CN115386358B - Natural surfactant compound system and preparation method thereof - Google Patents
Natural surfactant compound system and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a natural surfactant compound system and a preparation method thereof, wherein the natural surfactant compound system comprises the following components: choline chloride, citric acid and tea saponin. The compound system provided by the invention can effectively improve the inhibition of hydration expansion of clay minerals, and reduce various complex situations of oil reservoirs to a large extent; the compound system provided by the invention has low interfacial tension, and the prepared compound system can effectively improve the oil displacement efficiency and has obvious depressurization effect; the raw materials are widely available, the preparation process is simple, and the pollution to stratum is avoided.
Description
Technical Field
The invention belongs to the technical field of oil displacement agent preparation, and particularly relates to a natural surfactant compound system and a preparation method thereof.
Background
The low permeability oil reservoir resource occupies an important strategic position in China, and the third oil gas resource investigation result in China shows that the low permeability oil reservoir resource accounts for 49% of the total national resource. The low-permeability sandstone oil reservoir has the characteristics of poor flowing property, high water injection resistance and the like due to extremely poor oil reservoir physical property and higher interfacial resistance effect in a capillary, natural energy in the oil reservoir is insufficient, even if water injection is effective, the injection resistance is increased due to poor oil reservoir physical property, thin pore throat, high interfacial resistance and the like, even water cannot enter the oil reservoir, ground equipment and underground casing pipes can be in a high-pressure state due to high-pressure water injection, the equipment and the underground casing pipes are damaged, stratum is broken due to high pressure, and injection efficiency is reduced. Therefore, long-time high-pressure water injection is not feasible, interface resistance and injection pressure are reduced, the exploration of low-permeability reservoir water injection depressurization and injection increase means is the key for improving the water injection development effect, and the principle of depressurization and injection increase is based on the reduction of interface tension, so that the resistance effect generated by solid-liquid interfaces with more obvious influence on seepage in fine pore throats is less considered.
Surfactant flooding belongs to tertiary oil recovery, and is a chemical oil displacement technology capable of effectively improving the oil reservoir recovery rate by injecting surfactant into stratum to reduce interfacial tension between oil and water so as to achieve the effect of improving the oil reservoir recovery rate, and has wide application in China and abroad, the most common application is anionic surfactant, the least application is cationic surfactant, most of the surfactants in tertiary oil recovery currently use a multi-component compound system, as disclosed in patent CN109207136A, an anionic and cationic surfactant compound system applied to high-mineralization oil reservoir enables the compound system to achieve the interfacial tension (10) -3 mN/m), and as disclosed in patent CN103773346A, a cationic and anionic nonionic surfactant compound system for efficient oil displacementThe interfacial tension of the system can reach ultra-low interfacial tension, and the final recovery ratio is improved by 7.5%. However, the existing surfactants still have more problems such as poor surface activity and unsatisfactory recovery efficiency improvement effect, most of anionic surfactants and inorganic alkali are used together to cause corrosion to stratum, pipeline equipment and the like, and various surfactants for oil displacement have the problems of higher cost and the like.
Deep Eutectic Solvents (DES) are a particular class of solvents, which are mixtures of hydrogen bond donors and hydrogen bond acceptors. The interaction of these two substances results in a liquid with significantly different properties (at a temperature of 23.+ -. 2 ℃) than the composition properties. The main feature of DES is that its melting point is lower than either of its components. Thus, DES is typically a viscous liquid at room temperature, while its components are crystalline solids. Compared with other ionic liquids, the DES is biodegradable and nontoxic, and has the advantages of simple preparation, low price and wide raw material sources. Unlike conventional ionic liquids, DES is easily prepared in pure form. DES are also known as green solvents because of their negligible vapor pressure, nonflammability, low toxicity, electrochemical and thermal stability. DES is a molten salt, and mainly forms a large number of hydrogen bond networks or metal halide interactions through anions of the salt, rather than relying on electrostatic force between anions and cations as in ionic liquids, and has a large number of hydrogen bond networks in DES, which has great potential in inhibiting hydration expansion of clay.
