CN111632405A - Oil-water separation method based on magnetic Janus particles - Google Patents
Oil-water separation method based on magnetic Janus particles Download PDFInfo
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- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
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- C—CHEMISTRY; METALLURGY
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/48—Treatment of water, waste water, or sewage with magnetic or electric fields
- C02F1/488—Treatment of water, waste water, or sewage with magnetic or electric fields for separation of magnetic materials, e.g. magnetic flocculation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
The invention relates to an oil-water separation method based on magnetic Janus particles. The oil-water separation method comprises the following steps: a) putting magnetic Janus particles into an oil-water mixture, and emulsifying at 13000-20000 r/min by using a high-speed shearing emulsifying machine or emulsifying at 300-5000 r/min by using a high-speed stirrer to form an emulsion system comprising a continuous phase and a dispersed phase stabilized by the magnetic Janus particles, wherein each magnetic Janus particle simultaneously has a hydrophilic part and a hydrophobic part; b) applying an external magnetic field A to the emulsion system, causing the dispersed phase to aggregate, to form the emulsion system having an emulsion-enriched portion enriched with the dispersed phase and a liquid portion free of the dispersed phase, thereby separating the emulsion-enriched portion and the liquid portion.
Description
Technical Field
The invention relates to an oil-water separation method, in particular to an oil-water separation method based on magnetic Janus particles as a solid particle emulsifier.
Background
In the oil industry (oil extraction, oil refining, petrochemical industry, and the like), the mechanical industry, the textile industry, the cosmetic manufacturing industry, the catering industry, the food industry, and the like, or in the water body protection field, a situation where oil substances and water bodies are mixed often occurs. In particular, when a substance capable of functioning as an emulsifier (a compound which forms a stable emulsion from a mixture of two or more components which are not mutually soluble) is sometimes present in an oil-water mixture, an emulsion may be present in the oil-water mixture, and even the oil-water mixture as a whole may be an emulsion. In an emulsion, the dispersed phase is dispersed in the continuous phase in the form of droplets (micron-sized). The emulsifier reduces the interfacial tension of the components of the mixed system and forms a stronger film on the surface of the droplets or forms an electric double layer on the surface of the droplets due to the electric charge given by the emulsifier, preventing the droplets from aggregating with each other, thereby maintaining the emulsion homogeneous. Under the condition, the oil phase and the water phase are difficult to separate thoroughly, the difficulty of oil-water separation is greatly improved, the application of an emulsification system in the aspects of extraction, separation, tertiary oil recovery and the like is limited, and environmental pollution and resource waste can be caused.
In contrast, the basic principle of the conventional oil-water separation method is to destroy the interfacial stability of an emulsion or an approximate emulsion in an oil-water mixture as much as possible, realize the macroscopic layering of oil and water phases, and then separate the oil and water phases. Such as air flotation, centrifugation, addition of demulsifiers, and the like. However, the existing method has the defects of low separation efficiency, long separation time, high cost, easy secondary pollution, incapability of recycling, substandard water discharge, resource waste and the like. The most critical of these is the difficulty of emulsifier-stabilized droplets to rapidly coalesce and form large-sized oil phases.
The prior art discloses a technology for oil-water separation by adopting an adsorption material. For example, patent document 1 discloses a superhydrophobic magnetic PS/SiO2The oil-water separation material takes ferroferric oxide as a magnetic core, PS as an inner shell and super-hydrophobic SiO2Is a shell. The oil-water separation material has an adsorption effect on oil in the oil-containing wastewater, and can reach a level of 90%. However, thisThe oil absorption capacity of class technologies is limited and depends on the composition of the oily wastewater to be treated; and the oil-adsorbed adsorbent usually requires a specific desorption process, resulting in a complicated oil-water separation process.
In addition, the prior art also discloses an oil-water separation technology of Pickering emulsion by using a solid emulsifier. For example, non-patent document 1 discloses a technique for separating oil from water using magnetic particles based on P (NIPAM-co-AA) as a solid emulsifier. However, it can be seen from the photographs disclosed in this document that although such solid emulsifiers can produce an oil-water separation effect, the effect cannot be achieved to a desired level.
The Janus particles with one hydrophilic side and one lipophilic side have amphipathy similar to a small molecular surfactant, and can be used as a solid emulsifier to stabilize an oil-water interface to form a stable emulsion. As a special surfactant, Janus particles with amphiphilicity have the Pickering effect and the capability of reducing surface tension. In addition, the two sides of the particle often have different wettability, which can significantly enhance the emulsifying capacity and emulsion stability. When added to an emulsion, Janus particles can replace emulsifier molecules on the surface of the emulsion and thus also participate in the stabilization of the oil-water interface. Meanwhile, paramagnetic components are compounded into Janus particles, so that magnetic Janus particles can be obtained, the magnetic Janus particles become a novel magnetically recyclable solid emulsifier, and enrichment can be realized through an external magnetic field. The magnetically recyclable solid emulsifier can stabilize an oil-water interface to form a stable emulsion system on one hand; on the other hand, the stable emulsion liquid drop can be enriched through an external magnetic field, and the separation of oil and water phases of an emulsion system is realized. The separation process does not need demulsification, and has high speed and thorough separation effect. And the magnetic Janus particles can be recycled, so that the cost is reduced, and the environmental pollution is avoided.
