CN112480895A - PH-responsive oil displacement agent composition, oil displacement agent, and preparation method and application thereof - Google Patents
PH-responsive oil displacement agent composition, oil displacement agent, and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a pH response type oil displacement agent composition, an oil displacement agent, and a preparation method and application thereof. The oil displacement agent composition comprises chitosan and a surfactant; the mass ratio of the two is (5-8): (2-5). The oil displacement agent comprises chitosan, a surfactant, a pH regulator and water; the mass ratio of the chitosan to the surfactant is (5-8): (2-5); the total mass of the chitosan and the surfactant accounts for 0.05-0.15 wt% of the mass concentration of the total oil displacement agent; the pH value of the oil displacement agent is 6.33-6.58. By compounding chitosan and a surfactant, the prepared emulsion-shaped oil displacement agent can show certain pH responsiveness and can realize the regulation and control of 'emulsification-demulsification'; the oil displacement agent has excellent stability and viscoelasticity when the pH value is 6.33-6.58, has a better oil displacement effect when being applied to oil extraction in an oil field, and can further improve the recovery ratio of crude oil on the basis of water flooding.
Description
Technical Field
The invention belongs to the technical field of oil extraction in oil fields, and relates to a pH response type oil displacement agent composition, an oil displacement agent, and a preparation method and application thereof.
Background
With the improvement of the refinement degree of oil field development, the emulsion is widely applied in the field of oil field development. A large number of indoor experiments and mine field applications show that the produced liquid has good emulsification effect and better effect of improving the recovery ratio, because the emulsion plays a dual role in oil displacement and profile control in the stratum migration process.
The problems of difficult demulsification and incapability of recycling the emulsifier exist in the current emulsion oil-displacing process, and the physical and chemical properties of the emulsifier are found to be along with the external environmental conditions (such as pH, temperature, light and CO) by researching the emulsifier with environmental stimulus responsiveness2/N2Magnetic field, ions, etc.) and the properties of the emulsifier can be regulated and controlled by adjusting external environmental factors, thereby realizing the rapid and controllable intelligent conversion of the emulsion between emulsification and emulsion breaking.
Aiming at the problems that emulsion breaking is difficult and an emulsifier cannot be recycled all the time in the emulsion oil displacement process, a displacement system with pH response behavior is needed to be provided, so that efficient and environment-friendly development of an oil field is realized.
Disclosure of Invention
Based on the technical problems in the prior art, the first purpose of the invention is to provide an oil displacement agent composition, the oil displacement agent composition adopts the compounding of chitosan and a surfactant, and the prepared emulsion-shaped oil displacement agent can show certain pH responsiveness and can realize the regulation and control of 'emulsification-demulsification'; the second purpose of the invention is to provide an oil displacement agent, wherein the pH value of the oil displacement agent is 6.33-6.58, and the oil displacement agent has excellent stability and viscoelasticity; the third purpose of the invention is to provide a preparation method of the oil displacement agent; the fourth purpose of the invention is to provide the application of the oil displacement agent composition in oil recovery in oil fields; the fifth purpose of the invention is to provide the application of the oil displacement agent in oil recovery in oil fields, which has better oil displacement effect and can further improve the recovery ratio of crude oil on the basis of water flooding.
The purpose of the invention is realized by the following technical scheme:
in one aspect, the present invention provides an oil-displacing agent composition comprising chitosan and a surfactant;
the mass ratio of the chitosan to the surfactant is (5-8): (2-5).
In the above oil-displacing agent composition, preferably, the surfactant includes one or more of alkyl glycoside (APG), Sodium Dodecyl Sulfate (SDS), and dodecyl dimethyl betaine (BS12), but is not limited thereto.
In another aspect, the present invention also provides an oil-displacing agent comprising chitosan, a surfactant, a pH adjuster, and water;
the mass ratio of the chitosan to the surfactant is (5-8): (2-5);
the total mass of the chitosan and the surfactant accounts for 0.05-0.15 wt% of the mass concentration of the total oil displacement agent;
the pH value of the oil displacement agent is 6.33-6.58.
In the oil displacement agent, preferably, the pH adjuster includes an acid or an alkali; the acid includes hydrochloric acid, but is not limited thereto; the base includes sodium hydroxide, but is not limited thereto.
