CN113230918B - Efficient low-energy-consumption membrane emulsification system and method - Google Patents
Efficient low-energy-consumption membrane emulsification system and method Download PDFInfo
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- CN113230918B CN113230918B CN202110355326.6A CN202110355326A CN113230918B CN 113230918 B CN113230918 B CN 113230918B CN 202110355326 A CN202110355326 A CN 202110355326A CN 113230918 B CN113230918 B CN 113230918B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
- B01F25/40—Static mixers
- B01F25/45—Mixers in which the materials to be mixed are pressed together through orifices or interstitial spaces, e.g. between beads
- B01F25/452—Mixers in which the materials to be mixed are pressed together through orifices or interstitial spaces, e.g. between beads characterised by elements provided with orifices or interstitial spaces
- B01F25/4521—Mixers in which the materials to be mixed are pressed together through orifices or interstitial spaces, e.g. between beads characterised by elements provided with orifices or interstitial spaces the components being pressed through orifices in elements, e.g. flat plates or cylinders, which obstruct the whole diameter of the tube
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
- B01F23/40—Mixing liquids with liquids; Emulsifying
- B01F23/41—Emulsifying
- B01F23/4105—Methods of emulsifying
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
- B01F23/40—Mixing liquids with liquids; Emulsifying
- B01F23/45—Mixing liquids with liquids; Emulsifying using flow mixing
Abstract
The invention discloses a high-efficiency low-energy-consumption membrane emulsification system which comprises a liquid-based porous membrane unit, a disperse phase channel and a continuous phase chamber, wherein the liquid-based porous membrane unit is arranged in a communication path of the disperse phase channel and the continuous phase chamber; the liquid-based porous membrane unit comprises functional liquid and a porous membrane, wherein the functional liquid at least partially infiltrates the porous membrane, and a liquid-liquid interface is formed between the disperse phase liquid and the liquid-based porous membrane unit in the process that the disperse phase liquid enters the continuous phase chamber from the disperse phase channel through the liquid-based porous membrane unit. The invention also discloses an emulsification method thereof. The invention can obviously improve the emulsification quality, reduce the energy consumption and has universality.
Description
Technical Field
The invention relates to the technical field of membrane emulsification, in particular to a high-efficiency low-energy-consumption membrane emulsification system and method.
Background
The emulsification technology has important application value in the fields of food, daily chemicals, petroleum, coating, industrial cleaning and the like, and the emulsification technology is required in ice cream, margarine, cosmetics, oil field displacement and the like. At present, the reported emulsification techniques rely on mechanical stirring, ultrasonic dispersion emulsification, high pressure homogenization, microfluidic droplet technology, membrane emulsification and other emulsification methods. The mechanical stirring method is the most common emulsification technique in factories due to simple operation, but the emulsion droplet size obtained by the mechanical stirring method is usually not uniform, and the size of the emulsion particle size cannot be regulated by setting stirring parameters. Ultrasonic dispersion emulsification and high pressure homogenization require a large amount of energy consumption and noise pollution, and are generally only used for small-scale preparation of emulsions in laboratories. Although the microfluidic droplet technology can prepare the emulsion with uniform particle size, the method needs special chip design and accurate sample injection equipment, has low preparation efficiency and is not suitable for large-scale industrial production.
Membrane emulsification technology is a new emulsification process that has been developed recently and, although it is milder in terms of operating conditions than the previous emulsification techniques, it has more limitations in terms of choice of membrane materials. In addition, the currently reported membrane emulsification techniques have limitations on the type of emulsion preparation. For example, hydrophilic membranes can only be used to prepare O/W (oil-in-water) type emulsions, while hydrophobic membranes can only be used to prepare W/O (water-in-oil) type emulsions. The process of preparing uniform emulsion through the membrane pores by the dispersion phase liquid requires additional energy input such as stirring and the like, which is not in accordance with the current concept of green sustainable development. Therefore, the development of a novel, efficient, energy-saving and universal membrane emulsification technology has important significance for the industrial application of the membrane emulsification technology.