For example, magnetic Janus particles are prepared and used for oil-water separation in patent document 2. However, the oil-water separation effect in patent document 2 is still difficult to achieve a desired effect, and the oil-water separation technique has not been studied intensively.
It is seen that there is still room for improvement in establishing a technology capable of performing oil-water separation simply and efficiently.
Patent document
Patent document 1: CN106277162A
Patent document 2: WO 2016/026464A1
Non-patent document
Non-patent document 1: influence of monomer proportion of P (NIPAM-co-AA) particles on oil-water emulsification performance and application of P (NIPAM-co-AA) particles in oil-water separation in petrochemical industry, 2017, vol.46, No. 6, page 772-777.
Disclosure of Invention
Problems to be solved by the invention
In view of the above-mentioned drawbacks of the prior art, the present invention is directed to provide a method for separating oil from water, which can be widely applied to various oil-water mixtures, particularly to an oil-water mixture having an emulsion, can simply and efficiently separate oil from water, and has excellent environmental friendliness and economy.
Means for solving the problems
According to the intensive research of the inventor of the present invention, it is found that the technical problems can be solved by implementing the following technical scheme:
[1] an oil-water separation method, comprising the steps of:
a) putting magnetic Janus particles into an oil-water mixture, and emulsifying at 13000-20000 r/min by using a high-speed shearing emulsifying machine or emulsifying at 300-5000 r/min by using a high-speed stirrer to form an emulsion system comprising a continuous phase and a dispersed phase stabilized by the magnetic Janus particles, wherein each magnetic Janus particle simultaneously has a hydrophilic part and a hydrophobic part;
b) applying an external magnetic field A to the emulsion system, causing the dispersed phase to aggregate, to form the emulsion system having an emulsion-enriched portion enriched with the dispersed phase and a liquid portion free of the dispersed phase, thereby separating the emulsion-enriched portion and the liquid portion.
[2] The oil-water separation method according to [1], wherein the magnetic Janus particles are used in an amount of 0.001 to 5 wt% based on the total weight of the oil-water mixture in step a).
[3] The oil-water separation method according to [1] or [2], wherein the magnetic Janus particle is snowman-shaped.
[4] The oil-water separation method according to any one of [1] to [3], wherein in the step b), the magnetic field strength of the external magnetic field A is 0.05T to 2T.
[5] The oil-water separation method according to any one of [1] to [4], wherein the external magnetic field A is applied for 1 second to 30 minutes in step b).
[6] The oil-water separation method according to any one of [1] to [5], further comprising the steps of:
c) applying an external magnetic field B having a greater magnetic field strength than the external magnetic field A to the separated emulsion portion enriched in the dispersed phase, thereby breaking the emulsion and recovering the magnetic Janus particles.
[7] The oil-water separation method according to [6], wherein in the step c), the magnetic field strength of the external magnetic field B is 0.1T to 5T.
[8] The oil-water separation method according to any one of [1] to [7], wherein the combination of the hydrophilic portion and the hydrophobic portion of the magnetic Janus particles is selected from the group consisting of silica/polystyrene-divinylbenzene, silica/poly (meth) acrylate monomer-divinylbenzene, silica/polystyrene-di (meth) acrylate monomer, silica/poly (meth) acrylate monomer-di (meth) acrylate monomer, silica/polystyrene- (meth) acrylate monomer-di (meth) acrylate monomer, titania/polystyrene-divinylbenzene, titania/poly (meth) acrylate monomer-divinylbenzene, titanium dioxide/poly (meth) acrylate monomer-divinylbenzene, and mixtures thereof, At least one of titanium dioxide/polystyrene-di (meth) acrylate monomer, titanium dioxide/poly (meth) acrylate monomer-di (meth) acrylate monomer.
ADVANTAGEOUS EFFECTS OF INVENTION
Through the implementation of the technical scheme, the invention can obtain the following technical effects:
(1) the magnetic Janus particles are amphiphilic and function as a solid emulsifier, so that the oil-water separation method of the present invention can be widely applied to various oil-water mixtures without depending on factors such as the oil-water ratio of the oil-water mixture, the presence or absence of an emulsion, or the type (water-in-oil type or oil-in-water type) of the emulsion contained therein.
(2) The oil-water separation method can rapidly realize excellent emulsification effect and separation effect, and is simple to operate, so that the oil-water separation method has the advantages of reducing industrial cost and simplifying industrial equipment for water-oil separation.
(3) The magnetic Janus particles can be recycled, so that the oil-water separation method is green, economical and free of secondary pollution.
