by using acetone, absolute ethyl alcohol and distilled water;
(3) installing the syringe and the needle tube filled with the crude oil on a driving system;
(4) uniformly preparing an aerosol surfactant and absolute ethyl alcohol according to a certain mass ratio, and then injecting an ethanol solution of the aerosol surfactant and liquid carbon dioxide into a high-pressure closed container according to a certain mass ratio to uniformly prepare for later use;
(5) adjusting the temperature of the high-temperature high-pressure reaction kettle to 60 ℃, injecting a certain amount of ethanol solution of the gas-soluble surfactant and liquid carbon dioxide into the high-temperature high-pressure reaction kettle, and adjusting the injection amount to reach the required experimental pressure after the temperature is stable;
(6) adjusting the base to enable the needle head to appear in the visual window, and driving the motor to enable the oil drops to form a downward suspension oil drop on the needle point of the syringe;
(7) input of CO in control system2And the oil drop density, the volume of the oil drop and the dynamic interfacial tension are measured in real time through a data image acquisition system;
(8) increasing the pressure, re-extruding oil drops, repeating the experiment, and measuring the interfacial tension of the carbon dioxide and the crude oil under different pressures;
(9) and obtaining the pressure when the interfacial tension is zero according to a linear extrapolation method, namely the minimum miscible pressure of the carbon dioxide and the crude oil.
The experimental results are as follows:
as shown in Table 1, Table 1 shows MMP and P of carbon dioxide and crude oil in the presence of different surfactants and ethanol contents determined by interfacial tension disappearance methodmax(ii) a The miscible pressure of carbon dioxide and crude oil was measured at different ratios of the addition of the aerosol surfactant to ethanol. As can be seen from Table 1, in the absence of ethanol, only 2EH-PO was added5-EO9Or NP-9 to supercritical carbon dioxide, and although both can be dissolved in supercritical carbon dioxide, the amount of dissolution is low under low pressure conditions, resulting in a high purity by supercritical processingThe interfacial carbon dioxide dissolves less surfactant carried to the gas-liquid interface and has weak ability to lower interfacial tension, so that its effect on MMP is not very significant, but when the pressure is higher, its dissolution amount increases, so that it causes P to be affectedmaxThe influence of (a) is significant. This shows that the two surfactants can only have better solubility in the supercritical carbon dioxide when the injection pressure is higher (generally about 20 MPa), and can only be injected into the formation to reduce the miscible pressure by the dissolution and entrainment of the supercritical carbon dioxide. Therefore, in order to reduce the requirement of the method on injection pressure, the aerosol surfactant and the absolute ethyl alcohol are prepared into an ethanol solution of the aerosol surfactant in a certain mass ratio in advance, so that the injection pressure required for dissolving the surfactant in the carbon dioxide is reduced, and the injection is facilitated.
In addition, it can be seen from table 1 that the addition of ethanol can significantly improve the performance of the surfactant in reducing the miscible pressure, indicating that ethanol can exert a good synergistic effect with the two surfactants. Particularly, when the mass ratio of the surfactant to the ethanol is 1: 10 when the system is added into liquid carbon dioxide when being prepared into ethanol solution of surfactant, and when the system is heated to a supercritical state, MMP and P of carbon dioxide and crude oil can be remarkably reducedmax. Therefore, the ethanol solution (without water) prepared with the aerosol surfactant in advance, which is preferred in the invention, is not a conventional aqueous solution of the aerosol surfactant, and not only is beneficial to dissolving the surfactant in carbon dioxide and is convenient for dissolving, carrying and injecting the carbon dioxide, but also can play a role in reducing the mixed phase pressure of the carbon dioxide and crude oil by the synergy of the ethanol and the surfactant.
