CN110760298B - Surfactant-free microemulsion and preparation method thereof - Google Patents

Surfactant-free microemulsion and preparation method thereof Download PDF

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CN110760298B
CN110760298B CN201911012017.8A CN201911012017A CN110760298B CN 110760298 B CN110760298 B CN 110760298B CN 201911012017 A CN201911012017 A CN 201911012017A CN 110760298 B CN110760298 B CN 110760298B
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microemulsion
surfactant
butanol
mixed
oil phase
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CN110760298A (en
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刘雪婧
耿铁
赵春花
孙强
刘刚
罗健生
丁玉
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China Oilfield Services Ltd
China National Offshore Oil Corp CNOOC
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Abstract

The invention provides a surfactant-free microemulsion and a preparation method thereof. The surfactant-free microemulsion comprises an oil phase, a water phase and a mixed amphiphilic solvent; the mixed amphiphilic solvent is a mixed solution consisting of butanol which can be mixed and dissolved with oil phase and ethanol which can be mixed and dissolved with water phase. The volume ratio of the oil phase to the water phase is 9: 1-1: 9. The preparation method of the microemulsion is simple and convenient, the oil phase, the water phase and the mixed amphiphilic solvent are mixed according to a certain proportion at room temperature, and the microemulsion is obtained by uniformly stirring and is easy for industrial implementation. The microemulsion of the invention can be used in the fields of oilfield development, daily chemical industry, functional material preparation, drug carriers, pesticide preparations and the like.