Drawings
FIG. 1 is a scanning electron micrograph of magnetic Janus particles.
FIG. 2 is a graph of the effect of emulsions stabilized by magnetic Janus particles.
Fig. 3 is an optical microscope picture of a magnetic Janus particle stabilized emulsion.
FIG. 4 is a diagram showing the effect of stabilizing the emulsion oil-water separation of magnetic Janus particles under an external magnetic field.
Detailed Description
The present invention will be described in detail below. The technical features described below are explained based on typical embodiments and specific examples of the present invention, but the present invention is not limited to these embodiments and specific examples. It should be noted that:
in the present specification, the term "Janus particle" refers to a Janus particle in the broad sense of the art, i.e., a particle that is not only asymmetric (anisotropic) in structural morphology, but also asymmetric in compositional properties, or both.
In the present specification, the "(meth) acrylate" used includes the meanings of "methacrylate" and "acrylate"; the "(meth) acrylic acid" used includes the meaning of "methacrylic acid" as well as "acrylic acid".
In the present specification, the numerical range represented by "numerical value a to numerical value B" means a range including the end point numerical value A, B.
In the present specification, the numerical ranges indicated by "above" or "below" mean the numerical ranges including the numbers.
In the present specification, the meaning of "may" includes both the meaning of performing a certain process and the meaning of not performing a certain process.
As used herein, the term "optional" or "optional" is used to indicate that certain substances, components, performance steps, application conditions, and the like are used or not used.
In the present specification, the unit names used are all international standard unit names, and the "%" used means weight or mass% content, if not specifically stated.
In the present specification, the term "particle diameter" as used herein means an "average particle diameter" if not specifically stated, and can be measured by a commercially available particle sizer or an electron scanning microscope.
In the present specification, reference to "some particular/preferred embodiments," "other particular/preferred embodiments," "embodiments," and the like, means that a particular element (e.g., feature, structure, property, and/or characteristic) described in connection with the embodiment is included in at least one embodiment described herein, and may or may not be present in other embodiments. In addition, it is to be understood that the described elements may be combined in any suitable manner in the various embodiments.
The oil-water separation method comprises the following steps:
a) putting magnetic Janus particles into an oil-water mixture, and emulsifying at 13000-20000 r/min by using a high-speed shearing emulsifying machine or emulsifying at 300-5000 r/min by using a high-speed stirrer to form an emulsion system comprising a continuous phase and a dispersed phase stabilized by the magnetic Janus particles, wherein each magnetic Janus particle simultaneously has a hydrophilic part and a hydrophobic part;
b) applying an external magnetic field A to the emulsion system, causing the dispersed phase to aggregate, to form the emulsion system having an emulsion-enriched portion enriched with the dispersed phase and a liquid portion free of the dispersed phase, thereby separating the emulsion-enriched portion and the liquid portion.
The above steps will be described in detail below.
a) Emulsification step
In this step, the magnetic Janus particles are put into an oil-water mixture and emulsified using a high-speed shear emulsifier or an impeller to form an emulsion system comprising a continuous phase and a dispersed phase.
In some embodiments, in the case of a high shear emulsifying machine, the shear rate of the high shear emulsifying machine is 13000 to 20000r/min, preferably 14000 to 19000 r/min. When the shearing speed is less than the range, an emulsion system obtained by using a high-speed shearing emulsifying machine tends to be unstable, and sufficient oil-water separation is difficult to realize. When the shear rate is more than this range, the emulsion system obtained by using the high-shear emulsifying machine tends to be unstable.
In other embodiments, when a high-speed stirrer is used, the stirring speed of the high-speed stirrer is 300 to 5000r/min, preferably 500 to 4500 r/min. When the shear rate is less than this range, the emulsion system obtained by the high-speed stirrer tends to be unstable, and sufficient oil-water separation is difficult to achieve. When the shear rate is more than this range, the emulsion system obtained by using the high-speed stirrer tends to be unstable.
The amount of the magnetic Janus particles is not particularly limited, and may be appropriately adjusted according to the oil-water ratio in the oil-water mixture to be treated. In some embodiments, the amount of the magnetic Janus particles is preferably 0.001 to 5 wt%, more preferably 0.01 to 3 wt%, and still more preferably 0.02 to 1 wt% relative to the total weight of the oil-water mixture, from the viewpoint of better obtaining the technical effects of the present invention. In some embodiments, the amount of the magnetic Janus particles is preferably 0.02 to 1% by weight relative to the total weight of the dispersed phase (aqueous phase or oil phase) in the oil-water mixture, from the viewpoint of better obtaining the technical effects of the present invention.
In the present invention, the manner of charging the magnetic Janus particles is not particularly limited, and the magnetic Janus particles may be charged into the oil-water mixture before or during the application of the dynamic conditions, and may be charged at once or in portions.
In this step, the emulsification time is not particularly limited, but is preferably 0.5 to 30 minutes, and more preferably 1 to 15 minutes.