In the oil-displacing agent, the oil-displacing agent is preferably composed of chitosan, alkyl glycoside, a pH regulator and water;
the mass ratio of the chitosan to the alkyl glycoside is 4: 1;
the total mass of the chitosan and the alkyl glycoside accounts for 0.1 wt% of the mass concentration of the total oil displacement agent;
the pH value of the oil displacement agent is 6.33.
In the oil displacement agent, preferably, the oil displacement agent consists of chitosan, sodium dodecyl sulfate, a pH regulator and water;
the mass ratio of the chitosan to the sodium dodecyl sulfate is 4: 1;
the total mass of the chitosan and the lauryl sodium sulfate accounts for 0.1 wt% of the mass concentration of the total oil displacement agent;
the pH value of the oil displacement agent is 6.33.
In the oil displacement agent, preferably, the oil displacement agent consists of chitosan, dodecyl dimethyl betaine, a pH regulator and water;
the mass ratio of the chitosan to the dodecyl dimethyl betaine is 4: 1;
the total mass of the chitosan and the dodecyl dimethyl betaine accounts for 0.1 wt% of the mass concentration of the total oil displacement agent;
the pH value of the oil displacement agent is 6.33.
In another aspect, the present invention further provides a preparation method of the oil displacement agent, including:
dissolving a surfactant in water according to a ratio, adding chitosan, stirring and dissolving, and finally adjusting the pH value of the solution to 6.33-6.58 by using a pH regulator to obtain the oil-displacing agent.
In another aspect, the invention also provides application of the oil displacement agent composition in oil recovery in oil fields.
In another aspect, the invention also provides application of the oil displacement agent in oil recovery in an oil field.
The invention has the beneficial effects that:
(1) in the oil displacement agent, emulsions stabilized by three chitosan/surfactant compound systems show certain pH responsiveness. In the preferred operation of the invention, the emulsion stabilized by chitosan/APG 1214 and chitosan/BS 12 compounded oil displacement agent shows the best stability at the pH value of 6.33; in contrast, the emulsion stabilized by this pH of 1.51 was the least stable. Therefore, the emulsion liquid stabilized by the chitosan/APG 1214 and chitosan/BS 12 compounded oil displacement agent has good pH responsiveness, and the regulation and control of emulsification-demulsification can be realized by adjusting the pH value of the oil displacement agent system.
(2) In the embodiment of the invention, the optimal chitosan/surfactant oil displacement agent is chitosan/APG 1214; the compounding mass ratio of the three pH response type compound oil displacement agents is 8: 2; when the pH values of the chitosan/APG 1214, chitosan/SDS and chitosan/BS 12 compound oil displacement agents are 6.33, 6.58 and 6.33 respectively, the emulsion stability is the best, and the viscoelasticity is also the best; and the optimum concentration of the system is preferably 0.1 wt%.
(3) The oil displacement agent disclosed by the invention has a good physical simulation oil displacement effect, and can further improve the crude oil recovery rate after the conventional water displacement is physically simulated in a rock core. In the preferred implementation operation of the invention, the oil displacement agent with the weight ratio of 8:2 of chitosan to APG1214 when the pH value is 6.33 has the best oil displacement effect, and the recovery ratio is further improved to 19.35% on the basis of water displacement.
Drawings
Fig. 1 is a comparison graph of interfacial tension of oil displacement agent compounded by chitosan and APG1214 and crude oil in different compounding mass ratios in example 1 of the present invention.
FIG. 2 is a comparison graph of TSI (time dependent chemical ionization) curves of oil displacement agents compounded by chitosan and APG1214 at a mass ratio of 8:2 under different pH values in example 1 of the invention.
FIG. 3 is a chart comparing the stability of chitosan and different surfactants in different formulation mass ratios in example 3 of the present invention.
FIG. 4 is a graph of the change of oil recovery rate with injected pore volume for core displacement experiment of chitosan/APG 1214 oil displacing agent with pH 6.33 in example 5 of the present invention.
Detailed Description
The technical solutions of the present invention will be described in detail below in order to clearly understand the technical features, objects, and advantages of the present invention, but the present invention is not limited to the practical scope of the present invention. The chitosan and the surfactant used in the examples are all commercially available and conventional in the art.
