A pathway structure for an interlocking conical array plate, its fabrication and application.
By modifying the pathway structure of the intercalation-type conical array plate and using 3D printing technology to prepare hydrophobic conical array plates, the problem of low oil-water emulsion separation efficiency in the existing technology is solved, achieving efficient, rapid and continuous oil-water separation effect, which is suitable for the separation of emulsions containing surfactants.
Patent Information
- Application Number
- CN202210122215.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2022-02-09
- Publication Date
- 2025-10-31
- Estimated Expiration
- 2042-02-09
AI Technical Summary
Existing technologies are insufficient for efficiently, rapidly, and continuously separating oil-water emulsions from oily wastewater, especially emulsions containing surfactants. Furthermore, traditional methods suffer from poor separation performance, high energy consumption, and susceptibility to contamination.
A hydrophobic conical array plate is fabricated using 3D printing technology to create a channel structure with interlocking conical array plates. The surface texture of the conical array is used to capture oil droplets, which are then directionally transported to the root of the array under the drive of Laplace pressure difference, thereby achieving oil-water separation and increasing the contact area and separation efficiency.
It achieves efficient, rapid, and continuous oil-water emulsion separation, especially suitable for emulsions containing surfactants, with a separation efficiency of over 98%. It is low in cost, low in energy consumption, easy to clean, and suitable for large-scale preparation.
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Figure CN116603274B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of functional materials technology. More specifically, it relates to a pathway structure for an interlocking conical array plate, its fabrication, and its application. Background Technology
[0002] With industrial development, clean water resources, especially potable freshwater resources, are becoming increasingly scarce. How to recover and treat clean water from industrial wastewater for continued use has become a key research focus. Traditional industrial wastewater is often oily, and oil-water emulsions, due to their small size and high stability, pose a significant challenge for oil-water separation. Furthermore, the use of large amounts of surfactants in industrial production further increases the stability of oily wastewater. Traditional separation methods such as gravity settling, adsorption, and flotation are only suitable for separating oil-water mixtures and not for emulsion separation. Currently, membrane separation is the most commonly used method for emulsion separation. Many types of membranes have been reported, such as all-inorganic membranes (Sci Rep 5, 9688 (2015)) and organic membranes (RSC Adv., 2015, 5, 57101-57113), which mainly achieve emulsion separation based on the size sieving effect. However, common membrane separation methods are difficult to use for continuous separation of large volumes of wastewater, and often require cleaning and replacement. This can lead to untimely wastewater treatment, affect production progress, or result in poor performance in separating surface-active oil-water emulsions, low separation cycle count, high energy consumption, secondary pollution, and an inability to efficiently and quickly treat emulsified oily wastewater. To overcome these problems, researchers recently reported an oil-water separation tube with a hydrophobic and oleophilic surface. By utilizing copper-containing nanorod structures on a conical array inside the tube to puncture oil droplets, the droplets are then directed to the root of the conical array under the drive of the Laplace pressure difference. The oil droplets then pass through the metal mesh of the substrate, achieving oil-water separation. However, the contact area between the conical array and the oil-water emulsion in this oil-water separation tube is relatively small, and the sidewalls are not sealed. There is a risk that when the oil-water separation tube is long, the inlet pressure may be increased to ensure the outlet flow rate, causing the sidewalls to be subjected to greater pressure and potentially leading to leakage.
[0003] Therefore, it is very important to study an oil-water separation device with good separation effect, fast separation speed, large processing capacity, continuous processing capability, large contact area, and good sealing performance. Summary of the Invention
[0004] Based on the above-mentioned shortcomings, the first objective of this invention is to provide a pathway structure for a mating conical array plate. This pathway structure of the mating conical array plate has excellent separation effect on oil-water emulsions such as n-hexane, gasoline, diesel, and silicone oil, and is especially suitable for the separation of oil-water emulsions containing surfactants. It can perform continuous separation, is easy to clean, and has the advantages of high separation efficiency, fast separation speed, good stability, and environmental friendliness.
[0005] A second objective of this invention is to provide a method for preparing the aforementioned pathway structure. This pathway structure of the interlocking conical array plate is inexpensive to manufacture, uses readily available raw materials, has a simple manufacturing process, and can be used for large-scale production.
[0006] The third objective of this invention is to provide an application of the above-described pathway structure in oil-water separation.