TABLE 1
Experimental example 4
Long core displacement experimental study of gas-soluble surfactant to reduce minimum miscible pressure:
the experimental conditions are as follows:
(1) simulating the oil reservoir temperature: 60 ℃;
(2) experimental oil: crude oil degassed in 89 blocks of the Shengli oilfield;
(3) carbon dioxide: the purity is 99.9 percent, and the product is produced by Qingdao Tianyuan gas manufacturing company Limited;
(4) air-soluble surfactant: 2-ethyl-1-hexanol-polyoxypropylene polyoxyethylene ether (fatty alcohol polyoxyethylene polyoxypropylene ether), n-5, m-9 (2 EH-PO)5-EO9) Nonylphenol polyoxyethylene ether, n ═ 9 (NP-9);
(5) core displacement device: and selecting a sand filling pipe with the length of 1000mm and the diameter of 25.4mm to perform a long core displacement experiment to determine the minimum miscible pressure of the system. Compared with the conventional tubule model method, the method has the following advantages: (1) the diameter of the sand filling pipe is larger, sand filling is easier, sand filling can be more uniform and compact, and the porosity of each group of experiment can be similar by sand filling; (2) because of the shorter length, the resistance to fluid flow within the tube is much less; (3) because the internal diameter is great, can directly pour out the grit in the sand-packed pipe, consequently wash easier, guaranteed the cleanliness of sand-packed pipe and shortened the experimental period greatly. Therefore, the minimum miscible pressure of the system is measured by using a long core displacement method in the part.
Purpose of the experiment:
simulating the process that the gas-soluble surfactant is continuously contacted with crude oil in the stratum flowing process after the supercritical carbon dioxide is dissolved and carried into the stratum, and determining the crude oil recovery ratio of the carbon dioxide under different pressures to obtain a pressure-recovery ratio curve by plotting, wherein the pressure at the inflection point of the curve is the minimum miscible pressure of the carbon dioxide and the crude oil determined by the long core displacement method.
Experimental procedure (experimental flow chart shown in fig. 9):
(1) calculating CO required by experiment2Mass according to CO2The ethanol solution of the aerosol surfactant is added into a high-pressure closed container shown in figure 7 according to a certain mass ratio;
(2) then pumping liquid carbon dioxide into the high-pressure closed container shown in FIG. 7, heating and pressurizing the container to convert the container into a supercritical state, and controlling the container to reach the required experimental pressure;
(3) and (6) filling sand. Filling a core tube model with 80-120 meshes of quartz sand, wherein the sand filling process needs a small amount of times, and the core tube is continuously knocked to tightly fill the sand;
(4) vacuumizing and weighing. And vacuumizing the sand filling pipe, and weighing the dry weight of the core pipe after 4 hours.
(5) Saturated water: weighing wet weight of saturated water of the sand-packed pipe model, calculating pore volume, porosity and water permeability, if the permeability is between 1000mD and 1500mD, carrying out the next step, otherwise, repeating the steps (1) and (2);
(6) saturated oil: heating the oil sample to the experimental temperature, and carrying out oil-water displacement by a sand filling pipe of saturated water at the speed of 0.5 mL/min-1Until no water is discharged;
(7) CO injection2Oil displacement: connecting the instruments as shown in FIG. 9, placing in a thermostat, starting the displacement experiment after the experiment temperature is reached, setting the back pressure required by the experiment, opening the valve of the high-pressure closed container and the six-way valve, and keeping the constant injection speed at 0.3 mL/min-1And recording the output oil quantity and the displacement pump reading when 0.05PV is injected, and collecting the pressure of the inlet and the outlet of the long core by a pressure collecting box. Stopping displacement when the accumulated gas injection exceeds 1.2PV pore volume;
(8) cleaning a sand filling pipe: after the displacement experiment is finished, sand is taken out, and the sand filling pipe is cleaned by petroleum ether so as to be used in the next group of experiments.
The experimental results are as follows:
as shown in fig. 10, the cumulative recovery of pure carbon dioxide displacement crude oil under different pressures was measured by using the long core displacement method, and as can be seen from fig. 10, when the pressure is small (15.56MPa, 16.92MPa, 17.82MPa), the ultimate recovery rate increases very quickly, and at this time, miscible phase is not reached, when the pressure is large (19.42MPa, 21.06MPa, 23.74MPa), the ultimate recovery rate can reach 92% at the maximum, and at this time, the oil-gas two-phase miscible phase, the minimum miscible phase pressure of carbon dioxide and crude oil two-phase is at the inflection point, and the minimum miscible phase pressure is 18.36 MPa.
