An emulsification system and method for preparing high internal phase emulsions in a continuous cutting environment

By combining a premixing device with a rotary emulsifying device, and utilizing concentric rotating packing layers and a jet-type liquid distributor, the problem of uneven shearing of the emulsifying equipment under a continuous cutting environment is solved, and efficient and stable preparation of high internal phase emulsions is achieved, thereby improving production efficiency and product quality.

CN118949733BActive Publication Date: 2025-10-14BEIJING UNIV OF CHEM TECH
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Patent Information

Application Number
CN202410907556.2
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-07-08
Publication Date
2025-10-14
Estimated Expiration
2044-07-08

AI Technical Summary

Technical Problem

Existing emulsification equipment has uneven shear space distribution during continuous operation, low emulsification efficiency, unstable product quality, and is difficult to meet continuous production requirements.

Method used

A premixing device is used for preliminary emulsification, and the concentrically arranged rotating packing layer and jet liquid distributor of the rotating emulsifying device are combined to achieve efficient and uniform liquid feeding and cutting. The independent control of the multi-layer flow channel ensures the consistency of shear strength and residence time.

Benefits of technology

It achieves efficient and stable preparation of high internal phase emulsion, improves production efficiency and product quality, and is particularly suitable for large-scale preparation of high-viscosity emulsions.

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Abstract

The application discloses an emulsification system and a preparation method of high internal phase emulsion in a continuous cutting environment, wherein the emulsification system comprises a premixing device for premixing raw materials to obtain a mixed liquid, a rotary emulsification device capable of rotating around an axis, the rotary emulsification device comprising a plurality of concentric rotary packing layers, each rotary packing layer being provided with an independent flow channel, the flow channel comprising opposite feeding ports and discharging ports, and a feeding mechanism, a plurality of feeding mechanisms being respectively arranged at the inner periphery or the outer periphery of each rotary packing layer to supply the mixed liquid to the feeding ports. The high internal phase emulsion product with uniform particle size and good stability can be produced by adopting a continuous operation mode and by accurately controlling process parameters such as continuous rotary cutting speed and temperature. Compared with traditional emulsification equipment, the system has high efficiency and wide application range, and is especially suitable for scale preparation of high-viscosity emulsion.
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Description

TECHNICAL FIELD

[0001] The present application relates to the field of emulsification, and more particularly, to an emulsification system and a method for preparing high internal phase emulsions in a continuous cutting environment. BACKGROUND

[0002] Emulsification is a common chemical unit operation, which is widely used in many industrial fields such as new chemical materials, food, cosmetics, paints, etc. The emulsification process is to forcibly mix two immiscible liquids through mechanical force or chemical means to form a dispersed phase uniformly dispersed in a continuous phase. Good emulsification effect can not only improve the stability and sensory performance of the product, but also how to design an efficient and reliable emulsification device has been one of the research hotspots in the chemical field.

[0003] The traditional emulsification device mostly adopts intermittent operation in the actual operation process, and needs to be stopped regularly for cleaning and maintenance, which has low production efficiency and is difficult to meet the requirements of continuous production. The existing continuous emulsification equipment has the problems of uneven shear space distribution, low emulsification efficiency in a continuous cutting environment, unstable product quality, and poor product quality repeatability.

[0004] Therefore, it is urgent to develop an efficient and stable emulsification system and a method for preparing high internal phase emulsions in a continuous cutting environment. SUMMARY

[0005] The purpose of the present application is to provide an efficient and stable emulsification system and a method for preparing high internal phase emulsions in a continuous cutting environment.

[0006] The first aspect of the present application provides an emulsification system, comprising a premixing device for premixing raw materials to obtain a mixed liquid; a rotary emulsification device rotatable about its axis; the rotary emulsification device comprises a plurality of concentric rotary packing layers, each rotary packing layer is provided with an independent flow channel, and the flow channel comprises opposite feed ports and discharge ports; a plurality of feeding mechanisms are arranged at the inner or outer periphery of each rotary packing layer to supply the mixed liquid to the feed ports.

[0007] Optionally, the feeding mechanism comprises a jet liquid distributor, which uniformly distributes the mixed liquid between the rotary packing layers.

[0008] Optionally, the jet liquid distributor uniformly distributes the mixed liquid between the rotary packing layers in the form of high-pressure spraying.