[0007] To achieve the first objective mentioned above, the present invention adopts the following technical solution:
[0008] This invention provides a passage structure for interlocking conical array plates, comprising a first conical array plate and a second conical array plate arranged in an interlocking configuration, a passage structure formed by the interlocking of the first and second conical array plates, and an inlet and an outlet provided on the outer wall of the passage structure; wherein,
[0009] The first conical array plate includes a first substrate and a first conical array arranged in a honeycomb pattern thereon; the second conical array plate includes a second substrate and a second conical array arranged in a honeycomb pattern thereon; the cone height, the spacing between adjacent cones, and the diameter of the cone bottom are on the millimeter scale, and the cone surface texture is on the micrometer scale.
[0010] The pathway structure is U-shaped and its inner surface is hydrophobic.
[0011] The interlocking conical array plate pathway structure provided by this invention effectively utilizes the surface texture and protrusions of the conical array to achieve collision and capture of oil droplets in the flowing emulsion. Driven by the Laplace pressure difference, the oil droplets are then directionally transported to the root of the conical array for collection. The collected oil droplets converge to form an oil film, which floats on the water layer and is discharged out of the pathway with the liquid flow, achieving oil-water separation. The interlocking first and second conical array plates increase the collision area with oil droplets in the flowing emulsion, increasing the collision probability within a limited pathway length, thus providing a prerequisite for further improving separation efficiency.
[0012] Furthermore, the oil phase in the oil-water emulsion includes, but is not limited to, one or more of the following: n-hexane, n-hexadecane, isooctane, gasoline, diesel, and silicone oil.
[0013] Furthermore, the cone height of the first and second cone arrays is 1-8 mm, the distance between adjacent cones is 1-4 mm, and the diameter of the cone bottom is 0.5-2 mm.
[0014] In one specific embodiment, the formed flow path is a loop-shaped path. Other shapes of flow paths can also be designed by adjusting the interlocking form of the first and second conical array plates. The purpose is to design a longer path length within a limited overall size to increase the chance of collision and capture of oil droplets in the flowing emulsion by the conical array.
[0015] Furthermore, the first and second conical array plates are made of Anycubic photosensitive resin, a common rigid photosensitive resin used in 3D printing technology.
[0016] Furthermore, the area of the pathway structure is 162–648 cm². 2 .
[0017] Furthermore, when the area of the pathway structure is 162–324 cm² 2 At this time, the separation efficiency of oil-water emulsion is 93%-95%; preferably, when the area of the passage structure is 324-486 cm². 2 At this time, the separation efficiency of oil-water emulsion is 95%-98%; preferably, the area of the passage structure is 486-648 cm². 2 At that time, the separation efficiency of oil-water emulsion was 98%-99%.
[0018] It should be noted that in this invention, the area is 162cm². 2 The separation performance of the pathway structure is considered as a unit processing area. Under one unit processing area, multiple length-width combinations can be designed, such as 18cm*9cm, 27cm*6cm, 54cm*3cm, etc. When the pathway structure is 18cm*9cm, a separation efficiency of not less than 93% can be achieved for oil-water emulsions containing surfactants. Those skilled in the art can directly increase the area of the pathway structure or use a pathway structure with one unit processing area to perform multiple separation processes for oil-water emulsions to improve the separation efficiency according to application needs. When directly increasing the area of the pathway structure, the actual area of the pathway structure can be 1 to 4 times the unit processing area, such as 1.1 times, 1.2 times, 1.3 times, 1.4 times, 1.5 times, 1.7 times, 1.9 times, 2.1 times, 2.2 times, 2.5 times, 2.7 times, 2.9 times, 3.1 times, 3.2 times, 3.5 times, 3.7 times, 3.9 times, etc.
[0019] To achieve the second objective mentioned above, the present invention adopts the following technical solution:
[0020] This invention provides a method for preparing the above-mentioned pathway structure, comprising the following steps:
[0021] The first and second conical array plate models were constructed using 3D software. The model parameters were set, and then the raw materials were poured into the material tank. The models were printed using a 3D printer to obtain the first and second conical array plates. The surfaces of the first and second conical array plates were modified to be hydrophobic and interlocked. The side walls were then sealed, and inlet and outlet ports were reserved on the side walls.
[0022] To ensure print integrity, the material (i.e., Anycubic photosensitive resin) in the material tank must be added to the maximum mark before printing.
[0023] Furthermore, the parameters of the 3D printer are set to a light intensity of 50%-80% and a layer thickness of 10-50μm for slices.
[0024] Furthermore, the model parameters include cone height, distance between adjacent cones, and cone bottom diameter.
[0025] To achieve the third objective mentioned above, the present invention adopts the following technical solution:
[0026] This invention provides an application of the above-described pathway structure in oil-water separation.