Description

Surfactant-free microemulsion and preparation method thereof
Technical Field
The present invention relates to colloid material technology, and is especially one kind of surfactant-free microemulsion formed with mixed amphiphilic solvent and its preparation process.
Background
Microemulsions (microemulsions) are liquid/liquid colloidal dispersion systems, originally discovered by hoor and Schulman in 1943, and Schulman et al, 1959, proposed the concept "microemulsions" for describing such systems. The general definition of microemulsion is now: thermodynamically stable, isotropic, transparent dispersions of at least two mutually incompatible liquids (often referred to as oil and water phases) and a surfactant. The surfactant has both hydrophilic group and lipophilic group in its molecule, and has amphiphilic structure to form ordered molecular film in the oil/water interface and thus to stabilize the micro emulsion system. The microemulsion (SBMEs) based on the surfactant is widely applied to the fields of oilfield development, daily chemical industry, functional material preparation, drug carriers and the like, and is concerned.
Since the microemulsion systems reported in the research are basically formed in the presence of surfactants and even cosurfactants (mostly short-chain alcohols), the surfactants have long been considered as indispensable components of the microemulsions. Smith et al discovered in 1977 that microemulsions could be formed in the hexane-water-isopropanol ternary system, indicating that surfactants were not an essential component of microemulsions. Subsequent extensive studies have demonstrated that microemulsions can be formed in a ternary system consisting of an oil phase, an aqueous phase and an "amphiphilic solvent" (e.g. isopropanol) in the absence of surfactants. By "amphiphilic solvent" is meant a solvent that is miscible with both the oil phase and the water phase; it has no traditional surface activity and no ordered molecular film formed at the oil/water interface. This microemulsion, formed from an oil phase, an aqueous phase and an amphiphilic solvent in the absence of a surfactant, is called a "surfactant-free microemulsions" (SFMEs). Similar to SBMEs, SFMEs also have wide application prospects in the fields of oilfield development, daily chemical industry, functional material preparation, drug carriers and the like. In particular, SFMEs are more advantageous in application, and can avoid the defects of high cost, high toxicity, difficult product purification in the preparation of functional materials and the like caused by the fact that an SBMEs system contains a large amount of surfactant (generally more than 10 wt%).
Disclosure of Invention
In order to overcome the defects of the prior art, the invention discloses a surfactant-free microemulsion formed by mixing amphiphilic solvents. The microemulsion disclosed by the invention is formed by mixing an oil phase, a water phase and a mixed amphiphilic solvent, and does not contain a traditional surfactant;
the application provides a surfactant-free microemulsion and a preparation method thereof. The surfactant-free microemulsion comprises an oil phase, a water phase and a mixed amphiphilic solvent;
wherein the amphiphilic solvent is a mixed solution of butanol and ethanol;
the ratio of the volume of the mixed amphiphilic solvent to the total volume of the oil phase and the water phase is (1.5:1) - (9: 1).
In the surfactant-free microemulsion provided by the invention, the volume ratio of the oil phase to the water phase is (9:1) - (1: 9).
In the surfactant-free microemulsion provided by the invention, the volume ratio of butanol to ethanol in the mixed amphiphilic solvent is (6:1) - (1: 3).
Preferably, the volume ratio of butanol to ethanol in the mixed amphiphilic solvent is (4:1) - (2: 1).
In the surfactant-free microemulsion provided by the invention, the volume ratio of the oil phase, the water phase and the amphiphilic solvent (namely butanol and ethanol) is as follows: 1:3:8:8 or 5:5:24:6 or 2:1:12.75: 4.25.
In the surfactant-free microemulsion provided by the invention, the butanol is selected from one or more of n-butanol, isobutanol, sec-butanol and tert-butanol.
In the surfactant-free microemulsion provided by the invention, the oil phase is alkane with a carbon chain length of 10-18;
preferably, the oil phase is selected from one or more of dodecane, pentadecane and a gas oil.
In the surfactant-free microemulsion provided by the invention, the carbon number of the gassed oil is 12-18, preferably 12-15.
In the surfactant-free microemulsion provided by the invention, the water phase is pure water or an aqueous solution of inorganic salt.
In the surfactant-free microemulsion provided by the invention, the aqueous solution of the inorganic salt is selected from NaCl, KCl and MgCl2、CaCl2、NaNO3、KNO3、Mg(NO3)2、Ca(NO3)2、Na2SO4、K2SO4And MgSO4One or more anhydrous organic salt aqueous solutions;
preferably, the concentration of the aqueous inorganic salt solution is not higher than the saturation concentration of the inorganic salt.
In the surfactant-free microemulsion provided by the invention, the surfactant-free microemulsion is a uniform and transparent system and is stable within the temperature range of-10-95 ℃.
The novel surfactant-free microemulsion can be used in the fields of oilfield development (such as drilling fluid and enhanced oil displacement system), daily chemical industry, preparation of functional materials, drug carriers, pesticide preparations and the like.
On the other hand, the preparation method of the surfactant-free microemulsion comprises the following steps: mixing the oil phase, the water phase and the mixed amphiphilic solvent according to the proportion at room temperature, and stirring uniformly. The preparation method has the advantages of simple process, mild conditions, no need of special equipment, low energy consumption, low cost and easy industrial implementation.
Compared with the prior art, the invention has the technical characteristics that:
1. the microemulsion is prepared by adopting a mixed amphiphilic solvent consisting of a lipophilic solvent and a hydrophilic solvent, so that the number of SFMEs systems is greatly expanded;
2. the microemulsion has good stability and wide temperature resistance range, and is stable in the temperature range of-10 to 95 ℃;
3. the microemulsion of the invention does not contain surfactant, has more advantages than the conventional surfactant microemulsion in some applications, and can avoid the problems of high cost, high toxicity, difficult product purification (such as during the preparation of nano materials) and the like caused by the existence of the surfactant;
4. the preparation method is simple, low in energy consumption and cost and easy for industrial implementation.
Additional features and advantages of the application will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by the practice of the application. Other advantages of the application may be realized and attained by the instrumentalities and combinations particularly pointed out in the specification, claims, and drawings.
Drawings
The accompanying drawings are included to provide an understanding of the present disclosure and are incorporated in and constitute a part of this specification, illustrate embodiments of the disclosure and together with the examples serve to explain the principles of the disclosure and not to limit the disclosure.
Figure 1 is a photograph of the appearance of a sample of the microemulsion prepared in example 1.
Figure 2 is a plot of the particle size distribution of the microemulsion samples prepared in example 1.
FIG. 3 is a scanning electron micrograph of a sample of the microemulsion prepared in example 1 by freeze etching.
Detailed Description
The following examples are intended to illustrate and explain the present invention in more detail and to make the contents of the invention more visually understandable, but the present invention is not limited to the following examples.