The oil water mixture and magnetic Janus particles are described in detail below.
(1) Oil-water mixture
The source of the oil-water mixture to be treated is not particularly limited, and for example, it may be oil-containing wastewater generated in the petroleum industry (oil extraction, oil refining, petrochemical industry, and the like), the mechanical industry, the textile industry, the cosmetic manufacturing industry, the catering industry, the food industry, or the like, or other oil-water mixtures requiring separation, such as contaminated water. In some specific embodiments, examples of the oil component of the oil-water mixture that makes up the oil phase include, without limitation: natural petroleum oils, petroleum products (e.g., such as kerosene, gasoline, benzene, toluene, n-hexane, cyclohexane, xylene, naphthalene, etc.), tars and fractions thereof, edible animal and vegetable oils and fats, and the like. As the oil component of the present invention, the above-mentioned substances may be present alone or in a combination of two or more. In addition to water and oil components, the oil-water mixture of the present invention may include surfactants (e.g., emulsifiers, etc.), particulate matter insoluble in both phases, matter soluble in the oil component, matter soluble in water, and the like, depending on the source.
There is no particular limitation on the dispersion state of the oil phase and the aqueous phase in the oil-water mixture. In some embodiments, the miscella of the present invention may be a non-emulsion. In other embodiments, at least a portion of the miscella of the present invention may be an emulsion, and even all may be an emulsion. When at least a part of the oil-water mixture of the present invention may be an emulsion, the type of the emulsion is not particularly limited, and may be an oil-in-water type, a water-in-oil type, or the like.
In some specific embodiments, the oil-water ratio (oil phase: water phase) in the oil-water mixture of the present invention is preferably 1:10000000 to 1000000:1, more preferably 1:100000 to 100000:1, still more preferably 1:80000 to 80000:1, and even more preferably 1:50000 to 50000:1 by weight ratio.
(2) Magnetic Janus particles
A portion of each of the magnetic Janus particles of the present invention has a hydrophilic property and another portion has a hydrophobic property, in other words, each of the magnetic Janus particles of the present invention has both a hydrophilic part and a hydrophobic part. The specific chemical composition of the magnetic Janus particles of the present invention is not particularly limited as long as one part thereof has hydrophilicity and the other part thereof has hydrophobicity, and can be adjusted according to the composition of the oil-water mixture to be treated.
In some embodiments, the hydrophilic portion of the magnetic Janus particles of the present invention can have hydroxyl groups (including alcoholic hydroxyl groups, silicon hydroxyl groups, phenolic hydroxyl groups, and the like), ether groups, amide groups, carboxyl groups, anhydrides or salts thereof, and the like. In some embodiments, the hydrophilic portion of the magnetic Janus particles of the present invention can be comprised of organic materials, inorganic materials, or both. Examples of the forming monomer of the organic substance constituting the hydrophilic portion include, but are not limited to, acrylic monomers, pyrrolidone monomers, acrylamide monomers, (poly) ethylene glycol monomers, (poly) propylene glycol monomers, and the like. These monomers may be used alone or in combination of two or more. Examples of the inorganic substance constituting the hydrophilic portion include, without limitation, silicon monoxide, silicon dioxide, titanium dioxide, aluminum oxide, and the like. These inorganic substances may be used alone or in combination of two or more. In some preferred embodiments, the hydrophilic portion of the magnetic Janus particles of the present invention preferably comprises an inorganic substance, more preferably comprises silica.
In some embodiments, the hydrophobic portion of the magnetic Janus particles of the present invention comprises an organic substance. In this case, examples of the forming monomer of the organic substance constituting the hydrophobic portion include, without limitation, styrene-based monomers (e.g., styrene, p-methylstyrene, α -methylstyrene, etc.), (meth) acrylate-based monomers (e.g., methyl (meth) acrylate, ethyl (meth) acrylate, butyl (meth) acrylate, octyl (meth) acrylate, etc.), silane-based monomers, siloxane-based monomers, olefin-based monomers, acetal-based monomers, and the like. These resins may be used alone or in combination of two or more. In some preferred embodiments, the hydrophobic portion of the magnetic Janus particles of the present invention preferably comprises a polystyrene-based resin or a poly (meth) acrylate-based resin. In other preferred embodiments, the hydrophobic portion of the magnetic Janus particles of the present invention preferably comprises a crosslinking component. Examples of crosslinking components include, without limitation: divinylbenzene, di (meth) acrylate monomers (e.g., ethylene glycol di (meth) acrylate, propylene glycol di (meth) acrylate, butylene glycol di (meth) acrylate, etc.), tri (meth) acrylate monomers (e.g., glycerol tri (meth) acrylate, trimethylolpropane tri (meth) acrylate), etc., tetra (meth) acrylate monomers (e.g., pentaerythritol tetra (meth) acrylate), penta (meth) acrylate monomers (e.g., dipentaerythritol penta (meth) acrylate), hexa (meth) acrylate monomers (e.g., dipentaerythritol hexa (meth) acrylate), etc.
