CN112138430B - Magnetic nanorod demulsifier, preparation method thereof and method for treating nanoemulsion by using magnetic nanorod demulsifier - Google Patents

Magnetic nanorod demulsifier, preparation method thereof and method for treating nanoemulsion by using magnetic nanorod demulsifier Download PDF

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CN112138430B
CN112138430B CN202010929224.6A CN202010929224A CN112138430B CN 112138430 B CN112138430 B CN 112138430B CN 202010929224 A CN202010929224 A CN 202010929224A CN 112138430 B CN112138430 B CN 112138430B
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demulsifier
demulsification
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nanorod
stirring
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CN112138430A (en
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熊永娇
彭开铭
黄翔峰
李乐雪
吴宝强
贺梦凡
刘佳
陆丽君
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Tongji University
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    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D17/00Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
    • B01D17/02Separation of non-miscible liquids
    • B01D17/04Breaking emulsions
    • B01D17/047Breaking emulsions with separation aids

Abstract

The invention discloses a magnetic nanorod demulsifier, a preparation method thereof and a method for treating nanoemulsion by using the same, belonging to the technical field of demulsifiers. The preparation method of the demulsifier comprises the following steps: FeCl is added3·6H2O and FeSO4·7H2O is in the general formula N2Dissolving in deionized water under the condition to obtain iron salt solution, Fe3+/Fe2+The weight ratio of substances is 2.15, dissolving polyethyleneimine in distilled water to obtain polyethyleneimine solution, wherein the molecular weight of polyethyleneimine is 10000, the weight ratio of N/Fe substances is not less than 1.47, and continuously introducing N2And dropwise adding the polyethyleneimine solution into the iron salt solution under stirring, dropwise adding concentrated ammonia water at the water bath temperature of 50-80 ℃, stirring for reaction for 1-4 h, separating solid particles in the reaction solution by using a magnet, cleaning the solid particles by using deionized water, re-dispersing the solid particles into the deionized water, adding the glutaraldehyde solution, stirring, uniformly mixing, and performing magnetic field separation. The emulsion breaker prepared by the invention can realize high-efficiency emulsion breaking of emulsion with the mass ratio of the surfactant to the oil of 0-0.909 Na.

Description

Magnetic nanorod demulsifier, preparation method thereof and method for treating nanoemulsion by using magnetic nanorod demulsifier
Technical Field
The invention relates to a magnetic nanorod demulsifier, a preparation method thereof and a method for treating nanoemulsion by using the same, belonging to the technical field of demulsifiers.
Background
The mechanical and electronic industry is an important component of the manufacturing industry of Chinese equipment and is an important basis for the development of the national economy of China. Has huge development potential and innovation prospect in the adjustment and progress of the current Chinese economic structure. Meanwhile, the problems of environmental pollution risks and the like caused by waste emulsion generated in the production process and product consumption of the mechanical and electronic industry are increasingly highlighted.
Compared with general oily wastewater or emulsion wastewater, the waste emulsion generated in the mechano-electronic industry has the following typical characteristics: the oil drop size is in a nanometer level, belongs to the category of nanoemulsion, and contains high-concentration mineral oil and a surfactant, wherein the oil content is usually 1-5%, and the content of the surfactant in the oil is up to 30%. The proportion of the surfactant to the oil is high, so that the distribution of the surfactant in the emulsion is very complex, the surfactant is distributed on the surface of nano-scale oil drops to form a stable oil-water interface, and the excessive surfactant is also distributed in a continuous phase to form a micelle structure and a stable 3D network structure, so that the difficulty of emulsion breaking and separation of the emulsion is greatly enhanced.
The traditional method for treating the emulsion mainly comprises a chemical demulsification method, a low-temperature evaporation method, a membrane separation method and the like, but the traditional method is difficult to realize the effective treatment of the emulsion with a high surfactant/oil ratio and also faces great problems, such as the generation of high-volume-ratio oil-containing sludge, the difficulty in sludge-water separation and the like caused by the need of obviously increasing the adding amount of a chemical demulsification agent in the demulsification process, the membrane separation flux can be rapidly reduced in a membrane separation system, the membrane pollution is aggravated, and the concentration of pollutants in water can be obviously increased in the low-temperature evaporation. Therefore, the development of a novel demulsification and separation technology has important practical application value for solving the problem of difficult demulsification of the nano-emulsion, particularly the nano-emulsion with high surfactant/oil ratio.