[0027] Furthermore, the oil-water separation is the separation of an oil-water emulsion containing a surfactant. The surfactant includes anionic, cationic, or nonionic surfactants, such as sodium dodecyl sulfate, hexadecyltrimethylammonium bromide, sodium dodecylbenzenesulfonate, Tween 80, etc.
[0028] The beneficial effects of this invention are as follows:
[0029] The channel structure of the interlocking conical array plate of this invention exhibits excellent separation effects on oil-water emulsions such as hexane, gasoline, diesel, and silicone oil, and is particularly suitable for separating oil-water emulsions containing surfactants. A 648 cm⁻¹ plate is used. 2 The cone array plate achieves a separation efficiency exceeding 98% after separation. When separating oil-water emulsions containing surfactants, it offers advantages such as fast separation speed (up to 100 mL / min), high separation efficiency (≥93%), continuous separation capability, easy cleaning, reusability, good stability, large contact area with the oil-water emulsion, low cost, low energy consumption, no need for additional chemical reagents, and environmental friendliness. For continuous emulsion separation, the overall dimensions of the pathway structure can be designed and adjusted according to application needs, offering high adjustability. The pathway structure of this interlocking cone array plate is inexpensive to manufacture, uses readily available raw materials, and has a simple manufacturing process, making it suitable for large-scale preparation. Attached Figure Description
[0030] The specific embodiments of the present invention will be described in further detail below with reference to the accompanying drawings.
[0031] Figure 1 A schematic diagram of the pathway structure of the interlocking conical array plate of the present invention is shown;
[0032] Among them, 1 is a first conical array plate, 2 is a second conical array plate, 3 is a first conical array, 4 is a first substrate, 5 is a second conical array, 6 is a second substrate, 7 is a liquid inlet, and 8 is a liquid outlet.
[0033] Figure 2 The image shows a scanning electron microscope (SEM) image of the pathway structure of the interlocking conical array plate prepared in Example 1.
[0034] Figure 3 The image shows a scanning electron microscope (SEM) image of the surface texture of the cone array in the pathway structure of the interlocking cone array plate prepared in Example 1.
[0035] Figure 4 A physical image of the pathway structure of the interlocking conical array plate prepared in Example 1 is shown.
[0036] Figure 5 The diagram shows the connection of the pathway structure of the interlocking conical array plate in the oil-water separation experimental apparatus.
[0037] Figure 6 The diagram shows the experimental results of the separation of the pathway structure of the interlocking conical array plate prepared in Example 1.
[0038] Figure 7 The pathway structure of the interlocking conical array plate prepared in Example 1 is shown before the separation experiment and when using a 648cm² plate. 2 Comparison of fluorescence micrographs in aqueous phase after the separation experiment of interlocking cone array plates;
[0039] (a) shows the result before the separation experiment, and (b) shows the result after the separation experiment.
[0040] Figure 8 The diagram shows the separation effect data obtained in repeated experiments for the pathway structure of the interlocking conical array plate prepared in Example 1. Detailed Implementation
[0041] To more clearly illustrate the present invention, the following description, in conjunction with preferred embodiments and accompanying drawings, further clarifies the invention. Similar components in the drawings are indicated by the same reference numerals. Those skilled in the art should understand that the specific description below is illustrative rather than restrictive and should not be construed as limiting the scope of protection of the present invention.
[0042] Example 1
[0043] In the 3D software Cinema 4D, a first and a second conical array plate model were constructed. The first and second conical arrays were arranged in a honeycomb pattern, with a cone height of 4 mm, a cone base diameter of 1 mm, and a spacing of 1.4 mm between adjacent cones. The cone surface texture was at the micrometer level, and the overall dimensions of the pathway structure were 18 cm * 9 cm. The models were then printed using an Anycubic Mono X printer, employing Anycubic ordinary rigid photosensitive resin, transparent in color. The resin was poured into the feed trough to the maximum mark to ensure sufficient material. Printing parameters were set to 60% light intensity and 20 μm layer thickness. The printed first and second conical array plates were coated with Ultra-ever Dry 4001 paint for hydrophobic modification. After hydrophobic modification, they were matched and interlocked, and the sidewalls were sealed with adhesive, with inlets and outlets pre-reserved on the sidewalls. Multiple identical interlocking conical array plates can be fabricated and connected in series as needed to increase the total processing area.
[0044] Figure 1 This is a schematic diagram of the passage structure of the interlocking conical array plate of the present invention. The passage structure includes a first conical array plate, a second conical array plate, an inlet, and an outlet. The first conical array plate includes a first conical array and a first substrate, and the second conical array plate includes a second conical array and a second substrate.