Furthermore, the hydrophobic portion of the magnetic Janus particles of the present invention can be hollow, porous, or solid, as desired.
In some preferred embodiments, the combination of hydrophilic and hydrophobic portions (hydrophilic/hydrophobic portions) of the magnetic Janus particles of the present invention is preferably selected from the group consisting of silica/polystyrene (as described in WO 2016/026464a 1), silica/poly (meth) acrylate-based monomers, silica/polystyrene-divinylbenzene, silica/poly (meth) acrylate-based monomers-divinylbenzene, silica/polystyrene-di (meth) acrylate-based monomers, silica/poly (meth) acrylate-based monomers-di (meth) acrylate-based monomers, silica/poly (meth) acrylate-di (meth) acrylate-based monomers, and mixtures thereof, At least one of silicon dioxide/polystyrene- (methyl) acrylate monomer-di (methyl) acrylate monomer, titanium dioxide/polystyrene, titanium dioxide/poly (methyl) acrylate monomer, titanium dioxide/polystyrene-divinylbenzene, titanium dioxide/poly (methyl) acrylate monomer-divinylbenzene, titanium dioxide/polystyrene-di (methyl) acrylate monomer, and titanium dioxide/poly (methyl) acrylate monomer-di (methyl) acrylate monomer. In some more preferred embodiments, the combination of hydrophilic and hydrophobic portions (hydrophilic/hydrophobic portions) of the magnetic Janus particles of the present invention is more preferably selected from the group consisting of silica/polystyrene-divinylbenzene, silica/poly (meth) acrylate-based monomer-divinylbenzene, silica/polystyrene-di (meth) acrylate-based monomer, silica/poly (meth) acrylate-based monomer-di (meth) acrylate-based monomer, silica/polystyrene- (meth) acrylate-based monomer-di (meth) acrylate-based monomer, titania/polystyrene-divinylbenzene, silica/poly (meth) acrylate-based monomer-di (meth) acrylate-based monomer, silica/polystyrene-divinylbenzene, silica/poly (meth) acrylate-based monomer, and mixtures thereof, At least one of titanium dioxide/poly (meth) acrylate monomer-divinylbenzene, titanium dioxide/polystyrene-di (meth) acrylate monomer, and titanium dioxide/poly (meth) acrylate monomer-di (meth) acrylate monomer.
The magnetic Janus particles of the present invention include a magnetic component, such as, for example, iron (Fe) trioxide2O3) Ferroferric oxide (Fe)3O4) Iso-iron oxide, chromium dioxide (CrO)2) Magnetic ferrite (MFe)2O4) Magnetic spinel (MR)2O4) Magnetic hexaferrite (MFe)12O19) Magnetic orthoferrite (RFeO)3) Magnetic garnet M3R2(AO4)3Wherein M represents a divalent metal, R represents a trivalent metal and a represents a tetravalent metal. From the viewpoint of easy availability, the magnetic component is preferably ferroferric oxide. The magnetic component may optionally be present in the hydrophilic portion of the magnetic Janus particleA hydrophobic moiety, or both. In some preferred embodiments, the magnetic component of the present invention is present at least in the hydrophobic portion of the magnetic Janus particles from the viewpoint of better achieving the technical effects of the present invention, and more preferably, the magnetic component of the present invention is supported on the hydrophobic portion of the magnetic Janus particles.
Further, from the viewpoint of better achieving the technical effects of the present invention, the magnetic Janus particles of the present invention are preferably magnetic particles that are asymmetric (anisotropic) in structural morphology, for example, magnetic particles having a shape of a cylinder, a disk, a hamburger, a dumbbell, a chain, a half-raspberry, a raspberry, or a snowman, and can be selected according to the composition of the oil-water mixture to be treated. From the viewpoint of further more preferably achieving the technical effects of the present invention, the magnetic Janus particles of the present invention are more preferably magnetic particles having a snowman shape. In the present invention, the term "snowman-like" refers to a three-dimensional structure (as shown in fig. 1) in which two spheres (or approximate spheres) of the same or different sizes are stacked in a partially overlapping manner. In the case where the magnetic Janus particles of the present invention are snowman-shaped magnetic particles, the ratio of the diameters of the two spheres constituting "snowman-shaped" is preferably 1:4 to 4: 1.
The size of the magnetic Janus particles of the present invention is not particularly limited as long as it can function as a solid particle emulsifier, and can be adjusted according to the composition of the oil-water mixture to be treated. In some embodiments, the size of the magnetic Janus particles of the present invention is preferably 150 to 800nm, more preferably 250 to 600nm, from the viewpoint of better achieving the technical effects of the present invention. The size of the magnetic Janus particles of the present invention can be measured by means well known in the art, for example by Scanning Electron Microscopy (SEM).