The oil tea saponin is also called as oil tea saponin, is a natural glucoside compound contained in oil tea, is a natural nonionic surfactant extracted from waste materials after oil tea oil extraction, mainly comprises sugar bodies, sapogenin and organic acid, has a hydrophilic-lipophilic balance value (HLB) of 16, has good functions of foaming, foam stabilizing, emulsifying, wetting, solubilizing and the like, has wide raw material sources and extremely low cost, belongs to waste materials, belongs to natural surfactants, is nontoxic and harmless, can be applied to the field of crude oil exploitation, and has limited surface activity, and the effect of efficiently improving the crude oil recovery rate is not enough.
Disclosure of Invention
This section is intended to outline some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. Some simplifications or omissions may be made in this section as well as in the description summary and in the title of the application, to avoid obscuring the purpose of this section, the description summary and the title of the invention, which should not be used to limit the scope of the invention.
The present invention has been made in view of the above and/or problems occurring in the prior art.
Therefore, the invention aims to overcome the defects in the prior art and provide a natural surfactant compound system.
In order to solve the technical problems, the invention provides the following technical scheme: a natural surfactant complex system, which comprises the following components: choline chloride, citric acid and tea saponin.
The invention also aims at a preparation method of the natural surfactant compound system.
In order to solve the technical problems, the invention provides the following technical scheme: a preparation method of a natural surfactant compound system comprises the following steps:
preparing a deep eutectic solvent: mixing choline chloride and citric acid to prepare a deep eutectic solvent;
preparing a composite system: mixing the deep eutectic solvent with the sasanqua saponin, and adding water to obtain a composite system, namely a natural surfactant compound system.
As a preferable scheme of the preparation method of the natural surfactant compound system, the invention comprises the following steps: in the preparation of the natural deep eutectic solvent, choline chloride is prepared according to the molar ratio: citric acid=0.5-2:1.
As a preferable scheme of the preparation method of the natural surfactant compound system, the invention comprises the following steps: in the preparation of the natural deep eutectic solvent, choline chloride is prepared according to the molar ratio: citric acid=1:1.
As a preferable scheme of the preparation method of the natural surfactant compound system, the invention comprises the following steps: in the preparation of the composite system, according to the molar ratio, the deep eutectic solvent: tea saponin=0.5-2:1.
As a preferable scheme of the preparation method of the natural surfactant compound system, the invention comprises the following steps: in the preparation of the composite system, according to the molar ratio, the deep eutectic solvent: tea saponin=1:1.
As a preferable scheme of the preparation method of the natural surfactant compound system, the invention comprises the following steps: in preparing the deep eutectic solvent, choline chloride and citric acid are mixed in a heating environment.
As a preferable scheme of the preparation method of the natural surfactant compound system, the invention comprises the following steps: in the preparation of the deep eutectic solvent, choline chloride and citric acid are stirred and heated for 1 to 3 hours at the temperature of between 60 and 100 ℃.
As a preferable scheme of the preparation method of the natural surfactant compound system, the invention comprises the following steps: in the preparation of the deep eutectic solvent, the choline chloride and the citric acid are stirred and heated at 80 ℃ for 2 hours.
The invention has the beneficial effects that:
1. the compound system provided by the invention can effectively improve the inhibition of hydration expansion of clay minerals, and reduce various complex situations of oil reservoirs to a large extent;
2. the compound system provided by the invention has low interfacial tension, is reduced again on the basis of a natural surfactant, is quite stable in time change, and can still maintain low interfacial tension in a hypersalinity environment;
3. the compound system provided by the invention can effectively improve the oil displacement efficiency and has remarkable depressurization effect;
4. the compound system provided by the invention adopts natural surfactant to compound, belongs to waste material utilization, has wide raw material sources and simple preparation process, and has no pollution to stratum.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the description of the embodiments will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art. Wherein:
FIG. 1 shows the results of experiments for inhibiting the hydration swelling of montmorillonite in different systems in the practice of the invention.