[0045] Figure 2 The image shows a scanning electron microscope (SEM) image of the pathway structure of the plug-in cone array plate. The image reveals that the 3D-printed structure is relatively complete and has a regular overall structure.
[0046] Figure 3 The image shows a scanning electron microscope (SEM) image of the surface texture of the conical array in the pathway structure. The image reveals micron-level textures and protrusions on the surface, which are beneficial for increasing the capture and transport of oil droplets.
[0047] Figure 4 The image shows a physical picture of the flow path structure of the plug-in conical array plate, where the flow path is a curved loop.
[0048] Example 2
[0049] The experimental procedure was the same as in Example 1, except that the model parameters were adjusted. Specifically, the cone height was 6 mm, the bottom cone diameter was 1.5 mm, and the distance between adjacent cones was 2 mm. Other preparation conditions remained the same as in Example 1.
[0050] Experimental Example 1
[0051] The pathway structure of the interlocking conical array plate prepared in Example 1 is arranged according to... Figure 5 The following steps were taken to perform a connection and test the separation of oil-water emulsions containing surfactants:
[0052] The two ends of the passage structure of the interlocking conical array plate are connected with pins to facilitate the connection of rubber tubes (see...). Figure 4 Then, add 200 mL of sodium dodecyl sulfate aqueous solution (concentration 20 mg / 100 mL) to a 250 mL beaker, followed by 2–20 mL of low-viscosity silicone oil (PMX200-5CS), and mechanically stir to form an emulsion. Connect the inlet of the interlocking conical array plate's channel structure to a peristaltic pump. The emulsion in the beaker is pumped into the channel structure by the peristaltic pump. After flowing out of the channel, it is collected in another beaker, completing the separation. See the schematic diagram of the separation experiment connection. Figure 5 The separation rate was 100 mL / min, and the separation efficiency for each step is shown in Table 1.
[0053] Table 1. Summary of separation efficiency of emulsion flow through interlocking conical array plates
[0054]
[0055]
[0056] As shown in Table 1, after the oil-water emulsion was treated with the interlocking conical array plate prepared in Example 1, the 162cm... 2 The conical array plate exhibits significant oil-water separation performance, achieving a separation efficiency of 93.5%, indicating that this channel structure possesses excellent oil-water separation capabilities. Furthermore, the use of a 648cm² plate demonstrates this performance. 2 After the conical array plate was applied, the final separation efficiency reached 99.2%, with a residual oil content of 80.21 ppm. Meanwhile... Figure 6 The comparison diagrams before and after separation are shown, and it is not difficult to see that the pathway structure of the prepared interlocking conical array plate exhibits a good separation effect in separating oil-water emulsions containing surfactants.
[0057] Figure 7 The pathway structure of the intercalation cone array plate is shown before the separation experiment and when using a 648cm² plate. 2 Comparison of fluorescence microscopy images of the aqueous phase after the conical array plate. (a) shows that there are oil droplets of different sizes dispersed in the water, but after separation, no oil droplets can be detected in the water, indicating that the pathway structure has a good oil-water separation effect.
[0058] Experimental Example 2
[0059] This experiment investigated the separation effect of oil-water emulsions containing different surfactants. The test procedure was the same as in Experiment 1, using sodium dodecyl sulfate, hexadecyltrimethylammonium bromide, and Tween 80 for testing, with comparisons made using a 648cm³ surfactant. 2The separation efficiency and residual oil content of the conical array plate are shown in Table 2.
[0060] Table 2. Test data on the separation effect of oil-water emulsions containing different surfactants.
[0061] Types of surfactants Sodium dodecyl sulfate cetyltrimethylammonium bromide Twain 80 Separation efficiency 99.2% 98.9% 98.1% Residual oil content 80.21ppm 110.34ppm 189.94ppm
[0062] The data shows that the separation efficiency of emulsions containing different surfactants is over 98%, indicating that the pathway structure of the interlocking conical array plate has a good separation effect.
[0063] Experimental Example 3
[0064] This experimental example was used to investigate the effect of different oil types on the separation effect, comparing the separation effects of silicone oil, n-hexadecane, and isooctane. The test procedure was the same as in Experiment 1, with sodium dodecyl sulfate added as the surfactant, and a 648cm³ solution was used. 2 The results obtained after the conical array plate are shown in Table 3.