In the present invention, the magnetic Janus particles can be prepared by a method generally used in the art, for example, by emulsion polymerization, seeded emulsion polymerization, dispersion polymerization-seeded emulsion polymerization, and the like.
b) Magnetic aggregation separation step
In this step, an external magnetic field a is applied to the emulsion system, causing the dispersed phase to aggregate to form the emulsion system with an emulsion-enriched portion enriched with the dispersed phase and a liquid portion free of the dispersed phase, thereby separating the emulsion-enriched portion and the liquid portion.
The magnetic field strength of the external magnetic field a is generally appropriately selected depending on the kind of the magnetic Janus particles used and the composition of the oil-water mixture. In some embodiments, the magnetic field strength of the external magnetic field A is preferably 0.05T to 2T, more preferably 0.08T to 1.5T. When the magnetic field strength of the external magnetic field a is less than this range, aggregation of the dispersed phase tends to be difficult to achieve. When the magnetic field strength of the external magnetic field a is larger than this range, the dispersed phase stabilized by the magnetic Janus particles tends to be difficult to maintain stable.
In some embodiments, the application time of the external magnetic field a is preferably 1 second to 30 minutes, preferably 10 seconds to 20 minutes, and more preferably 2 minutes to 10 minutes, from the viewpoint of better achieving the technical effects of the present invention. When the application time of the external magnetic field a is less than this range, it tends to be difficult to achieve a satisfactory oil-water separation effect. When the application time of the external magnetic field a is longer than this range, the separation effect cannot be further improved in general, and the oil-water separation efficiency is adversely affected.
Generally, the external magnetic field a may be applied by means known in the art. The external magnetic field a may be applied, for example, by an electromagnet or a permanent magnet. These magnets may be a single magnet or any combination of magnets.
There is no particular limitation on the method of separating the enriched emulsion fraction and the liquid fraction, and means generally known in the art, such as magnetic adsorption of the enriched emulsion fraction, aspiration of the enriched emulsion fraction, flowing out of the liquid fraction, and the like, may be used.
c) Recovery procedure for magnetic Janus particles
The oil-water separation method of the present invention may further comprise a step of recovering the magnetic Janus particles as needed. In this step, an external magnetic field B of greater magnetic strength than the external magnetic field a is applied to the separated emulsion fraction enriched in the dispersed phase, thereby breaking the emulsion and recovering the magnetic Janus particles.
The magnetic field strength of the external magnetic field B is preferably greater than the magnetic field strength of the external magnetic field a. In some preferred embodiments, the magnetic field strength of the external magnetic field B is preferably 0.1T to 5T, more preferably 0.2T to 4T. When the magnetic field strength of the external magnetic field B is less than the above range, it tends to be difficult to achieve good demulsification. When the magnetic field strength of the external magnetic field B is larger than the above range, the demulsifying effect tends to be not further improved and the cost tends to be increased.
Generally, the external magnetic field B may be applied by means known in the art. The external magnetic field B may be applied by an electromagnet or a permanent magnet, for example. These magnets may be a single magnet or any combination of magnets.
The separated magnetic Janus particles can be used again in the oil-water separation method of the present invention after being subjected to washing, drying, etc. as needed.
Examples
Example 1
To a mixture of 20ml of water and 2ml of n-hexane, 0.1g (0.45 wt% with respect to the amount of the mixture) of magnetic Janus particles (such as the magnetic silica/polystyrene-divinylbenzene Janus particles shown in fig. 1) was added. Stirring at 1000r/min for 2min to form oil-in-water emulsion. This system was adsorbed with a 0.3T magnet for 5min, and n-hexane droplets stabilized by magnetic Janus particles (dispersed phase) were fixed by magnetic field enrichment, and a water phase as a continuous phase was made to flow out, thereby separating an enriched emulsion portion containing n-hexane droplets stabilized by magnetic Janus particles, and the oil-water separation efficiency (oil-water separation efficiency, which is the weight of the separated oil phase (n-hexane in this example)/total weight of the oil phase in the mixture) was 90%.
To the resulting enriched emulsion fraction, an external magnetic field was applied with a 3T magnet, thereby breaking the enriched emulsion fraction. The magnetic Janus particles were recovered by applying an external magnetic field continuously with a 3T magnet. Further, the magnetic Janus particles were washed twice with 50ml of dichloromethane and dried in vacuum to obtain a magnetic Janus powder.
Example 2
To 200ml of refined oily sewage, 0.4g (0.2 wt% with respect to the amount of refined oily sewage) of magnetic Janus particles (such as the magnetic silica/polystyrene-divinylbenzene Janus particles shown in fig. 1) was added and stirred at a high speed of 1000r/min for 2min to form an emulsion. After the system is adsorbed by a 0.8T magnet for 5min, a water phase serving as a continuous phase flows out, so that an enriched emulsion part containing oil stains stabilized by magnetic Janus particles is separated, oil-water separation is realized, and the oil-water separation efficiency is 92%.