The embodiment of the application provides a surfactant-free microemulsion and a preparation method thereof. The surfactant-free microemulsion comprises an oil phase, a water phase and a mixed amphiphilic solvent;
wherein the amphiphilic solvent is a mixed solution of butanol and ethanol;
the ratio of the volume of the mixed amphiphilic solvent to the total volume of the oil phase and the water phase is (1.5:1) - (9: 1).
In the surfactant-free microemulsion provided by the invention, the volume ratio of the oil phase to the water phase is (9:1) - (1: 9).
In the embodiment of the invention, the volume ratio of butanol to ethanol in the mixed amphiphilic solvent is (6:1) - (1: 3).
Preferably, the volume ratio of butanol to ethanol in the mixed amphiphilic solvent is (4:1) - (2: 1).
In an embodiment of the present invention, the butanol is selected from one or more of n-butanol, iso-butanol, sec-butanol, tert-butanol.
In the embodiment of the invention, the oil phase is alkane with a carbon chain length of 10-18;
preferably, the oil phase is selected from one or more of dodecane, pentadecane and a gas oil.
In the embodiment of the invention, the carbon number of the gassed oil is 12-18, preferably 12-15.
In an embodiment of the invention, the aqueous phase is pure water or an aqueous solution of an inorganic salt.
In an embodiment of the invention, the aqueous inorganic salt solution is selected from NaCl, KCl, MgCl2、CaCl2、NaNO3、KNO3、Mg(NO3)2、Ca(NO3)2、Na2SO4、K2SO4And MgSO4One or more inorganic salt aqueous solutions of (a);
preferably, the concentration of the aqueous inorganic salt solution is not higher than the saturation concentration of the inorganic salt.
In the embodiment of the invention, the surfactant-free microemulsion is a uniform and transparent system and is stable within the temperature range of-10 to 95 ℃.
In the embodiment of the present invention, the preparation method of the surfactant-free microemulsion comprises: mixing the oil phase, the water phase and the mixed amphiphilic solvent according to the proportion at room temperature, and stirring uniformly. The preparation method has the advantages of simple process, mild conditions, no need of special equipment, low energy consumption, low cost and easy industrial implementation.
The novel surfactant-free microemulsion provided by the embodiment of the invention can be used in the fields of oilfield development (such as drilling fluid and enhanced oil displacement system), daily chemical industry, functional material preparation, drug carriers, pesticide preparations and the like.
Example 1
Mixing 5 ml of n-dodecane, 15 ml of water, 40 ml of n-butanol and 40 ml of ethanol in a beaker, and uniformly stirring to obtain the microemulsion, wherein the volume ratio of n-dodecane to water is 1:3, the volume ratio of n-butanol to ethanol is 1:1, and the volume ratio of (n-butanol + ethanol)/(n-dodecane + water) is 4: 1.
The appearance of the prepared microemulsion sample is shown in figure 1, and a uniform and transparent system can be seen. The particle size distribution of the prepared microemulsion sample is shown in figure 2, and the average particle size is about 10 nm. The photograph of the prepared microemulsion sample by a cryoetching scanning electron microscope is shown in figure 3, and spherical liquid drops can be observed to prove that the microemulsion is.
The prepared microemulsion sample is frozen at-10 ℃ for 1 day and then melted at room temperature, and is stored at 95 ℃ for 2 weeks, and the system is not layered or the uniformity of the system is damaged, so that the system has good temperature resistance and stability.
Example 2:
mixing 12.5 ml of n-pentadecane, 12.5 ml of NaCl aqueous solution with the mass concentration of 1%, 60 ml of n-butanol and 15 ml of ethanol in a beaker, and uniformly stirring to obtain the microemulsion, wherein the volume ratio of the n-pentadecane to the aqueous solution is 1:1, the volume ratio of the n-butanol to the ethanol is 4:1, and the volume ratio of (n-butanol + ethanol)/(n-pentadecane + aqueous solution) is 3: 1.
The prepared microemulsion sample is frozen at-10 ℃ for 1 day and then melted at room temperature, and is stored at 95 ℃ for 2 weeks, and the system is not layered or the uniformity of the system is damaged, so that the system has good temperature resistance and stability.
Example 3:
10 ml of Saraline185V from Shell and 5 ml of CaSO with a concentration of 2% by mass4Aqueous solution, 63.75 ml of n-butanol and 21.25And (3) mixing the milliliters of ethanol in a beaker, and uniformly stirring to obtain the microemulsion, wherein the volume ratio of the gas-made oil to the water solution is 2:1, the volume ratio of n-butyl alcohol to ethanol is 3:1, and the volume ratio of (n-butyl alcohol + ethanol)/(the gas-made oil + the water solution) is 5.7: 1.
The prepared microemulsion sample is frozen at-10 ℃ for 1 day and then melted at room temperature, and is stored at 95 ℃ for 2 weeks, and the system is not layered or the uniformity of the system is damaged, so that the system has good temperature resistance and stability.
Example 4:
mixing 12.5 ml of n-pentadecane, 12.5 ml of NaCl aqueous solution with the mass concentration of 1%, 60 ml of isobutanol and 15 ml of ethanol in a beaker, and uniformly stirring to obtain the microemulsion, wherein the volume ratio of the n-pentadecane to the aqueous solution is 1:1, the volume ratio of the isobutanol to the ethanol is 4:1, and the volume ratio of (isobutanol + ethanol)/(n-pentadecane + aqueous solution) is 3: 1.
The prepared microemulsion sample is frozen at-10 ℃ for 1 day and then melted at room temperature, and is stored at 95 ℃ for 2 weeks, and the system is not layered or the uniformity of the system is damaged, so that the system has good temperature resistance and stability.
Comparative example 1:
18.75 ml of n-dodecane, 56.25 ml of water, 12.5 ml of n-butanol and 12.5 ml of ethanol were mixed in a beaker and stirred, so that a homogeneous microemulsion could not be obtained, and the system rapidly separated into two layers upon standing.
In this comparative example, the n-dodecane/water volume ratio was 1/3, and the n-butanol/ethanol volume ratio was 1/1, the same as in example 1; however, the volume ratio of (n-butanol + ethanol)/(n-dodecane + water) was 1:3, which is different from example 1. The system of comparative example 1 did not form a microemulsion.
Comparative example 2:
mixing 25 ml of n-pentadecane, 25 ml of NaCl aqueous solution with the mass concentration of 1%, 40 ml of n-butanol and 10 ml of ethanol in a beaker, stirring to obtain homogeneous microemulsion, and quickly separating the system into two layers when standing.
In this comparative example, the volume ratio of n-pentadecane to the aqueous solution was 1/1, and the volume ratio of n-butanol to ethanol was 4/1, which was the same as in example 2; however, the volume ratio of (n-butanol + ethanol)/(n-pentadecane + aqueous solution) was 1:1, which was different from example 2. The system of comparative example 2 did not form a microemulsion.
Comparative example 3:
5 ml of n-dodecane, 15 ml of water and 80 ml of ethanol are mixed in a beaker and stirred to obtain homogeneous microemulsion, and the system is rapidly divided into two layers when standing.
Comparative example 4:
stirring 12.5 ml of n-pentadecane, 12.5 ml of NaCl aqueous solution with the mass concentration of 1% and 75 ml of n-butyl alcohol to obtain a homogeneous microemulsion, and rapidly separating the system into two layers during standing.
Although the embodiments disclosed in the present application are described above, the descriptions are only for the convenience of understanding the present application, and are not intended to limit the present application. It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the disclosure as defined by the appended claims.