From the analysis of reasons causing the emulsion to have super stability, the stable microstructure formed by the high proportion of the surfactant is an important reason for difficult demulsification. Therefore, by means of certain strength of acting force, the stable structure formed by the surfactant is broken, and the key point for realizing demulsification is to realize aggregation and separation of oil drops. In recent years, magnetic nanoparticles have attracted great attention in the field of water treatment due to the advantages of easy control, reusability and the like. As early as 2012, researchers first proposed the preparation of magnetic nanoparticle demulsifiers. Through the development of several years, most of the current research reports in the field of demulsification and separation utilize special surface substances or surface properties of magnetic nanoparticles to adhere liquid drops to cause aggregation or coalescence of the liquid drops to realize destabilization and demulsification of the emulsion, for example, the inventor proposes to realize destabilization of the emulsion by utilizing electrostatic action of magnetic nanospheres in earlier research, but research results show that the emulsion with high surfactant/oil ratio is limited by the electrostatic action. Other studies have also largely utilized the electrostatic interaction or interfacial activity of magnetic nanospheres to achieve demulsification of emulsions without surfactants or at low surfactant concentrations. However, the design concept of demulsification depending on the surface properties of the magnetic nanoparticles has severely limited the update of the magnetic nanoparticle demulsifier and the expansion of the application of the magnetic nanoparticle demulsifier in complex and high-stability emulsion.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a magnetic nanorod demulsifier, a preparation method thereof and a method for treating nanoemulsion by using the same, and the magnetic nanorod demulsifier prepared by the invention has wide application range and can realize efficient demulsification of nanoemulsion with the mass ratio of surfactant to oil being in the range of 0-0.909.
In order to achieve the technical purpose, the technical scheme of the invention is as follows:
a preparation method of a magnetic nanorod demulsifier comprises the following steps:
FeCl is added3·6H2O and FeSO4·7H2O is in the general formula N2Dissolving in deionized water under the condition to obtain ferric salt solution, wherein Fe3+/Fe2+The weight ratio of substances is 2.15, dissolving polyethyleneimine in distilled water to obtain polyethyleneimine solution, wherein the molecular weight of polyethyleneimine is 10000, the weight ratio of N/Fe substances is not less than 1.47, and continuously introducing N2And dropwise adding a polyethyleneimine solution into an iron salt solution under the stirring condition, uniformly mixing, dropwise adding concentrated ammonia water at the water bath temperature of 50-80 ℃, stirring for reaction for 1-4 h, separating solid particles in the reaction solution by using a magnet, cleaning the solid particles by using deionized water, re-dispersing the cleaned solid particles into the deionized water, adding a glutaraldehyde solution, stirring, uniformly mixing, and performing magnetic field separation to obtain the magnetic nanorod demulsifier.
The magnetic nanorod demulsifier prepared by the method.
The method for treating the nanoemulsion by adopting the magnetic nanorod demulsifier comprises the following steps: and adding a magnetic nanorod demulsifier into the nanoemulsion with the mass ratio of the surfactant to the oil of 0-0.909, stirring and mixing, and performing one or more times of demulsification separation by means of a magnetic field, wherein for the multiple times of demulsification separation, a new magnetic nanorod demulsifier is added into effluent after the last demulsification is completed before the next demulsification separation is performed, and the demulsification separation operation is repeated.
Preferably, the dosage of the magnetic nanorod demulsifier is 5g/L in each demulsification.
Preferably, the stirring condition is stirring and mixing for 60-180 s at the rotating speed of 2000 rpm.
Preferably, the strength of the magnetic field is 0.2-0.5T.
Preferably, when the mass ratio of the surfactant to the oil is 0-0.045, single demulsification is carried out, when the mass ratio of the surfactant to the oil is less than or equal to 0.045, 3 demulsification is carried out, when the mass ratio of the surfactant to the oil is less than or equal to 0.227, 4 demulsification is carried out, and when the mass ratio of the surfactant to the oil is less than or equal to 0.454, 6 demulsification is carried out.