To the resulting enriched emulsion fraction, an external magnetic field was applied with a 3T magnet, thereby breaking the enriched emulsion fraction. The magnetic Janus particles were recovered by applying an external magnetic field continuously with a 3T magnet. Further, 100ml of methylene chloride was added to the above magnetic Janus particles, and the mixture was washed twice and dried in vacuum to obtain magnetic Janus powder.
Example 3
To 10ml of kitchen waste water, 0.1g (1 wt% with respect to the amount of kitchen waste water) of magnetic Janus particles (magnetic silica/polystyrene-divinylbenzene Janus particles as shown in fig. 1) was added and stirred at a high speed of 2000r/min for 1min to form an emulsion. The system was adsorbed with a 0.3T magnet for 5min to allow the aqueous phase as the continuous phase to flow out, thereby separating the enriched emulsion fraction containing the oil stain stabilized by the magnetic Janus particles, achieving oil-water separation with an oil-water separation efficiency of 95%.
To the resulting enriched emulsion fraction, an external magnetic field was applied with a 3T magnet, thereby breaking the enriched emulsion fraction. The magnetic Janus particles were recovered by applying an external magnetic field continuously with a 3T magnet. Further, the magnetic Janus particles were washed twice with 20ml of dichloromethane and dried in vacuum to obtain a magnetic Janus powder.
Example 4
To 100ml of refined oily sewage, 0.2g (0.2 wt% with respect to the amount of refined oily sewage) of magnetic Janus particles (such as the magnetic silica/polystyrene-divinylbenzene Janus particles shown in fig. 1) was added and the emulsion was formed by high-speed shearing at a rotation speed of 15000r/min for 1 min. After the system is adsorbed by a 0.8T magnet for 5min, a water phase serving as a continuous phase flows out, so that an enriched emulsion part containing oil stains stabilized by magnetic Janus particles is separated, oil-water separation is realized, and the oil-water separation efficiency is 91%.
To the resulting enriched emulsion fraction, an external magnetic field was applied with a 3T magnet, thereby breaking the enriched emulsion fraction. The magnetic Janus particles were recovered by applying an external magnetic field continuously with a 3T magnet. Further, 100ml of methylene chloride was added to the above magnetic Janus particles, and the mixture was washed twice and dried in vacuum to obtain magnetic Janus powder.
Example 5
To 200ml of refined oily wastewater, 0.4g (0.2% by weight relative to the amount of refined oily wastewater) of non-crosslinked magnetic silica/polystyrene Janus particles was added, and the mixture was stirred at 1000r/min at a high speed for 2min to form an emulsion. After the system is adsorbed by a 0.8T magnet for 5min, a water phase serving as a continuous phase flows out, so that an enriched emulsion part containing oil stains stabilized by magnetic Janus particles is separated, oil-water separation is realized, and the oil-water separation efficiency is 90%.
To the resulting enriched emulsion fraction, an external magnetic field was applied with a 3T magnet, thereby breaking the enriched emulsion fraction. The magnetic Janus particles were recovered by applying an external magnetic field continuously with a 3T magnet. Further, 100ml of methylene chloride was added to the above magnetic Janus particles, and the mixture was washed twice and dried in vacuum to obtain magnetic Janus powder.
It should be noted that the non-crosslinked magnetic Janus particles, while also amphiphilic, can also be used for oil-water separation. However, since the solvent resistance of the non-crosslinked Janus particles is poor, for example, under the action of organic solvents such as N, N-dimethylformamide and tetrahydrofuran, the linear PS can be dissolved or partially dissolved, so that the particle morphology is damaged, and collapse or holes occur, thereby affecting the oil-water separation effect. Thus, non-crosslinked Janus particles are not suitable for certain oil-water two-phase systems. In addition, the recycling times of the non-crosslinked Janus particles can be greatly reduced, and the application of the non-crosslinked Janus particles is limited.
Example 6
To 200ml of refined oily sewage, 0.4g (0.2 wt% with respect to the amount of refined oily sewage) of magnetic Janus particles (such as the magnetic silica/polystyrene-divinylbenzene Janus particles shown in fig. 1) was added and stirred at a high speed of 1000r/min for 2min to form an emulsion. After the system is adsorbed by a 0.8T magnet for 5min, a water phase serving as a continuous phase flows out, so that an enriched emulsion part containing oil stains stabilized by magnetic Janus particles is separated, oil-water separation is realized, and the oil-water separation efficiency is 90%.
To the resulting enriched emulsion fraction, an external magnetic field was applied with a 5T magnet, thereby breaking the enriched emulsion fraction. The magnetic Janus particles were recovered by applying an external magnetic field continuously with a 5T magnet. Further, 100ml of methylene chloride was added to the above magnetic Janus particles, and the mixture was washed twice and dried in vacuum to obtain magnetic Janus powder.