[0009] Optionally, the premixing device comprises a roller extrusion device, the roller extrusion device comprises a roller and an extrusion screw located inside the roller, the side wall of the roller is provided with a discharge gap, and the extrusion screw cooperates with the roller to extrude the mixed liquid from the discharge gap.

[0010] Optionally, the premixing device further comprises a collection groove and a cooling structure installed on the collection groove, the collection groove is used for collecting the mixed liquid extruded from the discharge gap, and the cooled mixed liquid is supplied to the feeding mechanism.

[0011] Optionally, the roller extrusion device comprises a pair of planetary rollers or double helix rollers.

[0012] Optionally, the flow channels are bent and staggered from the feeding port to the discharging port.

[0013] Optionally, each rotating packing layer comprises a plurality of flow channels, and the feeding port of each flow channel corresponds to one feeding mechanism.

[0014] Optionally, the plurality of flow channels are uniformly distributed in the circumferential direction of the rotating packing layer.

[0015] The second aspect of the present application provides a method for preparing high internal phase emulsion in a continuous cutting environment, which uses the emulsifying system of any one of the first aspect of the present application, and the method comprises: preliminarily emulsifying two-phase fluid through the premixing device, after preliminary emulsification, high-pressure atomization spraying through the jet liquid distributor and entering the flow channels of the plurality of concentrically arranged rotating packing layers through the feeding port, and realizing high-efficiency emulsification under the action of high-speed rotation of the rotating emulsifying device.

[0016] According to the technical content disclosed in the present application, the following beneficial effects are achieved:

[0017] The emulsifying system provided by the present application uses the premixing device to premix raw materials to obtain a mixed liquid, thereby providing a more stable and uniform raw material basis for the subsequent high-speed emulsification process; the plurality of feeding mechanisms are arranged at the inner circumferences of each rotating packing layer to supply the mixed liquid to the feeding port. The feeding mechanisms arranged between the rotating packing layers realize uniform feeding of the feeding liquid, increase the liquid-liquid contact area, and promote the emulsification reaction of the high internal phase emulsion; the rotating emulsifying device comprises a plurality of concentrically arranged rotating packing layers, each rotating packing layer is provided with an independent flow channel, and the flow channel comprises opposite feeding ports and discharging ports; the regular structure of the plurality of concentrically arranged rotating packing layers of the rotating emulsifying device is beneficial to forming a uniform flow field distribution, ensuring that the shear strength and residence time of each region are relatively consistent during the entire emulsification process, and the high-speed rotation of the rotating packing layer also generates centrifugal force, which further promotes the full contact and emulsification of the two phases. The system adopts a continuous operation mode, and through accurate control of process parameters such as continuous rotation cutting speed and temperature, a high internal phase emulsion product with uniform particle size and good stability can be produced. Compared with traditional emulsifying equipment, the system has high efficiency and wide application range, and is especially suitable for scale preparation of high-viscosity emulsion.

[0018] Other features and advantages of the present application will become apparent from the following detailed description of exemplary embodiments thereof, with reference to the accompanying drawings. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and, together with the description, serve to explain the principles of the invention.

[0020] Figure 1 It is a schematic structural diagram of the premixing device of the present invention.

[0021] Figure 2 It is a schematic structural diagram of the rotary emulsification device of the present invention.

[0022] Explanation of the reference numerals: 11, liquid inlet; 12, extrusion screw; 13, discharge gap; 14, roller; 15, motor; 16, collecting tank; 21, rotating packing layer; 22, jet liquid distributor. DETAILED DESCRIPTION

[0023] Various exemplary embodiments of the present invention will now be described in detail with reference to the accompanying drawings. It should be noted that unless otherwise specifically stated, the relative arrangement of components and steps, numerical expressions and numerical values ​​set forth in these embodiments do not limit the scope of the present invention.

[0024] The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses.

[0025] Technologies, methods, and equipment known to ordinary technicians in the relevant art may not be discussed in detail, but where appropriate, the technologies, methods, and equipment should be considered part of the specification.

[0026] In all examples shown and discussed herein, any specific values ​​should be interpreted as merely exemplary and not limiting. Therefore, other examples of the exemplary embodiments may have different values.

[0027] It should be noted that like reference numerals and letters refer to like items in the following figures, and therefore, once an item is defined in one figure, it need not be further discussed in subsequent figures.

