Conductive filter material and method of making and use thereof

CN118001839BActive Publication Date: 2026-10-09ZHEJIANG NORMAL UNIV
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Patent Information

Application Number
CN202311364509.X
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-10-18
Publication Date
2026-10-09
Estimated Expiration
2043-10-18

AI Technical Summary

Technical Problem

我们可以将此类改性措施总结为“被动抗污”,油滴仅仅是被隔绝在水化层外,一旦超亲水表面受到损害,随时存在着油滴突破水化层的潜在风险

Benefits of technology

[0028] 1. This invention grows TiSe2 nanoparticles with superhydrophilicity on the surface of titanium foam for the first time through a one-step hydrothermal method. The resulting conductive filter material TiSe2/TF has both superhydrophilicity and underwater superoleophobicity, and can be used as both a filter material and a cathode electrode.

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Abstract

The application provides a conductive filter material and a preparation method and application thereof, the conductive filter material is obtained by modifying metal foam titanium through a one-step hydrothermal method to grow TiSe2 nanoparticles in situ on the surface of the metal foam titanium, the conductive filter material has superhydrophilicity and underwater superoleophobicity, and can be used as a filter material and a cathode electrode simultaneously, when filtering oil-containing wastewater, the conductive filter material can realize active antifouling performance through a double mechanism of in-situ aeration and dielectrophoresis force in combination with an external electric field, and has super-strong antifouling property and durability while having a separation efficiency of 99% or above.
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Description

Technical Field

[0001] This invention relates to the field of surface modification technology for metal foam materials, specifically to a conductive filter material, its preparation method, and its application. Background Technology

[0002] Oily wastewater originates widely from various industrial sectors, including natural gas, food processing, petroleum extraction, and petrochemicals, posing a significant threat to the natural environment and human health. In particular, the frequent occurrence of offshore oil spills has raised public concern about separating clean water resources from oily wastewater. Commonly used methods for treating oily wastewater include gravity sedimentation, flotation, thermal treatment, coagulation, flocculation, and skimming; however, these methods often suffer from low efficiency, high energy consumption, or secondary pollution. Membrane separation technology, with its advantages of high efficiency and low energy consumption, is a promising technology for treating oily wastewater. However, membrane fouling restricts its application in oil-water separation; the sharp decline in water flux and lifespan is a problem that urgently needs to be addressed. Therefore, developing antifouling membrane materials is crucial for treating oily wastewater.

[0003] In recent years, inspired by superwetting biological surfaces, many researchers have constructed micro- and nanostructures on membrane surfaces to create hydration layers that resist oil adhesion. Some representative research results have demonstrated excellent separation performance due to their superhydrophilicity and underwater superoleophobicity. However, a decline in separation performance is unavoidable under extreme filtration environments or high-intensity continuous filtration. This is because, under such operating conditions, the constructed superhydrophilic surface undergoes oxidation or deterioration, resulting in insufficient hydrophilic polymer coverage. Oil droplets can then break through the defects in the hydration layer and adhere to the membrane surface under transmembrane pressure, forming a filter cake. This leads to a rapid decrease in water flux and separation performance. We can summarize this type of modification as "passive antifouling," where oil droplets are merely isolated outside the hydration layer. Once the superhydrophilic surface is damaged, there is always a potential risk of oil droplets breaking through the hydration layer.

[0004] Therefore, it is urgent to find a filter material that is both "actively anti-fouling" and has a long service life. Summary of the Invention

[0005] To overcome the shortcomings of the prior art, the main objective of this invention is to provide a conductive filter material, its preparation method, and its application. This conductive filter material is obtained by modifying titanium foam in a one-step hydrothermal method to grow TiSe2 nanoparticles in situ on its surface. The conductive filter material has both superhydrophilicity and underwater superoleophobicity, and can be used as both a filter material and a cathode electrode. When filtering oily wastewater, it can achieve active antifouling performance through a dual mechanism of in-situ aeration and dielectric electrophoresis in combination with an external electric field. It has a separation efficiency of over 99% while exhibiting superior antifouling and durability.

[0006] To achieve the above objectives, according to a first aspect of the present invention, a conductive filter material is provided.

[0007] The conductive filter material comprises titanium foam and TiSe2 nanoparticles grown in situ on at least a portion of the surface of the titanium foam.

[0008] Furthermore, the TiSe2 nanoparticles are spherical and protruding.

[0009] Furthermore, the pore size of the foamed titanium is less than or equal to 5 μm and greater than 0.

[0010] To achieve the above objectives, according to a second aspect of the present invention, a method for preparing a conductive filter material is provided.

[0011] The preparation method of this conductive filter material includes the following steps:

[0012] Pretreatment of foamed titanium;

[0013] The pretreated foamed titanium is subjected to a hydrothermal reaction with a reaction solution to obtain the conductive filter material; wherein the reaction solution contains selenium.

[0014] Furthermore, the pretreatment process includes: firstly, ultrasonically cleaning the foamed titanium with acetone and hydrochloric acid solutions in sequence, then rinsing with deionized water, and finally performing a first drying treatment.

[0015] Furthermore, the foamed titanium is ultrasonically cleaned in the acetone and hydrochloric acid solutions for 10-15 minutes each;

[0016] Preferably, the temperature of the first drying treatment is 60-65°C.