Comparative example 1
To 100ml of refined oily water, 0.2g of magnetic Janus particles (magnetic silica/polystyrene-divinylbenzene Janus particles as shown in FIG. 1) were added and the mixture was sheared at high speed at 12000r/min for 1min to form an emulsion. After the system is adsorbed by a 0.8T magnet for 5min, a water phase serving as a continuous phase flows out, so that an enriched emulsion part containing oil stains stabilized by magnetic Janus particles is separated, oil-water separation is realized, and the oil-water separation efficiency is 77%.
To the resulting enriched emulsion fraction, an external magnetic field was applied with a 3T magnet, thereby breaking the enriched emulsion fraction. The magnetic Janus particles were recovered by applying an external magnetic field continuously with a 3T magnet. Further, 100ml of methylene chloride was added to the above magnetic Janus particles, and the mixture was washed twice and dried in vacuum to obtain magnetic Janus powder.
Comparative example 2
0.4g of magnetic Janus particles (such as the magnetic silica/polystyrene-divinylbenzene Janus particles shown in FIG. 1) was added to 200ml of refined oily water and stirred at 6000r/min for 2min at high speed to form an emulsion. After the system is adsorbed by a 0.8T magnet for 5min, a water phase serving as a continuous phase flows out, so that an enriched emulsion part containing oil stains stabilized by magnetic Janus particles is separated, oil-water separation is realized, and the oil-water separation efficiency is 79%.
To the resulting enriched emulsion fraction, an external magnetic field was applied with a 3T magnet, thereby breaking the enriched emulsion fraction. The magnetic Janus particles were recovered by applying an external magnetic field continuously with a 3T magnet. Further, 100ml of methylene chloride was added to the above magnetic Janus particles, and the mixture was washed twice and dried in vacuum to obtain magnetic Janus powder.
It should be noted that, although the technical solutions of the present invention are described by specific examples, those skilled in the art can understand that the present disclosure should not be limited thereto.
Having described embodiments of the present disclosure, the foregoing description is intended to be exemplary, not exhaustive, and not limited to the disclosed embodiments. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments. The terminology used herein is chosen in order to best explain the principles of the embodiments, the practical application, or improvements made to the technology in the marketplace, or to enable others of ordinary skill in the art to understand the embodiments disclosed herein.
Industrial applicability
The oil-water separation method based on the magnetic Janus particles as the solid emulsifier can be industrially used for oil-water separation of various oil-water mixtures, particularly oil-water mixtures with emulsions.
Claims (8)
1. An oil-water separation method is characterized by comprising the following steps:
a) putting magnetic Janus particles into an oil-water mixture, and emulsifying at 13000-20000 r/min by using a high-speed shearing emulsifying machine or emulsifying at 300-5000 r/min by using a high-speed stirrer to form an emulsion system comprising a continuous phase and a dispersed phase stabilized by the magnetic Janus particles, wherein each magnetic Janus particle simultaneously has a hydrophilic part and a hydrophobic part;
b) applying an external magnetic field A to the emulsion system, causing the dispersed phase to aggregate, to form the emulsion system having an emulsion-enriched portion enriched with the dispersed phase and a liquid portion free of the dispersed phase, thereby separating the emulsion-enriched portion and the liquid portion.
2. The method according to claim 1, wherein the magnetic Janus particles are used in the amount of 0.001 to 5 wt% based on the total weight of the oil-water mixture in the step a).
3. The oil-water separation method according to claim 1 or 2, wherein the magnetic Janus particles are snowman-shaped.
4. The oil-water separation method according to any one of claims 1 to 3, wherein the magnetic field strength of the external magnetic field A in step b) is 0.05T to 2T.
5. The oil-water separation method according to any one of claims 1 to 4, wherein the external magnetic field A is applied for 1 second to 30 minutes in step b).
6. The oil-water separation method according to any one of claims 1 to 5, further comprising the steps of:
c) applying an external magnetic field B having a greater magnetic field strength than the external magnetic field A to the separated emulsion portion enriched in the dispersed phase, thereby breaking the emulsion and recovering the magnetic Janus particles.
7. The oil-water separation method according to claim 6, wherein in the step c), the magnetic field strength of the external magnetic field B is 0.1T to 5T.
8. The oil-water separation method according to any one of claims 1 to 7, wherein the combination of the hydrophilic portion and the hydrophobic portion of the magnetic Janus particles is selected from the group consisting of silica/polystyrene-divinylbenzene, silica/poly (meth) acrylate monomer-divinylbenzene, silica/polystyrene-di (meth) acrylate monomer, silica/poly (meth) acrylate monomer-di (meth) acrylate monomer, silica/polystyrene- (meth) acrylate monomer-di (meth) acrylate monomer, titanium dioxide/polystyrene-divinylbenzene, and mixtures thereof, At least one of titanium dioxide/poly (meth) acrylate monomer-divinylbenzene, titanium dioxide/polystyrene-di (meth) acrylate monomer, and titanium dioxide/poly (meth) acrylate monomer-di (meth) acrylate monomer.
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