From the above description, it can be seen that the present invention has the following advantages:
in the emulsion field, a large number of studies have shown that the mass ratio of surfactant to oil is of great significance for the microstructural characteristics and stability of the emulsion. It not only has a decisive effect on the size of oil drops, but also has an important indication effect on the distribution and aggregation state of the surfactant in the emulsion. Generally, the higher the index, the smaller the oil droplet size of the emulsion, and the higher the proportion of surfactant in the continuous phase, the more stable the emulsion formed and the greater the difficulty of handling, given the same dispersion technique and oil concentration. At present, the magnetic nanoparticle processing object is usually a coarse emulsion with a low mass ratio of a surfactant to oil, and the size of liquid drops is large and is distributed between several micrometers and dozens of micrometers. Compared with the prior art, the magnetic nanorod demulsifier is designed and prepared, has a strong shearing effect under the action of a magnetic field, can effectively disturb a net structure formed by a surfactant by utilizing a larger cross section of the magnetic nanorod demulsifier, and destroys a stable microstructure of an emulsion, so that the demulsification effect is remarkably improved. In addition, the magnetic nanorod demulsifier is continuously updated by optimizing the demulsification mode to perform multiple demulsification, so that the high-efficiency demulsification separation of the nanoemulsion formed by the surfactant with ultrahigh concentration can be realized, and the nano-emulsion with ultrahigh stability can be applied to various nano-emulsions with the surfactant concentration/oil mass ratio in the range of 0-0.909.
Drawings
FIG. 1 is a TEM image of the magnetic nanorod demulsifier M-5 prepared in example 1;
FIG. 2 is a TEM image of the magnetic nanorod demulsifier M-4 prepared in example 2;
FIG. 3 is a TEM image of the magnetic nanoparticle demulsifier M-3 prepared from comparative example 1;
FIG. 4 is a TEM image of the magnetic nanoparticle demulsifier M-0 prepared from comparative example 1;
FIG. 5 is a graph of COD removal rates of different demulsifiers for nanoemulsion E1 and E2;
FIG. 6 is a graph of the removal rate of demulsifier M-4 to nanoemulsion E3 at different demulsification times;
FIG. 7 is a graph of the removal rate of demulsifier M-4 for nanoemulsion E4 at different demulsification times;
FIG. 8 is a graph of the removal rate of demulsifier M-4 for nanoemulsion E5 at different demulsification times;
Detailed Description
The features of the invention will be further elucidated by the following examples, without limiting the claims of the invention in any way.
Example 1
11.6g of FeCl3·6H2O (M. 270.3) and 5.56g FeSO4·7H2O (M278) in general formula2Dissolving in 250mL deionized water under the condition to obtain iron salt solution, dissolving 5.0g polyethyleneimine with molecular weight of 10000 (monomer M: 43.06, N: 0.116mol, N/Fe: 1.84) in 50mL distilled water to obtain polyethyleneimine solution, and continuously introducing N2And 500rpAnd M, dropwise adding a polyethyleneimine solution into an iron salt solution under the stirring condition, uniformly mixing, dropwise adding 30mL of concentrated ammonia water (25%) at the water bath temperature of 60 ℃, stirring for reacting for 2h, separating solid particles in the reaction solution by using a magnet, cleaning the solid particles by using deionized water, re-dispersing the cleaned solid particles into 50mL of deionized water, adding 250mL of 0.25% glutaraldehyde solution, stirring for 30min at 500rpm, performing magnetic field separation to obtain a stable-property magnetic nanorod demulsifier M-5, and characterizing the morphology of the magnetic nanorod demulsifier by using a TEM (transmission electron microscope), as shown in FIG. 1, the morphology of the M-5 is mainly a nanorod, the length of the nanorod is 60-125 nm, and the width of the nanorod is 10-20 nm.