FIG. 2 is an infrared spectrogram of DES, tea saponin and a compound system in the implementation of the invention;
in the figure, the figure a is an infrared spectrum chart of DES, oil tea saponin and a compound system, the figure b is an infrared spectrum chart of DES, the figure c is an infrared spectrum chart of oil tea saponin, and the figure d is an infrared spectrum chart of DES+oil tea saponin compound system;
Detailed Description
In order that the above-recited objects, features and advantages of the present invention will become more apparent, a more particular description of the invention will be rendered by reference to specific embodiments thereof which are illustrated in the appended drawings.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways other than those described herein, and persons skilled in the art will readily appreciate that the present invention is not limited to the specific embodiments disclosed below.
Further, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic can be included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
Example 1
Respectively weighing 0.381g of choline chloride and 0.519g of citric acid, stirring and heating in a constant-temperature water bath kettle at 200r/min for 2 hours at the experimental temperature of 80 ℃ in a molar ratio of 1:1, and uniformly mixing to obtain a Deep Eutectic Solvent (DES);
compounding the prepared DES and the oil tea saponin according to a molar ratio of 1:1, adding 100mL of water, and uniformly and fully stirring to obtain a compound system;
10g of sodium montmorillonite which is sieved by a 200-mesh sieve is weighed, and the sodium montmorillonite is pressed for 10min under 10MPa in a press (YLJ 600 press) to prepare the artificial rock core.
And respectively placing the artificial core in a culture dish of distilled water, 3wt% KCl and 3vol% compound system solution, soaking for 24 hours, completely immersing the surface of the artificial core by the solution, and photographing to record the hydration and expansion conditions of the artificial core in three different solutions at different soaking times.
The photographed picture is recorded in fig. 1.
As can be obtained from FIG. 1, the hydration expansion effects of sodium montmorillonite in different system (distilled water, 3% KCl, 1% compound system) solutions are compared, and on different time nodes, the core soaked by 1% compound system has more obvious expansion inhibition effect, K + Can be embedded into hexagonal holes of sodium-based montmorillonite lattice, and is difficult to exchange, thereby effectively preventing water molecules from entering the hole structure of the montmorillonite and inhibiting hydration expansion of the montmorillonite. Surfactant molecules in the compound system can enter hexagonal holes of sodium-based montmorillonite lattice preferentially and are adsorbed on the surface of the montmorillonite, DES forms a large number of hydrogen bond networks through anions of salt, in addition, the hydrophobicity of the compound system is enhanced, and hydration expansion of the montmorillonite is more effectively inhibited.
Example 2 (oil-water interfacial tension test)
Weighing 0.4g of choline chloride and 0.6g of citric acid respectively, stirring and heating in a constant-temperature water bath at 3000rpm for 2 hours at the experimental temperature of 80 ℃ in a molar ratio of 1:1, uniformly mixing to obtain a Deep Eutectic Solvent (DES), and adding 100mL of distilled water to prepare a DES solution;
weighing 1g of tea saponin, adding 100mL of water, and uniformly and fully stirring to prepare a surfactant solution;
the oil-water interfacial tension of DES and surfactant solution with mass concentration of 1wt% is measured by a rotary drop type interfacial tension meter (JJ 2000B2 of Shanghai middle morning digital technical equipment Co., ltd.) respectively, the rotating speed is 6000r/min, the experimental temperature is 40 ℃, and the experimental oil is crude oil of a certain block of a winning oil field;
weighing 0.127g of choline chloride and 0.173g of citric acid respectively, wherein the molar ratio is 1:1, preparing DES according to the choline chloride and the citric acid and the molar ratio of 1:1, respectively compounding with the sasanqua saponin according to the molar ratio of 2:8, 4:6, 5:5, 6:4 and 8:2, adding 100mL of water to obtain a compound system, and measuring the oil-water interfacial tension of the compound system by using a spinning-drop interfacial tensiometer.
The oil-water interfacial tension of the compound system prepared by DES and oil tea saponin according to different mole ratios measured by a rotary drop interfacial tensiometer is shown in table 1.