Example 1:
the embodiment provides a series of pH response type oil displacement agents and a preparation method thereof, and the preparation method specifically comprises the following steps:
dissolving certain amounts of APG1214, SDS and BS12 in water respectively, stirring by using a magnetic stirrer until the solutions are completely dissolved, adding chitosan respectively until the solutions are dissolved, compounding the chitosan with three surfactants according to different mass ratios, wherein the compounding mass ratio is 8:2, 6:4, 5:5, 4:6 and 2:8, and adjusting the pH value of a solution system to be in the range of 1.51-6.58 by hydrochloric acid or sodium hydroxide, for example: the pH value is 1.51, 4.40, 5.93, 6.33 and 6.58, and the total mass of the chitosan and the surfactant accounts for 0.1 wt% of the mass concentration of the total oil displacement agent.
Interfacial tension measurements were performed on a series of oil displacing agents prepared in this example. The interfacial tension of the oil displacement agent and the crude oil at different compounding ratios and pH values was measured at 45 ℃ by using a TX-500C (Bowing Industry Corp., USA) rotary droplet interfacial tensiometer (rotating speed of 6000r/min, measuring time of 40min, taking one point every 1 min), and the results are shown in FIG. 1. FIG. 1 shows the interfacial tension of the chitosan and APG1214 in different formulation mass ratios without adjusting the pH value, and it can be seen from FIG. 1 that the interfacial tension of the formulation system increases and then decreases with the increase of the proportion of the APG1214, and the interfacial tension is the lowest when the proportion of the chitosan and the APG1214 is 8:2 (i.e., 4: 1).
10mL of oil displacement agents with different pH values and 10mL of crude oil are sequentially added into an emulsion bottle, and are emulsified and dispersed for 2min by an IKA T18 digital ULTRA RURRAX dispersion machine (IKA company, Germany) at the rotating speed of 3000 r/min. Emulsion stability analysis was performed on a series of oil displacing agents prepared in this example. The optical analysis of the emulsion was measured using a Turbiscan Lab Expert stability Analyzer (formulation, France) with a total scan time of 2h and a scan interval of 5min for the scanning program, the results of which are shown in FIG. 2. FIG. 2 is a comparison graph of TSI (time dependent chemical index) change curves of oil displacement agents compounded by chitosan and APG1214 according to the mass ratio of 8:2 at different pH values.
As can be seen from fig. 2: the TSI curve of the chitosan/APG 1214 oil-displacing agent stabilized emulsion with different pH values is firstly reduced and then increased, which shows that the stability of the emulsion is also firstly enhanced and then weakened. The TSI curves at pH 5.93 and 6.33 were both low, with the curve at pH 5.93 rising slowly in the initial period but always tending to rise, and at 5500s exceeding the curve at pH 6.33. The curve with pH 6.33 increased faster in the initial stage and remained substantially constant in the later stage. Taken together, the emulsion formed with the chitosan/APG 1214 oil-displacing agent having a pH of 6.33 exhibited the best long-term stability.
Example 2:
this example discusses the effect of changes in chitosan concentration in oil-displacing agents that have no surfactant added but chitosan on the stability and permeability of the oil-displacing agent. The results of the experiment are shown in table 1 below:
table 1:
as can be seen from the experimental data in table 1: as the concentration of chitosan is increased, the system stability becomes worse. Under acidic conditions, the amino group (NH) in the chitosan molecule2) Capable of undergoing protonation to NH3 +So that strong intermolecular electrostatic repulsion exists, and molecules are not easy to coalesce. NH with increasing pH3 +Begin to deprotonate and convert to amino (NH)2) The electrostatic repulsion between molecules is weakened and the aggregation of molecules is continuously generated.
It is found that the emulsifying capacity of the emulsion is increased and then reduced with the increasing concentration. This is because the decrease in oil droplet size is promoted with the increase in chitosan concentration, but with further increase in chitosan concentration, the intramolecular and intermolecular interactions are enhanced due to the stronger electrostatic force, thereby reducing the probability of sufficient interaction of chitosan with the oil phase.
Example 3:
the embodiment discusses the influence of the change of different compounding ratios of chitosan and different surfactants in the oil displacement agent on the stability and the transmittance of the oil displacement agent, and the pH value of the oil displacement agent is not adjusted in the process. The results of the experiment are shown in FIG. 3.
FIG. 3 is a photograph of different formulation ratios of chitosan and APG1214 at the time of formulation (a) and after standing for two days (b); FIG. 3 is a photograph showing different ratios of chitosan to SDS as formulated (a) and after standing for two days (b); FIG. 3, III, is a photograph of different formulation ratios of chitosan and BS12 at the time of formulation (a) and after standing for two days (b).