Example 2
11.6g of FeCl3·6H2O (M. 270.3) and 5.56g FeSO4·7H2O (M278) in general formula2Dissolving in 250mL deionized water under the condition to obtain iron salt solution, dissolving 4.0g polyethyleneimine with molecular weight of 10000 (monomer M: 43.06, N/Fe: 1.47) in 50mL distilled water to obtain polyethyleneimine solution, and introducing N continuously2And dropwise adding a polyethyleneimine solution into an iron salt solution under the stirring condition of 500rpm, uniformly mixing, dropwise adding 30mL of concentrated ammonia water (25%) at the water bath temperature of 60 ℃, stirring for reacting for 2h, separating solid particles in the reaction solution by using a magnet, cleaning the solid particles by using deionized water, re-dispersing the cleaned solid particles into 50mL of deionized water, adding 250mL of 0.25% glutaraldehyde solution, stirring for 30min at 500rpm, performing magnetic field separation to obtain a stable-property magnetic nanorod demulsifier M-4, and characterizing the morphology by using a TEM (transmission electron microscope), as shown in FIG. 2, wherein the morphology of M-4 is mainly a nanorod, the length of the nanorod-shaped demulsifier is 30-100 nm, and the width of the nanorod-shaped demulsifier is 5-15 nm.
Comparative example 1
11.6g of FeCl3·6H2O (M. 270.3) and 5.56g FeSO4·7H2O (M278) in general formula2Dissolving in 250mL deionized water under the condition to obtain iron salt solution, dissolving 3.0g polyethyleneimine (monomer M: 43.06, N/Fe: 1.10) with molecular weight of 10000 in 50mL distilled water to obtain polyethyleneimine solution, and introducing N continuously2And stirring the polyethylene at 500rpmDropwise adding an imine solution into an iron salt solution, uniformly mixing, dropwise adding 30mL of concentrated ammonia water (25%) at a water bath temperature of 60 ℃, stirring for reacting for 2h, separating solid particles in the reaction solution by using a magnet, cleaning the solid particles by using deionized water, re-dispersing the cleaned solid particles into 50mL of deionized water, adding 250mL of 0.25% glutaraldehyde solution, stirring for 30min at 500rpm, performing magnetic field separation to obtain a stable-property magnetic nanoparticle demulsifier M-3, and characterizing the morphology by using a TEM (transmission electron microscope), as shown in FIG. 3, it can be known from FIG. 3 that when the quantity ratio of N/Fe substances is 1.10, the obtained magnetic nanoparticle demulsifier M-3 is mainly in a nanosphere shape, and the particle size is 10-20 nm.
Comparative example 2
11.6g of FeCl3·6H2O (M. 270.3) and 5.56g FeSO4·7H2O (M278) in general formula2Dissolving in 250mL deionized water under the condition to obtain iron salt solution, and continuously introducing N2And adding 50mL of distilled water into the ferric salt solution under the stirring condition of 500rpm, uniformly mixing, dropwise adding 30mL of concentrated ammonia water (25%) at the water bath temperature of 60 ℃, stirring for reacting for 2h, separating out solid particles in the reaction solution by using a magnet to obtain a magnetic nanoparticle demulsifier M-0 with stable property, and characterizing the morphology of the magnetic nanoparticle demulsifier M-0 by adopting a TEM (transmission electron microscope), as shown in FIG. 4, as can be seen from FIG. 4, when the quantity ratio of N/Fe substances is 0, the morphology of the obtained magnetic nanoparticle demulsifier M-0 is in a nanosphere shape, and the particle size of the magnetic nanoparticle demulsifier M-0 is 10-15 nm.
In order to research the demulsification effect of the magnetic nanorod demulsifier prepared by the invention, the inventor further develops the following demulsification experiment.
Experiment 1
Before the experiment, nanoemulsion E1 and E2 with the mass ratio of the surfactant to the oil of 0.0045 and 0.045 respectively are prepared, and the specific steps are as follows: 0.02g of sodium dodecyl benzene sulfonate is dissolved in 200mL of deionized water, 5mL of liquid paraffin is added, and the mixture is dispersed for 10min by an ultrasonic crusher to obtain nanoemulsion E1 (the particle size of oil drops is 285 nm). 0.2g of sodium dodecylbenzenesulfonate was dissolved in 200mL of deionized water, and 5mL of liquid paraffin (density 0.88 g/cm) was added3) Dispersing for 10min by using an ultrasonic dispersion machine to obtainNanoemulsion E2 (oil droplet size 265 nm).