Similarly, the minimum miscible pressures of the carbon dioxide and the crude oil after the addition of the aerosol surfactant are respectively tested according to the method are shown in table 2, and table 2 shows the minimum miscible pressures of the carbon dioxide and the crude oil under different surfactant and ethanol contents determined based on a long core displacement method.
TABLE 2
As can be seen from Table 2, in the absence of ethanol, only 2EH-PO was added5-EO9Or NP-9 is added into supercritical carbon dioxide, and the supercritical carbon dioxide is dissolved and carried with the surfactant to be injected into the rock core, so that the effect of reducing the interfacial tension can be achieved.
2EH-PO was compared with "No. 3" and "No. 6" in Table 25-EO9Or NP-9 and ethanol are not mixed in the early stage, but are respectively added into the supercritical carbon dioxide, and the effect of reducing the minimum miscible pressure is not achieved.
Firstly preparing ethanol solution of surfactant according to a certain mass ratio, then mixing with liquid carbon dioxide, heating and pressurizing to supercritical state, and then 2EH-PO5-EO9The addition of the ethanol solution or the ethanol solution of NP-9 can obviously improve the performance of the surfactant for reducing the miscible pressure, which shows that the ethanol can play a good synergistic effect with the two surfactants. Particularly, when the mass ratio of the surfactant to the ethanol is 1: 10 when preparing ethanol solution of surfactant, adding the system into liquid carbon dioxide, heating to supercritical state, and adding ethanolThe surfactant and the surfactant are cooperated on the interface of the carbon dioxide and the crude oil to reduce the interfacial tension, and the addition of the ethanol can improve the polarization effect of the supercritical carbon dioxide, is beneficial to the supercritical carbon dioxide to extract light components in the crude oil, and can remarkably reduce the minimum miscible pressure of the carbon dioxide and the crude oil; the ethanol related by the invention can not only improve the dissolving amount of the surfactant in the carbon dioxide, but also regulate and control the distribution coefficient of the surfactant in the carbon dioxide and crude oil phases, thereby regulating the migration depth of the surfactant along with the carbon dioxide in the stratum and improving the crude oil recovery ratio of the carbon dioxide.
Example 1
A method for reducing the minimum miscible pressure of carbon dioxide and crude oil based on an aerosol surfactant comprises the following steps:
FIG. 11 is a control flow diagram of a method for reducing minimum miscible pressure of carbon dioxide and crude oil for reservoirs of different depths in which the method of the present embodiment is implemented, comprising: the system comprises a liquid carbon dioxide tank truck 1, a high-pressure storage tank 2, a high-pressure stirring tank 3, ground pumping equipment 4, a heating device 5, an injection well 6, ground pumping equipment 7, an injection well 8, a deep oil reservoir 9 and a shallow oil reservoir 10.
Firstly, mixing a fatty alcohol polyoxyethylene polyoxypropylene ether or nonylphenol polyoxyethylene ether medicament and absolute ethyl alcohol according to a weight part ratio of 1: (10-20) adding the mixture into a high-pressure storage tank 2, and uniformly mixing for later use.
Then, the liquid carbon dioxide in the liquid carbon dioxide tank truck 1 and the prepared fatty alcohol polyoxyethylene polyoxypropylene ether ethanol solution or nonylphenol polyoxyethylene ether ethanol solution in the high-pressure storage tank 2 are injected into a high-pressure stirring tank 3 according to a certain mass ratio and are uniformly mixed for later use. Wherein, when the target oil reservoir is the deep oil reservoir 9, the mixing proportion is as follows: the fatty alcohol polyoxyethylene polyoxypropylene ether ethanol solution or the nonylphenol polyoxyethylene ether ethanol solution and the liquid carbon dioxide are in a mass ratio of 15-25%; when the target oil deposit is a shallow oil deposit 10, the mixing proportion is as follows: the fatty alcohol polyoxyethylene polyoxypropylene ether ethanol solution or the nonylphenol polyoxyethylene ether ethanol solution and the liquid carbon dioxide are in a proportion of 10-20% by mass.