Disclosure of Invention
The invention aims to overcome the defects in the prior emulsification technology and provides a membrane emulsification system and a membrane emulsification method with high efficiency and low energy consumption.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
a high-efficiency low-energy-consumption membrane emulsification system comprises a liquid-based porous membrane unit, a dispersed phase channel and a continuous phase chamber, wherein the liquid-based porous membrane unit is arranged in a communication path of the dispersed phase channel and the continuous phase chamber; the liquid-based porous membrane unit comprises a functional liquid and a porous membrane, wherein the functional liquid at least partially infiltrates the porous membrane, the functional liquid is immiscible with the dispersion phase liquid and the continuous phase liquid, and the porous membrane is a hydrophilic material or a hydrophobic material; the dispersion phase liquid forms a liquid-liquid interface with the liquid-based porous membrane unit in the process of entering the continuous phase chamber from the dispersion phase channel through the liquid-based porous membrane unit.
Optionally, the pore size of the porous membrane is 0.1 μm to 100 μm.
Alternatively, the porous membrane includes a nylon porous membrane, a polyvinylidene fluoride porous membrane, a polytetrafluoroethylene porous membrane, a polypropylene porous membrane, a porous glass membrane, a porous silicon membrane, and a metal porous membrane such as a copper mesh.
Optionally, the functional liquid is an oil-based liquid.
Optionally, the functional liquid is a perfluoropolyether lubricating oil.
Optionally, the wettability of the functional liquid to the porous membrane is higher than the wettability of the dispersed phase liquid to the porous membrane.
Optionally, a surfactant is dispersed in the dispersed phase liquid or the continuous phase liquid, and the surfactant includes anionic, cationic, nonionic, amphoteric surfactants.
Optionally, the apparatus further comprises a main body, the main body comprises two clamping pieces and a sealing material, the two clamping pieces are matched with each other through the sealing material to form a cavity for accommodating the liquid-based porous membrane unit, and the dispersed phase channel and the continuous phase chamber are respectively communicated with the cavity.
An emulsification method based on a membrane emulsification system with high efficiency and low energy consumption is characterized in that a liquid-based porous membrane unit is arranged in a communication path of a dispersed phase channel and a continuous phase chamber; distributing the surfactant in the continuous phase liquid or the dispersed phase liquid; charging a continuous phase liquid into a continuous phase chamber; and driving dispersed phase liquid to pass through the liquid-based porous membrane unit from the dispersed phase channel by adopting pressure to form dispersed phase liquid drops, and then, feeding the dispersed phase liquid drops into the continuous phase chamber.
Optionally, the flow speed of the dispersed phase liquid in the dispersed phase channel is 0.1-5 ml/min.
Alternatively, the dispersed phase liquid and the continuous phase liquid include, but are not limited to, water phase and oil phase liquids such as water, methanol, ethanol, alkanes, olive oil, soybean oil, toluene, methylene chloride, and the like.
The invention provides a membrane emulsification system and a membrane emulsification method, wherein the porous membrane is infiltrated by functional liquid, so that the pressure of dispersed phase liquid passing through the critical threshold of the membrane can be reduced, and further, the energy consumption is reduced; and when the disperse phase passes through the liquid-based porous membrane unit, a thin-layer channel of the functional liquid is formed, the thin-layer channel obstructs the contact between the mobile phase and the surface of the porous membrane, and the excellent anti-fouling performance is given to the substrate of the porous membrane material. The traditional membrane emulsification technology generally needs to be carried out along with stirring, and in the invention, the dispersed phase can directly form emulsion with the mobile phase through the liquid-based porous membrane unit without stirring, thereby avoiding noise generation, further simplifying equipment and reducing energy consumption. The membrane emulsification technology reported at present has limitation on the preparation type of the emulsion due to the limitation of membrane materials, for example, a hydrophilic membrane can only prepare O/W type emulsion, and a hydrophobic membrane can only prepare W/O type emulsion. Aiming at the problems of the membrane emulsification methods, the invention provides a universal membrane emulsification technology, and both hydrophilic membranes and hydrophobic membranes can be used for preparing O/W type emulsions and W/O type emulsions.