As can be obtained from Table 1, experiments show that the DES and the sasanqua saponin with the mass concentration of 1wt% respectively have high oil-water interfacial tension, and the compound system prepared by the DES and the sasanqua saponin in the molar ratio of 5:5 greatly reduces the oil-water interfacial tension, and the minimum reaches 1.12X10 -2 The low interfacial tension of mN/m does not change much with time.
Table 1 results of oil-water interfacial tension test for different systems
Example 3 (salt tolerance test)
Weighing 0.127g of choline chloride and 0.173g of citric acid respectively, stirring and heating for 2 hours in a constant-temperature water bath kettle according to 3000rpm, wherein the experimental temperature is 80 ℃, and uniformly mixing to obtain a Deep Eutectic Solvent (DES);
compounding the prepared DES and the oil tea saponin according to a molar ratio of 1:1, adding 100mL of water, and uniformly and fully stirring to obtain a compound system;
500mg, 1000mg, 1500mg, 2500mg and 4000mg CaCl are respectively added into the compound system 2 Testing the salt tolerance of the compound system to ensure that Ca in each group of compound system 2+ The concentration is 50mg/L, 100mg/L、150mg/L、250mg/L、400mg/L、；
Measuring the CaCl with different amounts by using a rotary drop type interfacial tension meter 2 The oil-water interfacial tension after the process is carried out, the rotating speed is 6000r/min, the experimental temperature is 40 ℃, and the experimental oil is crude oil of a certain block of a victory oil field.
From Table 2, at high concentration of Ca 2+ The lowest interfacial tension of the compound system still has 2.70 multiplied by 10 -2 mN/m, interfacial tension of the complex system with Ca 2+ The increase in concentration did not change much and was very stable over time, showing excellent salt resistance.
Table 2 results of salt tolerance test of the formulated system
Example 4 (wettability test)
Weighing 0.127g of choline chloride and 0.173g of citric acid respectively, stirring and heating for 2 hours in a constant-temperature water bath kettle according to 3000rpm, wherein the experimental temperature is 80 ℃, and uniformly mixing to obtain a Deep Eutectic Solvent (DES);
compounding the prepared DES and the oil tea saponin according to a molar ratio of 1:1, adding 100mL of water, and uniformly and fully stirring to obtain a compound system;
polishing the top end of the core obtained by the experiment through a core planer until the surface is smooth, soaking the core in distilled water for 48 hours, measuring the contact angle of the top end of the core through a fixed drop technology by using a metal injector and recording the contact angle;
and (3) placing the rock core in the prepared compound system, soaking for 48 hours, measuring the contact angle of water and oil phase at the moment, and determining the change of wettability of the compound system on the rock core through the change of the wetting angle.
Experimental results: the experimental results are shown in table 3, and the experiments show that after the core is treated by the compound system, the contact angle of the water phase and the oil phase is increased, the contact angle of the water phase is changed from 7.7 degrees to 64.4 degrees, the hydrophobicity is enhanced, the contact angle of the oil phase is changed from 27.7 degrees to 64.4 degrees, the lipophilicity is weakened, the surfactant is adsorbed on the surface of the core in the compound system, the interfacial property of the surface of the core is effectively changed, the adsorption of the oil drops on the surface of the rock is reduced, the lipophilicity of the core is obviously reduced, and the wettability of the surface of the core is reversed.
Table 3 results of wettability test of the Complex System
| Contact angle of aqueous phase | Oil phase contact angle | |
| Before testing | 47.8° | 27.7° |
| After testing | 53.4° | 64.4° |
Example 5 (Infrared Spectrometry test)
And respectively weighing 0.127g of choline chloride and 0.173g of citric acid, wherein the molar ratio is 1:1, stirring and heating for 2 hours in a constant-temperature water bath kettle, wherein the experimental temperature is 80 ℃, uniformly mixing to obtain a Deep Eutectic Solvent (DES), then adding 0.717g of tea saponin to dissolve the deep eutectic solvent in the DES, uniformly and fully stirring, and the molar ratio of the DES to the tea saponin is 1:1, thus preparing the compound system.