[0065] Table 3. Effects of different oil types on separation efficiency
[0066] Oil types silicone oil hexadecane Isooctane Separation efficiency 99.2% 98.5% 98.3% Residual oil content 80.21ppm 150.27ppm 169.74ppm
[0067] The pathway structure of the interlocking conical array plate showed high separation performance for silicone oil, n-hexadecane, and isooctane, with a separation efficiency of over 98%, which meets the application requirements.
[0068] Test Example 4
[0069] The pathway structure of the interlocking conical array plate prepared in Example 1 was subjected to 12 cycles of repeated testing to examine the durability of oil-water separation. The specific steps are as follows:
[0070] The pathway structure of the interlocking conical array plate in Example 1 is arranged according to... Figure 5 The connection method shown is used to fix the device, and a 648cm cable is used. 2 A conical array plate (i.e., four 18cm*9cm channel structures connected in series) was used to continuously separate oil-water emulsions containing sodium dodecyl sulfate. Experimental parameters were as described in Example 1. The experiment was repeated 12 times, and the separation efficiency data for the 1st, 3rd, 6th, 9th, and 12th iterations were recorded. The results are shown in […]. Figure 8 .have Figure 8 It is known that the pathway structure of the interlocking conical array plate provided by the present invention can maintain a high separation efficiency in 12 repeated experiments, with the separation efficiency fluctuating around 99%, indicating that the pathway structure of the interlocking conical array plate can be reused more than 12 times.
[0071] Obviously, the above embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the implementation of the present invention. For those skilled in the art, other variations or modifications can be made based on the above description. It is impossible to exhaustively list all the implementation methods here. All obvious variations or modifications derived from the technical solutions of the present invention are still within the protection scope of the present invention.
Claims
1. A pathway structure for an interlocking conical array plate, characterized in that, It includes a first conical array plate and a second conical array plate arranged in an interlocking configuration, a passage structure formed by the interlocking of the first and second conical array plates, and an inlet and an outlet provided on the outer wall of the passage structure; wherein, The first conical array plate includes a first substrate and a first conical array arranged in a honeycomb pattern thereon; the second conical array plate includes a second substrate and a second conical array arranged in a honeycomb pattern thereon; the cone height, the spacing between adjacent cones, and the diameter of the cone bottom are on the millimeter scale, and the cone surface texture is on the micrometer scale. The pathway structure is U-shaped, and its inner surface is hydrophobic; The cone height of the first and second cone arrays is 1-8 mm, the distance between adjacent cones is 1-4 mm, and the diameter of the cone bottom is 0.5-2 mm. The area of the pathway structure is 162-648 cm². 2 .
2. The pathway structure according to claim 1, characterized in that, The oil phase in an oil-water emulsion includes one or more of the following: n-hexane, n-hexadecane, isooctane, gasoline, diesel, and silicone oil.
3. The pathway structure according to claim 1, characterized in that, The first and second conical array plates are made of Anycubic photosensitive resin.
4. The pathway structure according to any one of claims 1 to 3, characterized in that, When the area of the pathway structure is 162-324 cm² 2 At that time, the separation efficiency of oil-water emulsion was 93%-95%.
5. The pathway structure according to any one of claims 1 to 3, characterized in that, When the area of the pathway structure is 324-486 cm² 2 At that time, the separation efficiency of oil-water emulsion was 95-98%.
6. The pathway structure according to any one of claims 1 to 3, characterized in that, The area of the pathway structure is 486-648 cm² 2 At that time, the separation efficiency of oil-water emulsion was 98%-99%.
7. A method for preparing a pathway structure as described in any one of claims 1 to 6, characterized in that, Includes the following steps: The first and second conical array plate models were constructed using 3D software. The model parameters were set, and then the raw materials were poured into the material tank. The models were printed using a 3D printer to obtain the first and second conical array plates. The surfaces of the first and second conical array plates were modified to be hydrophobic and interlocked. The side walls were then sealed, and inlet and outlet ports were reserved on the side walls.
8. The preparation method according to claim 7, characterized in that, The parameters of the 3D printer are set to light intensity of 50%-80% and layer thickness of 10-50μm slices.
9. The preparation method according to claim 7, characterized in that, The model parameters include cone height, distance between adjacent cones, and diameter of the cone base.
10. The application of a pathway structure as described in any one of claims 1 to 6 in oil-water separation.
11. The application according to claim 10, characterized in that, The oil-water separation refers to the separation of oil-water emulsions containing surfactants.
Citation Information
Patent Citations
Oil-water separation pipe with hydrophobic and oleophylic surface and preparation method and application thereof
CN112221201A