The invention has the beneficial effects that:
1. the porous membrane system for infiltrating the functional liquid related to the membrane emulsification technology can obviously reduce the pressure threshold value of the dispersed phase liquid passing through the membrane, thereby reducing the energy consumption.
2. The dispersed phase in the invention passes through the liquid-based porous membrane unit without directly contacting with the porous membrane, and has the advantage of pollution resistance.
3. The dispersed phase can directly form emulsion with the continuous phase through the liquid-based porous membrane unit, the process is simple, stirring is not needed, noise is avoided, and the method has the advantages of no noise, low energy consumption and simplified equipment.
4. The porous membrane soaked with the functional liquid can effectively improve the emulsification quality and effect.
5. The invention has no limit on the selection of the membrane material, and the membrane emulsification technology has universality.
6. The dispersed phase liquid, the continuous phase liquid, the functional liquid and the porous membrane can be selected according to different emulsification requirements, and the applicability is wide.
Drawings
FIG. 1 is a schematic view of an emulsification device according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of an emulsification technique according to an embodiment of the present invention;
FIG. 3 is a photograph showing the appearance of emulsion prepared by impregnating a nylon membrane with the functional liquid K103 of example 2;
FIG. 4 is a graph showing the comparison of the pressure threshold values of emulsions prepared from the nylon membrane impregnated with the functional liquid K103 of example 2;
FIG. 5 is a comparison of the pressure thresholds of emulsions prepared by soaking nylon membranes with the functional liquids K100, K103 and K107 of example 4;
FIG. 6 is an optical micrograph of an emulsion prepared by impregnating a nylon membrane with the functional liquids K100, K103 and K107 of example 4;
FIG. 7 is an optical micrograph of emulsions prepared from liquid-based porous nylon membranes of example 5 with different pore sizes;
FIG. 8 is a photograph of the appearance of emulsions prepared from the functional liquid K100 impregnated hydrophobic PVDF membrane and PVDF membrane of example 6.
Detailed Description
The invention is further explained below with reference to the figures and the specific embodiments.
An efficient and low energy consumption membrane emulsification system of the embodiment is based on the emulsification device shown in fig. 1. The device of the present invention mainly comprises a liquid-based porous membrane unit 1, a main body 5, a dispersed phase channel 6, and a continuous phase chamber 7. The liquid-based porous membrane unit 1 includes a functional liquid 11 and a porous membrane 12, and the functional liquid 11 at least partially infiltrates the porous membrane 12. The main body 5 includes two holding members 51 and a sealing material 52, and the sealing material 52 achieves a sealing effect in cooperation with a portion where the two holding members 51 are connected, forming a cavity for accommodating the liquid-based porous membrane unit 1. The liquid-based porous membrane unit 1 is arranged in a communication path of the disperse phase channel 6 and the continuous phase chamber 7, and the disperse phase channel 6 and the continuous phase chamber 7 are hermetically connected through the two clamping pieces 51, namely the liquid-based porous membrane unit 1 is positioned in a cavity, and the liquid-based porous membrane unit 1 is connected with the disperse phase channel 6 and the continuous phase chamber 7. The functional liquid 11 is immiscible with the dispersed-phase liquid and the continuous-phase liquid. The porous membrane may be a hydrophilic material or a hydrophobic material.
The emulsification principle of the present invention is shown in fig. 2, and the functional liquid 11 infiltrates the porous membrane 12 and the two cooperate to form a stable liquid-based porous membrane unit 1. Under certain pressure, the dispersed phase liquid 3 is dispersed into micro droplets through the liquid-based porous membrane unit 1 from the dispersed phase channel 6 and then enters the continuous phase liquid 4, and emulsion is formed at the interface of the dispersed phase and the continuous phase due to the adsorption effect of surfactant molecules. Wherein a liquid-liquid interface is formed between the dispersed phase liquid 3 and the liquid-based porous membrane unit 1 in the process of entering the continuous phase chamber 7.