Preparing a sample tablet by using a deep eutectic solvent, oil tea saponin and a +compound system prepared according to the proportion, placing the prepared potassium bromide blank tablet on a sample frame in a sample bin of an infrared spectrometer, determining to acquire a reference background spectrum, taking out the potassium bromide blank tablet after the acquisition of the background spectrum is finished, placing the sample tablet to be detected in the spectrometer, closing a bin cover to obtain an infrared spectrum of the sample, and recording the infrared spectrum of the obtained oil tea saponin, DES and compound system as figure 2.
As can be obtained from FIG. 2, compared with the individual tea saponin, the compound system has a wavelength of 2500cm -1 -3500cm -1 The wide and long-OH telescopic vibration peak appears in the range, which shows that a large amount of hydrogen bonds in DES are added into the compound system, so that the interfacial tension reducing capability of the compound system is greatly improved, and the compound system is also enabled to have the wavelength of 2010cm by adding the DES -1 There is a C.ident.C telescopic vibration peak with wavelength of 1732cm -1 The C=O telescopic vibration peak is arranged at the position, and the wavelength is 1478cm -1 、1409cm -1 Corresponding to C-H in-plane bending vibration peak with wavelength 1196cm -1 Corresponding to C-C telescopic vibration peak with wavelength of 1082cm -1 、955cm -1 The corresponding C-H in-plane bending vibration peak is with wavelength of 1006cm -1 、866cm -1 、783cm -1 The corresponding C-H out-of-plane bending vibration peak is that compared with the single oil tea saponin, the hydrophobicity of the compound system is enhanced, and the inhibition of the water-sensitive expansion of the sodium-based montmorillonite is also enhanced.
Example 6 (Displacement experiment)
And respectively weighing 0.127g of choline chloride and 0.173g of citric acid, wherein the molar ratio is 1:1, stirring and heating for 2 hours in a constant-temperature water bath kettle according to 3000rpm, wherein the experimental temperature is 80 ℃, uniformly mixing to obtain Deep Eutectic Solvent (DES), then adding 0.717g of tea-oil saponin, dissolving the deep eutectic solvent in the DES, uniformly and fully stirring, and the molar ratio of the DES to the tea-oil saponin is 1:1, thus obtaining the compound system.
Saturated distilled water is carried out on a core sample at normal temperature, the pressure of an injection end and an outlet end is monitored in real time, the core before and after the saturated water is weighed, the permeability and the porosity of the core are calculated, then saturated oil is carried out on the core, and basic parameters of experimental cores are shown in table 4;
placing the prepared compound system in a high-pressure container, loading saturated oil into a core holder and connecting the saturated oil to a core displacement device, injecting water to the outlet end for one time until the oil is not discharged any more and the pressure of the inlet end is stable, injecting compound system solution until the pressure is stable, injecting water again until the pressure is stable, recording the pressure of the inlet end and the oil/water output of each displacement stage, and analyzing the pressure reduction and injection increase effects and the recovery ratio improvement condition of the oil/water output.
Experiments on permeability and porosity were performed on cores. The experimental set confining pressure is 20MPa, the back pressure is 3MPa, the experimental temperature is 25 ℃, and the injection speed is 0.05mL/min.
Experimental results: the experimental results are shown in Table 5, and the experiment shows that after the compound system is injected, the injection pressure of the secondary water injection is stable, compared with the injection pressure of the primary water injection, the injection pressure is obviously reduced, the depressurization rate in the core sample 1-1 reaches 17.42%, and the depressurization rate in the core sample 1-2 reaches 19.66%; in the core sample 1-1, the recovery ratio is improved by 5.7% after the compound system is injected, the recovery ratio is improved by 0.5% after the secondary water injection, the final recovery ratio is 42.6%, and in the core sample 1-2, the recovery ratio is improved by 6.5% after the compound system is injected, the recovery ratio is improved by 0.7% after the secondary water injection, the final recovery ratio is 45.4%, and the oil displacement efficiency of the core sample is effectively improved.