The magnetic nanoparticle demulsifiers M-0, M-3 and M-5 prepared in example 1 and comparative examples 1 and 2 were used for single demulsification of nanoemulsion E1 and E2, and the specific steps were as follows: 0.5g of demulsifier was added to 100mL of nanoemulsion, stirred and mixed at 2000rpm for 120s, and subjected to magnetic separation under the condition of 0.25T magnetic field intensity. The effluent water is taken for measuring COD, the demulsification effect of the magnetic nanoparticle demulsifier is evaluated according to the removal rate of the COD in the emulsion, and the result is shown in figure 5.
As can be seen from FIG. 5, both the emulsion E1 with the low surfactant/oil ratio and the emulsion E2 with the high surfactant/oil ratio, M-0, have poor demulsification effects, with COD removal rates of 20.3% and 5.7%, respectively; compared with M-0, the demulsification effect of M-3 on E1 and E2 is greatly improved, particularly the demulsification effect on the low-surfactant/oil emulsion E1 is obviously improved, and the COD removal rates of M-3 on E1 and E2 reach 83.5% and 71.8% respectively; relative to M-0 and M-3, M-5 has the best demulsification effect on two emulsions E1 and E2, and the COD removal rate reaches 99.9 percent and 97.6 percent respectively.
Experiment 2:
before the experiment, firstly, a nanoemulsion E3 with the mass ratio of the surfactant to the oil of 0.227 is prepared, and the method specifically comprises the following steps: 1.0g of sodium dodecyl benzene sulfonate is dissolved in 200mL of deionized water, 5mL of liquid paraffin is added, and the mixture is dispersed for 10min by an ultrasonic dispersion machine to obtain nanoemulsion E3 (the particle size of oil drops is 241 nm).
The demulsifier M-4 prepared in the example 2 is used for demulsifying the nanoemulsion E3, and comprises the following specific steps: adding 0.5g of demulsifier into 100mL of nano emulsion, stirring and mixing at 2000rpm for 120s, carrying out magnetic attraction separation under the condition of 0.25T magnetic field intensity, adding 0.5g of demulsifier which is equal to that of the first demulsification into the effluent, carrying out the next demulsification by adopting the same operation as that of the first demulsification, and carrying out 3 demulsification in total. The COD of the emulsion is measured by taking the demulsification effluent of each round, and the removal rate of the COD of the emulsion under different demulsification times is shown in figure 6.
As can be seen from FIG. 6, for the emulsion E3 with a high surfactant/oil ratio (0.227), the magnetic nanorods almost have no effect of demulsification once, and as the number of times of demulsification increases, the demulsification effect of the magnetic nanorod demulsifier on the emulsion E3 greatly increases, and the COD removal rate of the emulsion and the number of times of demulsification show a positive correlation; when the demulsification frequency reaches 3 times, the removal rate of COD reaches 96.2 percent.
Experiment 3:
before the experiment, firstly, a nanoemulsion E4 with the mass ratio of the surfactant to the oil of 0.454 is prepared, and the method specifically comprises the following steps: 2.0g of sodium dodecyl benzene sulfonate is dissolved in 200mL of deionized water, 5mL of liquid paraffin is added, and the mixture is dispersed for 10min by an ultrasonic dispersion machine to obtain nanoemulsion E4 (the particle size of oil drops is 232 nm).
The demulsifier M-4 prepared in the example 2 is used for demulsifying the nanoemulsion E3, and comprises the following specific steps: adding 0.5g of demulsifier into 100mL of nano emulsion, stirring and mixing at 2000rpm for 120s, carrying out magnetic attraction separation under the condition of 0.25T magnetic field intensity, adding 0.5g of demulsifier which is equal to that of the first demulsification into the effluent, carrying out the next demulsification by adopting the same operation as that of the first demulsification, and carrying out 4 demulsification in total. The COD of the emulsion is measured by taking the demulsification effluent of each round, and the removal rate of the COD of the emulsion under different demulsification times is shown in figure 7.
As can be seen from fig. 7, for the emulsion E4 with a high surfactant/oil ratio (0.454), the magnetic nanorods have almost no effect of demulsification twice, and as the number of times of demulsification increases, the demulsification effect of the magnetic nanorod demulsifier on the emulsion E4 starts to increase significantly, and the COD removal rate of the emulsion goes through a lower plateau and then rises rapidly; when the demulsification times reach 4 times, the removal rate of COD reaches 96.1 percent.