As can be seen from fig. 3: (1) the interfacial tension of the compounded system is increased and then reduced along with the increase of the proportion of the APG1214, and the interfacial tension is lowest when the proportion of the chitosan/APG 1214 is 8: 2. Therefore, the compounding ratio of chitosan/APG is set as 8: 2. (2) As the proportion of SDS increases, the degree of coagulation gradually increases, and a large amount of flocs are separated out. Since chitosan is a cationic bio-polyelectrolyte, for oppositely charged polyelectrolyte/surfactant systems, the driving force for intermolecular assembly is the entropy increase due to the release of counterions and water molecules, which can produce large amounts of insoluble complexes at equimolar charge. In the case of chitosan alone in solution, the addition of SDS molecules first forms a water soluble electrostatic complex until a critical concentration, known as the Critical Aggregation Concentration (CAC), is reached. At concentrations above the CAC, water-insoluble complexes begin to form in large quantities and cause phase separation. The concentration of SDS is further increased and the chitosan/SDS-insoluble complex can be gradually re-solubilized again by the formation of anionic species. (3) Along with the increase of the proportion of the surfactant BS-12, the interfacial tension of the compound system is gradually reduced. The chitosan molecular chain is continuously expanded in the solution, and hydrophobic effect is generated between chitosan molecules and between chitosan-surfactant. If the concentration of the surfactant is increased, hydrophobic interaction between the hydrophobic chains of the surfactant and the hydrophobic regions of the chitosan macromolecules occurs through hydrophobic effect, the hydrophobic regions of the chitosan are converted into hydrophilic regions, and further expansion of the chitosan molecules is caused.
Example 4:
this example discusses the effect of pH response range on oil displacement agent stability, permeability and particle size. Wherein the compounding mass ratio of the chitosan to the surfactant is 8:2, the total mass of the chitosan and the surfactant accounts for 0.1 wt% of the mass concentration of the total oil displacement agent, and the experimental results are shown in the following tables 2 and 3:
table 2:
table 3:
as can be seen from tables 2 and 3:
firstly, the phenomena of three systems are divided into three stages to summarize the stability of the systems; reason analysis of the chitosan/SDS oil displacement agent: the effect on the polyelectrolyte adsorbing layer depends mainly on the molecular structure of the polyelectrolyte. Under a lower pH value, the charge of chitosan molecules is higher, the flexibility of the molecular coil is stronger, so that the SDS micelle can be fully combined with the flexible molecular chain of the chitosan under the electrostatic action to form a highly structured complex. With the increase of pH, the electrostatic repulsion between chitosan molecules is reduced, the rigidity of molecular random coils is stronger, SDS can be adsorbed only at the top end of the rigid molecular chain, the two cannot be fully combined, and the aggregation degree of the formed composite complex is not high. At the same time, the degree of association between chitosan molecular chains is increased, and insoluble aggregates are also formed.
Secondly, summarizing transmittance images of the three systems; in order to further study the change of the association degree of the compound system with the pH value, the light transmittance change of the compound system with different pH values is evaluated.
Secondly, summarizing particle size results of the three systems; in the presence of a surfactant, the properties of the chitosan aqueous solution can be changed remarkably, and the particle size distribution of the chitosan/APG 1214 compound system with different pH values is evaluated.
Finally, the three systems have good stability at pH values of 6.33, 6.58 and 6.33, respectively.
Example 5:
in the embodiment, pH response performance of emulsification-demulsification regulation and control of the oil displacement agent prepared by compounding chitosan and three surfactants is investigated, the adopted oil phase is liquid paraffin, the compounding mass ratio of the chitosan to the surfactants is 8:2, and the total mass of the chitosan and the surfactants accounts for 0.1 wt% of the mass concentration of the total oil displacement agent; the results of the experiment are shown in table 4:
table 4:
as can be seen from the experimental data in table 4: the oil displacement agent compounded by chitosan and APG1214 and the oil displacement agent compounded by chitosan and BS12 have the largest difference of emulsion stability when the pH value is 1.51 and the pH value is 6.33, so that better regulation and control of emulsification-demulsification can be realized, and the pH responsiveness is good.