The emulsifying method based on the emulsifying system comprises the following steps:
1) selecting a functional liquid, wherein the functional liquid can at least partially infiltrate the hydrophilic or hydrophobic porous membrane and is incompatible with the dispersed phase and the continuous phase liquid;
2) placing the liquid-based porous membrane unit in the body 5;
3) the surfactant molecules are distributed in the continuous phase or the dispersed phase;
4) charging a continuous phase liquid into the continuous phase chamber 7;
5) driven by pressure, the disperse phase liquid flows through the disperse phase channel 6 and forms tiny disperse phase droplets through the liquid-based porous membrane unit 1;
6) the dispersed phase drops enter the continuous phase liquid, and emulsion is formed at the interface of the dispersed phase and the continuous phase due to the adsorption effect of the surfactant molecules.
Example 1
The present emulsification system is used on the basis of an emulsification device as shown in figure 1. The device of the present invention mainly comprises a liquid-based porous membrane unit 1, a main body 5, a dispersed phase channel 6, and a continuous phase chamber 7. The liquid-based porous membrane unit 1 includes a functional liquid 11 and a porous membrane 12, and the functional liquid 11 at least partially infiltrates the porous membrane 12. The main body 5 includes two holding members 51 and a sealing material 52, and the sealing material 52 achieves a sealing effect in cooperation with a portion where the two holding members 51 are connected. A liquid-based porous membrane unit 1 is located within the chamber, and a liquid-based porous membrane unit 2 connects the dispersed phase inlet channel 4 and the continuous phase chamber 3.
The invention provides an efficient and low-energy-consumption emulsification method, which mainly comprises the following necessary steps:
the functional liquid is selected so that it at least partially infiltrates the hydrophilic or hydrophobic porous membrane and is incompatible with the dispersed and mobile phase liquids.
An emulsifying method for preparing n-octane-water emulsion by using anionic surfactant lauryl sodium sulfate. Referring to the emulsification apparatus shown in fig. 1 as a base, a nylon membrane (with a pore size of 1 μm) impregnated with perfluoropolyether lubricant oil (e.g., dupont Krytox 103, abbreviated as K103) was selected as the liquid-based porous membrane unit 1. Selecting the concentration of 1 × 10-3mol/L of aqueous sodium lauryl sulfate solution was added as a continuous phase and added to the continuous phase chamber 7. Normal octane is selected as a dispersed phase, and the dispersed phase passes through the dispersed phase channel 6 at the flow rate of 0.5mL/min and enters the continuous phase chamber 7 to form O/W type emulsion.
Example 2
An emulsifying method for preparing dodecane-water emulsion by using sodium dodecyl sulfate as anionic surfactant. Referring to the emulsification apparatus shown in FIG. 1 as a base, a nylon membrane (pore size 1 μm) impregnated with perfluoropolyether lube K103 was selected as the liquid-based porous membrane unit 1. Selecting the concentration of 1 × 10-3mol/L dodecyl sulfuric acidAqueous sodium solution was added as a continuous phase to the continuous phase chamber 7. Dodecane is selected as a dispersed phase, and the dodecane passes through the dispersed phase channel 6 at the flow rate of 0.5mL/min and enters the continuous phase chamber 7 to form O/W type emulsion. As shown in FIG. 3, the pressure threshold of the conventional nylon membrane is 38kPa, and the pressure threshold of the functional liquid soaked nylon membrane is 30kPa, so that 21% of input energy can be saved by calculation, namely, the energy consumption can be remarkably reduced.
Example 3
An emulsifying method for preparing dodecane-water emulsion from glycolic acid ethoxy-based oil ether serving as a nonionic surfactant. Referring to the emulsification apparatus shown in FIG. 1 as a base, a nylon membrane (pore size 1 μm) impregnated with perfluoropolyether lube K103 was selected as the liquid-based porous membrane unit 1. The concentration is 0.5 multiplied by 10-3mol/L glycolic acid ethoxy base ether aqueous solution was added as a continuous phase and added to the continuous phase chamber 7. Dodecane is selected as a dispersed phase, and the dodecane passes through the dispersed phase channel 6 at the flow rate of 0.5mL/min and enters the continuous phase chamber 7 to form O/W type emulsion. As shown in FIG. 4, the pressure threshold of the conventional nylon membrane and the pressure threshold of the functional liquid-infiltrated nylon membrane are both 58.4kPa and 46.7kPa, and 20% of input energy can be saved by calculation.