[0028] See also Figure 1 and Figure 2 The present invention discloses an emulsification system, including a premixing device, a rotary emulsifying device and a feeding mechanism.

[0029] The premixing device is arranged in a previous process of the rotary emulsifying device, and is used for premixing raw materials to obtain a mixed liquid. The premixing device comprises a roller extrusion device and a collecting tank 16. The roller extrusion device comprises a roller 14 and an extrusion screw 12 arranged inside the roller 14. The roller 14 is provided with a liquid inlet 11 on a barrel wall of the roller 14. The liquid inlet 11 comprises a single-phase liquid inlet and a two-phase liquid inlet after premixing. The roller 14 is provided with a discharging gap 13 on a side wall. The extrusion screw 12 cooperates with the roller 14 to extrude the mixed liquid from the discharging gap 13. The mixed liquid is discharged from the discharging gap 13 through rotary extrusion, which further increases the mixing and shearing effect of the raw materials in the roller 14, so that the preliminary emulsification is more thorough. The design of the screw extrusion can increase the residence time of the raw materials in the roller 14, thereby further promoting the mixing and emulsification effect of the raw materials. At the same time, through rotary extrusion, the raw materials are more fully extruded and sheared in the discharging gap 13, so that the particles are more delicate, the interface is more dispersed, and the emulsification effect and rheological property improvement are further improved. Such a design not only improves the emulsification efficiency of the premixing device, but also provides a more stable and uniform raw material basis for the subsequent high-speed emulsification process of the rotary emulsifying device, thereby comprehensively improving the performance of the entire emulsifying device. In some embodiments, the roller 14 extrusion device comprises a pair of planetary roller 14 or a double-screw roller 14.

[0030] A cooling structure is mounted on the collecting tank 16. The collecting tank 16 is used for collecting the mixed liquid extruded from the discharging gap 13 and supplying the cooled mixed liquid to the feeding mechanism. The cooling structure can ensure that the emulsion realizes good shearing at a lower viscosity. Cooling can keep the emulsion stable and prevent demulsification. When the temperature rises, the emulsifier affinity will decrease, the stability of the emulsion will be destroyed, and the interfacial tension between the dispersed phase and the continuous phase will also decrease, resulting in demulsification.

[0031] The rotating emulsification device is driven to rotate by the motor 15 at a rotating speed of 200-1200 r / min, and the rotating speed of the rotating emulsification device can be accurately controlled by adjusting the rotating speed of the motor 15 or the transmission ratio of the transmission device. In this embodiment, the rotating emulsification device includes three concentrically arranged rotating packing layers 21 and a bearing located at the center of the rotating emulsification device, the bearing is connected with the output shaft of the motor 15 to drive the rotating emulsification device to rotate. In some embodiments, each rotating packing layer 21 can be driven by an independent motor for independent control. The actual working condition is reasonably selected. Each rotating packing layer 21 is provided with an independent flow channel, and each rotating packing layer 21 includes a plurality of flow channels. The flow channel includes opposite inlet and outlet, and the mixed liquid can flow out from the outlet located at the inner edge and / or the outer edge of the packing layer 21, and then flow into the collecting container by gravity; the plurality of flow channels are uniformly distributed in the circumferential direction of the rotating packing layer 21, and the inlet of each flow channel corresponds to one feeding mechanism, or the inlets of the plurality of flow channels share one feeding mechanism; the flow channel is provided with staggered flow tracks, specifically, the flow channel is bent and staggered from the inlet to the outlet to increase the residence time, and the rotating speed of the whole paragraph can be accurately adjusted to realize fine shear force control; more specifically, the flow channel is provided with staggered flow tracks, and the staggered structure refers to that the rotating packing layer 21 is designed as a mutual embedding structure, and the middle layer is provided with a baffle to change the flow path and prolong the residence time.

[0032] The three concentrically arranged rotating packing layers 21 are the core components of the rotating emulsification device. The rotating packing layer 21 adopts a concentric circle multi-section structure to form a plurality of independent flow channels. The mixed liquid (such as oil phase and water phase) to be emulsified enters the central region of the rotating packing layer 21 through the inlet. The plurality of rotating packing layers 21 are driven to rotate at high speed by the motor 15. The mixed liquid is thrown to the periphery and enters the plurality of independent flow channels of the rotating packing layer 21. Each flow channel forms an independent flow region. The rotating speed of the rotating packing layer 21 is accurately controlled by adjusting the rotating speed of the motor 15. The flow rate and residence time of the raw materials in each flow channel can be adjusted. After the segmented emulsification, the emulsified product is output from the outlet at the periphery of the rotating packing layer 21 and enters the next process. The multi-channel regular rotating packing layer 21 of the rotating emulsification device can realize segmented flow and independent control of the raw materials, and greatly improves the flexibility and adaptability of the emulsification device.