Claims (5)

1. A microemulsion without surfactant comprises oil phase, water phase and mixed amphiphilic solvent;
wherein the amphiphilic solvent is a mixed solution of butanol and ethanol;
the ratio of the volume of the mixed amphiphilic solvent to the total volume of the oil phase and the water phase is (1.5:1) - (9: 1);
the oil phase is alkane with a carbon chain length of 10-18;
The volume ratio of the oil phase to the water phase is (9:1) - (1: 9);
the volume ratio of butanol to ethanol in the mixed amphiphilic solvent is (6:1) - (1: 3);
the volume ratio of butanol to ethanol in the mixed amphiphilic solvent is (4:1) - (2: 1);
the butanol is selected from one or more of n-butanol, isobutanol, sec-butanol and tert-butanol;
the oil phase is selected from one or more of dodecane, pentadecane and gas-made oil;
the carbon number of the gas oil is 12-18.
2. The surfactant-free microemulsion according to claim 1, wherein said aqueous phase is pure water or an aqueous solution of an inorganic salt.
3. The surfactant-free microemulsion according to claim 2, wherein said aqueous inorganic salt solution is selected from NaCl, KCl, MgCl2、CaCl2、NaNO3、KNO3、Mg(NO3)2、Ca(NO3)2、Na2SO4、K2SO4And MgSO4One or more inorganic salt aqueous solutions of (a).
4. The surfactant-free microemulsion according to claim 3, wherein the concentration of the aqueous inorganic salt solution is not higher than the inorganic salt saturation concentration.
5. A method of preparing the surfactant-free microemulsion of any one of claims 1 to 4, wherein the method comprises uniformly mixing the oil phase, the water phase and the mixed amphiphilic solvent.
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