Example 4
An emulsifying method for preparing dodecane-water emulsion by using different functional liquids. Referring to the emulsification apparatus shown in fig. 1, nylon membranes (pore size 1 μm) impregnated with different functional liquids (perfluoropolyether lubricants, dupont Krytox 100, dupont Krytox 103, and dupont Krytox107, abbreviated as K100, K103, and K107, respectively) were used as the liquid-based porous membrane unit 1. The concentration is 0.5 multiplied by 10-3mol/L glycolic acid ethoxy base ether aqueous solution was added as a continuous phase and added to the continuous phase chamber 7. Dodecane is selected as a dispersed phase, and the dodecane passes through the dispersed phase channel 6 at the flow rate of 0.5mL/min and enters the continuous phase chamber 7 to form O/W type emulsion. As shown in FIG. 5, the pressure threshold values of the nylon membranes soaked by the functional liquids K100, K103 and K107 are respectively 43.3kPa, 46.7kPa and 48.8kPa, the pressure threshold value of the traditional nylon membrane is 58.4kPa, and the soaking of the functional liquids K100, K103 and K107 into nylon is calculatedThe dragon film can save input energy by 25%, 20% and 16% respectively. As shown in FIG. 6, the average particle sizes of the droplets of the emulsions prepared from K100, K103 and K107 are 103 μm, 109 μm and 96 μm, respectively, and the average particle size of the droplets of the emulsions prepared from the conventional nylon membrane (with a pore size of 1 μm) is 145 μm, so that the nylon membrane impregnated with the functional liquid can effectively reduce the droplet size, i.e., enhance the emulsification effect.
Example 5
An emulsifying method for preparing dodecane-water emulsion with different particle sizes by using nonionic surfactant glycolic acid ethoxy base oil ether. Based on the emulsifying device shown in FIG. 1, functional liquid K103 was selected to infiltrate nylon membranes (0.45 μm, 1 μm, 5 μm, 8 μm) with different pore sizes. The concentration is 0.5 multiplied by 10-3mol/L glycolic acid ethoxy base ether aqueous solution was added as a continuous phase and added to the continuous phase chamber 7. Dodecane is selected as a dispersed phase, and the dodecane passes through the dispersed phase channel 6 at the flow rate of 0.5mL/min and enters the continuous phase chamber 7 to form O/W type emulsion. As shown in FIG. 7, the average particle diameters of the emulsion droplets prepared from the nylon membranes of 0.45 μm, 1 μm, 5 μm and 8 μm were 68 μm, 109 μm, 205 μm and 381 μm, respectively, and the emulsion particle diameters increased as the membrane pore diameters increased. The method provides a means of controlling the size of the emulsion droplets by adjusting the membrane pore size.
Example 6
An emulsifying method for preparing dodecane-water emulsion from glycolic acid ethoxy-based oil ether serving as a nonionic surfactant. Referring to the emulsification apparatus shown in fig. 1 as a basis, a hydrophobic PVDF membrane (with a pore size of 1 μm) impregnated with a functional liquid K100 was selected as the liquid-based porous membrane unit 1. The concentration is 0.5 multiplied by 10-3mol/L glycolic acid ethoxy base ether aqueous solution was added as a continuous phase and added to the continuous phase chamber 7. Dodecane is selected as a dispersed phase, and the dodecane passes through the dispersed phase channel 6 at the flow rate of 0.5mL/min and enters the continuous phase chamber 7 to form O/W type emulsion. As shown in FIG. 8, the O/W type emulsion can be formed by wetting the hydrophobic PVDF film with the functional liquid, whereas the O/W type emulsion cannot be formed by the conventional hydrophobic PVDF film.