Table 4 basic parameters of the core
Table 5 results of stable injection pressure and recovery test at each stage of displacement
It should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted without departing from the spirit and scope of the technical solution of the present invention, which is intended to be covered in the scope of the claims of the present invention.
Claims (4)
1. A preparation method of a natural surfactant compound system is characterized by comprising the following steps: the natural surfactant compound system comprises the following components: choline chloride, citric acid and tea-oil camellia saponin;
the method also comprises the following steps: preparing a deep eutectic solvent: mixing choline chloride and citric acid to prepare a deep eutectic solvent;
preparing a composite system: mixing a deep eutectic solvent and oil tea saponin, and adding water to prepare a compound system, wherein the compound system is a natural surfactant compound system;
in the preparation of the natural deep eutectic solvent, choline chloride is prepared according to the molar ratio: citric acid=0.5-2:1;
in the preparation of the composite system, according to the molar ratio, the deep eutectic solvent: tea saponin=0.5-2:1;
in the preparation of the deep eutectic solvent, choline chloride and citric acid are stirred and heated for 1-3 h at 60-100 ℃.
2. The method for preparing a natural surfactant complex system according to claim 1, characterized in that: in the preparation of the natural deep eutectic solvent, choline chloride is prepared according to the molar ratio: citric acid=1:1.
3. The method for preparing a natural surfactant complex system according to claim 1, characterized in that: in the preparation of the composite system, according to the molar ratio, the deep eutectic solvent: tea saponin=1:1.
4. The method for preparing a natural surfactant complex system according to claim 1, characterized in that: in the preparation of the deep eutectic solvent, choline chloride and citric acid are stirred and heated for 2 hours at 80 ℃.
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| CN1080291A (en) * | 1992-06-26 | 1994-01-05 | 郴州科技实业公司 | From tea waste, extract the method for refined saponin |
| CN1616480A (en) * | 2004-08-28 | 2005-05-18 | 王元华 | Method for producing dioscin by directly extracting saponin without pollution |
| CN104694103A (en) * | 2013-12-09 | 2015-06-10 | 青岛惠城石化科技有限公司 | Surfactant compounded system with oil reservoir adaptability |
| CN105154051A (en) * | 2015-09-25 | 2015-12-16 | 中国石油天然气股份有限公司 | Pressure-reducing injection-increasing surfactant compound composition and preparation method and application thereof |
| CN109054796A (en) * | 2018-08-22 | 2018-12-21 | 东营利丰化工新材料有限公司 | A kind of high efficiency composition oil displacement agent and preparation method thereof |
| CN111849444A (en) * | 2020-06-24 | 2020-10-30 | 中国石油天然气股份有限公司 | Ultra-low permeability oil reservoir pressure-reducing and injection-increasing system and preparation method thereof |
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- 2022-06-30 CN CN202210771013.3A patent/CN115386358B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1080291A (en) * | 1992-06-26 | 1994-01-05 | 郴州科技实业公司 | From tea waste, extract the method for refined saponin |
| CN1616480A (en) * | 2004-08-28 | 2005-05-18 | 王元华 | Method for producing dioscin by directly extracting saponin without pollution |
| CN104694103A (en) * | 2013-12-09 | 2015-06-10 | 青岛惠城石化科技有限公司 | Surfactant compounded system with oil reservoir adaptability |
| CN105154051A (en) * | 2015-09-25 | 2015-12-16 | 中国石油天然气股份有限公司 | Pressure-reducing injection-increasing surfactant compound composition and preparation method and application thereof |
| CN109054796A (en) * | 2018-08-22 | 2018-12-21 | 东营利丰化工新材料有限公司 | A kind of high efficiency composition oil displacement agent and preparation method thereof |
| CN111849444A (en) * | 2020-06-24 | 2020-10-30 | 中国石油天然气股份有限公司 | Ultra-low permeability oil reservoir pressure-reducing and injection-increasing system and preparation method thereof |
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