Example 6:
the embodiment provides an application of an oil displacement agent compounded by chitosan and three surfactants in oil field oil extraction, wherein the compounding mass ratio of the chitosan to the surfactants is 8:2, and the total mass of the chitosan and the surfactants accounts for 0.1 wt% of the total mass concentration of the oil displacement agent, and the application is as follows:
a simulated formation water having a degree of mineralization of 6276mg/L was used, and the specific ionic composition thereof is shown in Table 5.
Table 5:
core displacement enhanced recovery experiment:
core displacement experiments were performed using a natural outcrop core (average cross-sectional diameter of 2.5 cm; length of about 10 cm; average permeability of 100 mD). Injecting the simulated formation water into the rock core at the flow rate of 0.1mL/min to saturate crude oil; and monitoring the oil output, the liquid output and the pressure change until the water content of the produced liquid reaches more than 98 percent. And performing water flooding, chemical flooding and water flooding, wherein the experimental results are shown in table 6 and fig. 4, and fig. 4 is a graph showing the change of the recovery rate of the crude oil in the core displacement experiment of the oil displacement agent with the pH value of 6.33 and the pH value of APG 1214.
Table 6:
as can be seen from table 6: the chitosan system with the pH value of 6.33 has good response performance and also has good oil increasing effect, and the effect of increasing the recovery ratio reaches 12.57%. Compared with a single chitosan system, the compound system has improved recovery efficiency, wherein the chitosan/APG 1214 oil displacement agent has the most obvious synergy effect which reaches 19.35%; secondly, 18.74 percent of chitosan/BS 12 oil displacement agent; the minimum is 13.62 percent of the chitosan/SDS oil displacement agent.
Claims (10)
1. An oil-displacing agent composition comprising chitosan and a surfactant;
the mass ratio of the chitosan to the surfactant is (5-8): (2-5).
2. The oil-displacing agent composition of claim 1, wherein the surfactant comprises one or more of an alkyl glycoside, sodium lauryl sulfate, and dodecyl dimethyl betaine.
3. An oil displacement agent, which comprises chitosan, a surfactant, a pH regulator and water;
the mass ratio of the chitosan to the surfactant is (5-8): (2-5);
the total mass of the chitosan and the surfactant accounts for 0.05-0.15 wt% of the mass concentration of the total oil displacement agent;
the pH value of the oil displacement agent is 6.33-6.58.
4. The oil-displacing agent according to claim 3, wherein the pH-adjusting agent comprises an acid or a base; the acid comprises hydrochloric acid; the base comprises sodium hydroxide.
5. The oil-displacing agent according to claim 3 or 4, wherein the oil-displacing agent consists of chitosan, an alkyl glycoside, a pH adjusting agent, and water;
the mass ratio of the chitosan to the alkyl glycoside is 4: 1;
the total mass of the chitosan and the alkyl glycoside accounts for 0.1 wt% of the mass concentration of the total oil displacement agent;
the pH value of the oil displacement agent is 6.33.
6. The oil-displacing agent according to claim 3 or 4, wherein the oil-displacing agent consists of chitosan, sodium lauryl sulfate, a pH regulator and water;
the mass ratio of the chitosan to the sodium dodecyl sulfate is 4: 1;
the total mass of the chitosan and the lauryl sodium sulfate accounts for 0.1 wt% of the mass concentration of the total oil displacement agent;
the pH value of the oil displacement agent is 6.33.
7. The oil-displacing agent according to claim 3 or 4, wherein the oil-displacing agent consists of chitosan, dodecyl dimethyl betaine, a pH regulator, and water;
the mass ratio of the chitosan to the dodecyl dimethyl betaine is 4: 1;
the total mass of the chitosan and the dodecyl dimethyl betaine accounts for 0.1 wt% of the mass concentration of the total oil displacement agent;
the pH value of the oil displacement agent is 6.33.
8. A method for preparing an oil-displacing agent as claimed in any one of claims 3 to 7, which comprises:
dissolving a surfactant in water according to a ratio, adding chitosan, stirring and dissolving, and finally adjusting the pH value of the solution to 6.33-6.58 by using a pH regulator to obtain the oil-displacing agent.
9. Use of an oil-displacing agent composition according to claim 1 or 2 in oil recovery in oil fields.
10. Use of the oil displacement agent of any one of claims 3 to 7 in oil recovery in oil fields.
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