Example 7
An emulsifying method for preparing dodecane-water emulsion by using non-ionic surfactant span 80. Referring to the emulsification apparatus shown in FIG. 1 as a base, a stainless steel mesh membrane (pore size 1 μm) impregnated with perfluoropolyether lube K100 was selected as the liquid-based porous membrane unit 1. Span 80, at a concentration of 1% (mass fraction), was dissolved in dodecane and added as a continuous phase aqueous solution as a continuous phase and into the continuous phase chamber 7. Water is selected as a dispersed phase, and the water passes through a dispersed phase channel 6 at a flow rate of 0.5mL/min and enters a continuous phase chamber 7 to form a W/O type emulsion.
The above embodiments are only used to further illustrate the efficient and low energy consumption membrane emulsification system and method of the present invention, but the present invention is not limited to the embodiments, and any simple modifications, equivalent changes and modifications made to the above embodiments according to the technical spirit of the present invention fall within the protection scope of the technical solution of the present invention.
Claims (10)
1. A high-efficiency low-energy-consumption membrane emulsification system is characterized in that:
the device comprises a liquid-based porous membrane unit, a disperse phase channel and a continuous phase chamber, wherein the liquid-based porous membrane unit is arranged in a communication path of the disperse phase channel and the continuous phase chamber;
the liquid-based porous membrane unit comprises a functional liquid and a porous membrane, wherein the functional liquid at least partially infiltrates the porous membrane, the functional liquid is immiscible with the dispersion phase liquid and the continuous phase liquid, and the porous membrane is a hydrophilic porous membrane material or a hydrophobic porous membrane material; the dispersion phase liquid forms a liquid-liquid interface with the liquid-based porous membrane unit in the process of entering the continuous phase chamber from the dispersion phase channel through the liquid-based porous membrane unit.
2. The high efficiency, low energy consumption membrane emulsification system according to claim 1 wherein: the pore diameter of the porous membrane is 0.1-100 μm.
3. The high efficiency, low energy consumption membrane emulsification system according to claim 1 wherein: the porous membrane includes a nylon porous membrane, a polyvinylidene fluoride porous membrane, a polytetrafluoroethylene porous membrane, a polypropylene porous membrane, a porous glass membrane, a porous silicon membrane, and a metal porous membrane.
4. The high efficiency, low energy consumption membrane emulsification system according to claim 1 wherein: the functional liquid is an oil-based liquid.
5. The high efficiency, low energy consumption membrane emulsification system according to claim 4 wherein: the functional liquid is a perfluoropolyether lubricating oil.
6. The high efficiency low energy consumption membrane emulsification system according to claim 1, wherein: the wettability of the functional liquid to the porous membrane is stronger than the wettability of the dispersed phase liquid to the porous membrane.
7. The high efficiency, low energy consumption membrane emulsification system according to claim 1 wherein: the dispersed phase liquid or the continuous phase liquid is dispersed with a surfactant, and the surfactant comprises anionic, cationic, nonionic and amphoteric surfactants.
8. The high efficiency, low energy consumption membrane emulsification system according to claim 1 wherein: the main body comprises two clamping pieces and sealing materials, the two clamping pieces are matched through the sealing materials to form a cavity for containing the liquid-based porous membrane unit, and the disperse phase channel and the continuous phase chamber are respectively communicated with the cavity.
9. An emulsification method based on the membrane emulsification system according to any one of claims 1 to 8, wherein: installing a liquid-based porous membrane unit in a communication path of the dispersed phase channel and the continuous phase chamber; distributing the surfactant in the continuous phase liquid or the dispersed phase liquid; charging a continuous phase liquid into a continuous phase chamber; and driving dispersed phase liquid to pass through the liquid-based porous membrane unit from the dispersed phase channel by adopting pressure to form dispersed phase liquid drops, and then, feeding the dispersed phase liquid drops into the continuous phase chamber.
10. The emulsification method according to claim 9, wherein: the flow velocity of the dispersed phase liquid in the dispersed phase channel is 0.1-5 ml/min.
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