[0033] The feeding mechanism selects a pressurized jet liquid distributor 22, and multiple jet liquid distributors 22 are arranged in the annular space between the three-layer spaced rotating packing layers 21 respectively to supply the mixed liquid to the feed port of the rotating packing layer 21. Specifically, multiple pressurized jet liquid distributors 22 are uniformly arranged along the circumferential direction between the outermost rotating packing layer 21 and the intermediate rotating packing layer 21 and between the intermediate rotating packing layer 21 and the innermost rotating packing layer 21, respectively. The jet liquid distributor 22 uniformly distributes the two-phase fluid (mixed liquid) into each rotating packing layer 21 (among) by high-pressure jetting and enters the flow channel from the feed port, wherein the feed port of the flow channel of the outermost rotating packing layer 21 and the intermediate rotating packing layer 21 is located at the inner edge, and the feed port of the innermost rotating packing layer 21 is located at the outer edge. The jetting pressure of the jet liquid distributor 22 can be independently adjusted to meet the needs under different working conditions. The jetting direction of the jet liquid distributor 22 matches the arrangement of the flow channel of the rotating packing layer 21 to realize seamless connection. The jet liquid distributor 22 ensures that the two-phase fluid enters each rotating packing layer 21 at a uniform speed and pressure, avoiding uneven liquid flow between different flow channels. Due to the high-pressure jetting distribution of the jet liquid distributor 22, the liquid can be fully atomized and uniformly distributed between the rotating packing layers 21, thereby greatly increasing the liquid-liquid contact area. Through the operation of the jet liquid distributor 22, uniform raw material feeding and sufficient liquid-liquid contact are provided for the subsequent emulsification reaction, which is beneficial to the efficient performance of the emulsification reaction.

[0034] The second aspect of the application provides a method for preparing high internal phase emulsions in a continuous cutting environment, which uses the emulsification system of any one of the first aspect of the application. The method comprises: preliminarily emulsifying the two-phase fluid through the premixing device. After preliminary emulsification, high-pressure atomization jetting is performed by the jet liquid distributor 22, and the mixed liquid enters the flow channel of the multiple concentric rotating packing layers 21 through the feed port. Under the action of high-speed rotation of the rotating emulsification device, efficient emulsification is realized.

[0035] The whole process is as follows: the two-phase fluid is preliminarily emulsified by the premixing device. In this device, the raw material is extruded out of the discharge gap 13 after being extruded by the spiral rotating extruder, realizing deep preliminary emulsification. Then, after cooling in the collection tank 16, the raw material enters the rotating emulsification device, and further efficient emulsification is realized under the action of high-speed rotation and pressure-jet distribution. In this process, the raw material is continuously cut, and the regular structure of the rotating packing layer 21 is beneficial to the formation of uniform flow field distribution, ensuring that the shear strength and residence time of each region in the whole emulsification process are relatively consistent. Finally, the emulsion product after efficient emulsification has good quality stability. The whole process realizes the continuous and efficient emulsification process through the organic combination of the premixing device and the rotating emulsification device, providing a reliable guarantee for the production of high-quality emulsion products.

[0036] Case Study 1: Utilizing a continuous shearing process for emulsification of a high internal phase emulsion, including a drum 14 extrusion premixing unit and a rotary emulsifier, a water-in-oil emulsion was prepared with a specific composition of 2:1 by volume. The water phase consisted of an aqueous solution containing 30-40% silica sol, the oil phase consisted of one or more monomers such as acrylate, polyurethane acrylate, and epoxy resin, and the solvents included toluene, cyclohexane, etc. The preparation process involved adding an emulsifier such as SPAN80 to the oil phase, followed by premixing with the water phase via drum 14 shearing. The premixed phases were then conveyed to a high-rotation emulsifier (1000 rpm) where the emulsified droplets were continuously sheared. The resulting emulsion had a uniform and fine appearance, a particle size of 0.2-2 μm, excellent stability, and a smooth texture. Hourly production capacity reached 20-30 kg.