Experimental group 4:
before the experiment, firstly, a nanoemulsion E5 with the mass ratio of the surfactant to the oil of 0.909 is prepared, and the method specifically comprises the following steps: 4.0g of sodium dodecyl benzene sulfonate is dissolved in 200mL of deionized water, 5mL of liquid paraffin is added, and the mixture is dispersed for 10min by an ultrasonic dispersion machine to obtain nanoemulsion E5 (the particle size of oil drops is 202 nm).
The demulsifier M-4 prepared in the example 2 is used for demulsifying the nanoemulsion E3, and comprises the following specific steps: adding 0.5g of demulsifier into 100mL of nano emulsion, stirring and mixing at 2000rpm for 120s, carrying out magnetic attraction separation under the condition of 0.25T magnetic field intensity, adding 0.5g of demulsifier which is equal to that of the first demulsification into the effluent, carrying out the next demulsification by adopting the same operation as that of the first demulsification, and carrying out 6 demulsification in total. The COD of the emulsion is measured by taking the demulsification effluent of each round, and the removal rate of the COD of the emulsion under different demulsification times is shown in figure 8.
As can be seen from fig. 8, for the emulsion E5 with high surfactant/oil (0.909), the magnetic nanorod demulsifier has almost no effect of performing tertiary demulsification, and as the number of demulsification increases, the demulsification effect of the magnetic nanorod demulsifier on the emulsion E5 starts to increase significantly, and the COD removal rate of the emulsion goes through a lower plateau and then rises rapidly; when the demulsification frequency reaches 6 times, the removal rate of COD reaches 92.1 percent.
It should be understood that the detailed description of the invention is merely illustrative of the invention and is not intended to limit the invention to the specific embodiments described. It will be appreciated by those skilled in the art that the present invention may be modified or substituted equally as well to achieve the same technical result; as long as the use requirements are met, the method is within the protection scope of the invention.

Claims (7)

1. The preparation method of the magnetic nanorod demulsifier is characterized by comprising the following steps:
FeCl is added3•6H2O and FeSO4•7H2O is in the general formula N2Dissolving in deionized water under the condition to obtain iron salt solution, Fe3+/Fe2+The weight ratio of the substances is 2.15, dissolving polyethyleneimine in distilled water to obtain polyethyleneimine solution, wherein the molecular weight of polyethyleneimine is 10000, the weight ratio of N/Fe substances is greater than 1.47, and continuously introducing N2And dropwise adding a polyethyleneimine solution into an iron salt solution under the stirring condition, uniformly mixing, dropwise adding concentrated ammonia water at the water bath temperature of 50-80 ℃, stirring for reaction for 1-4 h, separating solid particles in the reaction solution by using a magnet, cleaning the solid particles by using deionized water, re-dispersing the solid particles into the deionized water, adding a glutaraldehyde solution, stirring, uniformly mixing, and performing magnetic field separation to obtain the magnetic nanorod demulsifier.
2. A magnetic nanorod demulsifier prepared by the preparation method of the magnetic nanorod demulsifier of claim 1.
3. A method of treating nanoemulsion using the magnetic nanorod demulsifier of claim 2, comprising the steps of: and adding a magnetic nanorod demulsifier into the nanoemulsion with the mass ratio of the surfactant to the oil of 0-0.909, stirring and mixing, and performing one or more times of demulsification separation by means of a magnetic field, wherein for the multiple times of demulsification separation, a new magnetic nanorod demulsifier is added into effluent after the last demulsification is completed before the next demulsification separation is performed, and the demulsification separation operation is repeated.
4. The method of claim 3, wherein the amount of the magnetic nanorod demulsifier added at each demulsification time is 5 g/L.
5. The method according to claim 3, wherein the stirring conditions are stirring and mixing at 2000rpm for 60 to 180 seconds.
6. The method of claim 3, wherein the magnetic field has a strength of 0.2 to 0.5T.
7. The method of claim 3, wherein a single demulsification is performed when the surfactant to oil mass ratio is 0 to 0.045, wherein 3 demulsification is performed when 0.045< surfactant to oil mass ratio.ltoreq.0.227, wherein 4 demulsification is performed when 0.227< surfactant to oil mass ratio.ltoreq.0.454, and wherein 6 demulsification is performed when 0.454< surfactant to oil mass ratio.ltoreq.0.909.
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