When the target oil reservoir is a deep oil reservoir 9, the fatty alcohol polyoxyethylene polyoxypropylene ether ethanol solution or the nonylphenol polyoxyethylene ether ethanol solution which is prepared in the high-pressure stirring tank 3 and liquid carbon dioxide are injected into the target layer through an injection well 8 by using ground pumping equipment 7, the injected liquid carbon dioxide is gradually changed into a supercritical state in a shaft along with the increase of the injection depth because the burial depth of the deep oil reservoir 9 is more than 1500m, at the moment, the fatty alcohol polyoxyethylene polyoxypropylene ether or the nonylphenol polyoxyethylene ether in the liquid carbon dioxide is dissolved in the supercritical carbon dioxide under the auxiliary action of ethanol, the ethanol and the fatty alcohol polyoxyethylene polyoxypropylene ether or the nonylphenol polyoxyethylene ether are dissolved into a stratum through the supercritical carbon dioxide, and are contacted with crude oil under the good diffusion mass transfer effect of the supercritical carbon dioxide, the dissolution action is generated, the interfacial tension of the carbon dioxide and the crude oil is reduced, and the minimum miscible pressure of the carbon dioxide and the crude oil is further reduced, so that the injected carbon dioxide and the crude oil are easy to form a miscible region, and miscible displacement of reservoir oil is realized.
When the target oil reservoir is a shallow oil reservoir 10, because the buried depth is less than 1500m, liquid carbon dioxide is difficult to be fully heated and converted into a supercritical state in a shaft, so that a surfactant and ethanol cannot be fully dissolved in the shaft, and because the shaft depth is shallow, the pressure required by pumping is small, and the pressure required by construction is easy to realize by ground pumping equipment, aiming at the shallow oil reservoir 10, the fatty alcohol polyoxyethylene polyoxypropylene ether ethanol solution or the nonylphenol polyoxyethylene ether ethanol solution prepared in the high-pressure stirring tank 3 and the liquid carbon dioxide are heated and pressurized on the ground through a heating device 5 by the ground pumping equipment 4, so that the liquid carbon dioxide can be converted into the supercritical state when reaching an injection well 6, and the fatty alcohol polyoxyethylene polyoxypropylene ether or the nonylphenol polyoxyethylene ether in the liquid carbon dioxide is dissolved in the supercritical carbon dioxide under the auxiliary action of ethanol, the supercritical carbon dioxide is dissolved and carries ethanol and fatty alcohol polyoxyethylene polyoxypropylene ether or nonylphenol polyoxyethylene ether to enter a stratum, the ethanol and fatty alcohol polyoxyethylene polyoxypropylene ether or nonylphenol polyoxyethylene ether are contacted with crude oil, the ethanol and fatty alcohol polyoxyethylene polyoxypropylene ether or nonylphenol polyoxyethylene ether are fully contacted with the crude oil under the good diffusion mass transfer effect of the supercritical carbon dioxide, the dissolving effect is generated, the interfacial tension of the carbon dioxide and the crude oil is reduced, the minimum miscible pressure of the carbon dioxide is further reduced, the injected carbon dioxide and the crude oil are easy to form a miscible phase region, and miscible phase oil displacement.
The alcohol solution of the fatty alcohol polyoxyethylene polyoxypropylene ether or the alcohol solution of the nonylphenol polyoxyethylene ether adopted in the embodiment does not contain water, so that the injection capability is strong no matter the alcohol solution is mixed with liquid carbon dioxide for injection or mixed with the liquid carbon dioxide and then heated and pressurized on the ground to form supercritical state injection in the injection process, the injection method is particularly suitable for unconventional oil reservoirs such as ultra-low permeability oil reservoirs and compact oil reservoirs with extremely low permeability, and the defect that a miscible phase pressure system is difficult to inject into a stratum due to the fact that water cannot be injected is avoided. After the system is injected into a stratum, the system can be efficiently and fully contacted with crude oil under the action of good mass transfer diffusion of supercritical carbon dioxide, and the minimum miscible pressure is reduced. The problems of insufficient contact, unobvious change of gas-liquid interface characteristics and the like caused by the existence of a water phase are avoided.
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