[0037] The emulsification system and method provided by the present invention generally process objects including two-phase liquid systems, that is, systems composed of two immiscible liquids. Such liquid-liquid systems include but are not limited to oil-water emulsion systems, solvent-water emulsion systems, emulsion systems of organic phase and aqueous phase, etc. In the fields of new chemical materials, food, cosmetics, medicine and industry, these high-viscosity liquid-liquid systems often need to be efficiently emulsified to obtain stable emulsified products. The emulsification device and process of the present invention are suitable for processing these two-phase liquid systems. Through the innovative design of the device structure and process flow, efficient and stable emulsification reactions are achieved, thereby improving production efficiency and product quality.

[0038] In summary, the emulsification system provided by the present invention is composed of a segmented structure of concentric multi-stage rotating packing layers 21, which improves the emulsification efficiency and adaptability. A pressurized jet liquid distributor 22 is arranged between the rotating packing layers 21 to achieve uniform feeding of the liquid, increase the liquid-liquid contact area, and promote the emulsification reaction of the high internal phase emulsion. A roller 14 extrusion premixing device is provided in front of the emulsification device to achieve preliminary emulsification through gap collision. The system is conducive to achieving segmented emulsification and independent control through segmented flow channel design and high-speed rotation, thereby improving emulsification efficiency and product quality. The entire process includes preliminary emulsification, efficient emulsification and uniform flow field distribution, and finally obtains an emulsion product with good quality stability. These innovative designs effectively solve the challenges of traditional emulsification devices in a continuous cutting environment, provide a reliable solution for improving the uniform emulsification of high internal phase emulsions, and have broad application prospects.

[0039] Although some specific embodiments of the present invention have been described in detail by way of examples, it should be understood by those skilled in the art that the above examples are for illustration only and are not intended to limit the scope of the present invention. It should be understood by those skilled in the art that modifications may be made to the above embodiments without departing from the scope and spirit of the present invention. The scope of the present invention is defined by the appended claims.

Claims

1. An emulsification system, characterized in that: include: A premixing device, used to premix the raw materials to obtain a mixed liquid; A rotary emulsifying device that can rotate around its axis; The rotary emulsifying device comprises a plurality of concentrically arranged rotating packing layers, each of the rotating packing layers is provided with an independent flow channel, and the flow channel comprises a relative feed port and a discharge port; A feeding mechanism, wherein a plurality of feeding mechanisms are respectively arranged on the inner periphery or the outer periphery of each rotating packing layer to supply the mixed liquid to the feed port; The feeding mechanism includes a jet liquid distributor, which evenly distributes the mixed liquid between each of the rotating packing layers; The premixing device includes a roller extrusion device, which includes a roller and an extrusion screw located inside the roller. The side wall of the roller is provided with a discharge gap. The extrusion screw cooperates with the roller to extrude the mixed liquid from the discharge gap. The flow channel extends from the feed port to the discharge port in a bent and staggered manner.

2. The emulsification system according to claim 1, characterized in that: The jet-type liquid distributor evenly distributes the mixed liquid between the rotating packing layers in the form of high-pressure spray.

3. The emulsification system according to claim 1, characterized in that: The premixing device further includes a collecting tank and a cooling structure installed on the collecting tank. The collecting tank is used to collect the mixed liquid squeezed out from the discharge gap and supply the cooled mixed liquid to the feeding mechanism.

4. The emulsification system according to claim 1, characterized in that: Each rotating packing layer includes a plurality of flow channels, and the feed port of each flow channel corresponds to one feeding mechanism.

5. The emulsification system according to claim 4, characterized in that: The plurality of flow channels are evenly distributed in the circumferential direction of the rotating packing layer.

6. A method for preparing a high internal phase emulsion under a continuous cutting environment, characterized in that: The method uses the emulsification system according to any one of claims 1 to 5, and the method comprises: The two-phase fluid is preliminarily emulsified through the premixing device. After the preliminarily emulsified, the fluid is sprayed by the high-pressure atomization of the jet-type liquid distributor and enters the flow channel of the multiple concentrically arranged rotating packing layers through the feed port. Under the high-speed rotation of the rotating emulsifying device, efficient emulsification is achieved.

Citation Information

Patent Citations

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