[0017] Furthermore, the reaction solution is a dispersion solution of selenium powder;

[0018] Preferably, the reaction solution contains ethylenediamine;

[0019] Preferably, the mass percentages of the selenium powder and the ethylenediamine in the reaction solution are 1-3% and 45-50%, respectively.

[0020] Furthermore, the temperature of the hydrothermal reaction is 180–200°C, preferably 180°C; the reaction time is 4–6 hours, preferably 5 hours.

[0021] Furthermore, it also includes: washing and second drying the obtained conductive filter material;

[0022] Preferably, the washing process involves repeated rinsing with deionized water;

[0023] Preferably, the temperature of the second drying treatment is 60-65°C.

[0024] To achieve the above objectives, according to a third aspect of the present invention, an application of a conductive filter material is provided.

[0025] The application of the conductive filter material provided in the first aspect of the present invention or the conductive filter material prepared by the method provided in the second aspect of the present invention in the treatment of oily wastewater;

[0026] Preferably, the oily wastewater is an oil-in-water emulsion and / or an oil-water mixture.

[0027] Advantages of this invention:

[0028] 1. This invention grows TiSe2 nanoparticles with superhydrophilicity on the surface of titanium foam for the first time through a one-step hydrothermal method. The resulting conductive filter material TiSe2 / TF has both superhydrophilicity and underwater superoleophobicity, and can be used as both a filter material and a cathode electrode.

[0029] 2. The microbubbles generated by in-situ aeration using the hydrogen evolution reaction (HER) can spontaneously combine with oil stains, increasing their buoyancy. At the same time, by utilizing the reduction in the interfacial energy and potential energy of the bubbles, the kinetic energy of the oil contaminants is increased through their spontaneous aggregation. Subsequently, under the electric field generated by the conductive filter material TiSe2 / TF, the emulsion droplets are subjected to dielectric force and spontaneously leave the surface of the filter material, achieving the effect of "active anti-fouling".

[0030] Calculations and tests show that under this anti-fouling mechanism, the conductive filter material TiSe2 / TF reduces membrane fouling by more than 90%, achieving almost zero membrane fouling. Furthermore, the separation efficiency consistently exceeds 99% in 100 manual cycle tests.

[0031] 3. The preparation method provided by the present invention has the advantages of simple process, low equipment requirements, low cost, and easy large-scale industrial application. Attached Figure Description

[0032] Various other advantages and benefits will become apparent to those skilled in the art upon reading the following detailed description of preferred embodiments. The accompanying drawings are for illustrative purposes only and are not intended to limit the invention. In the drawings:

[0033] Figure 1 A schematic diagram of the experimental method for preparing the conductive filter material TiSe2 / TF in the embodiments provided by the present invention;

[0034] Figure 2 Scanning electron microscope (SEM) images and nanoparticle morphology images of the conductive filter material TiSe2 / TF prepared in the embodiments provided by the present invention; wherein, Figure 2 a- Figure 2 c shows scanning electron microscope (SEM) images of the conductive filter material TiSe2 / TF at different magnifications; Figure 2 d represents the morphology of the nanoparticles from a cross-sectional perspective;

[0035] Figure 3 The retention rate and flux of the conductive filter material TiSe2 / TF prepared in the embodiments of the present invention for separating gasoline oil-in-water emulsion are shown in the diagram; wherein, Figure 3 (a) Retention rate and flux diagram for separating gasoline-in-water emulsions without an applied electric field; Figure 3 (b) Retention rate and flux diagram for separating gasoline-in-water emulsions under an external electric field;

[0036] Figure 4 The retention rate and flux of the conductive filter material TiSe2 / TF prepared in the embodiments of the present invention for separating n-hexane oil-in-water emulsion are shown in the figure; wherein, Figure 4 (a) Rejection and flux diagram for separating n-hexane oil-in-water emulsions without an applied electric field; Figure 4 (b) Rejection rate and flux diagram for separating n-hexane oil-in-water emulsion under an external electric field;

[0037] Figure 5 The retention rate and flux of the conductive filter material TiSe2 / TF prepared in the embodiments of the present invention for separating oil-in-water emulsions of edible oil are shown in the figure; wherein, Figure 5 (a) Retention rate and flux of oil-in-water emulsions separated without an applied electric field; Figure 5 (b) Retention rate and flux diagram for separating oil-in-water emulsions of edible oil under an external electric field;

[0038] Figure 6 The retention rate and flux of the conductive filter material TiSe2 / TF prepared in the embodiments of the present invention for separating oil-in-water emulsions of petroleum ether are shown in the figure; wherein, Figure 6 (a) Retention rate and flux of oil-in-water emulsions of petroleum ether separated without an applied electric field; Figure 6 (b) Rejection rate and flux diagram for separating oil-in-water emulsions of petroleum ether under an external electric field;

[0039] Figure 7 Microscopic images, particle size distribution images, and optical photographs of the conductive filter material TiSe2 / TF prepared in the embodiments of the present invention before and after separation of the emulsion and filtrate;

[0040] Figure 8 A schematic diagram illustrating the potential mechanism by which the conductive filter material TiSe2 / TF prepared in the embodiments of the present invention improves separation efficiency under an electric field;

[0041] Figure 9 (a) is an LSV curve of the conductive filter material TiSe2 / TF prepared in the embodiments provided by the present invention;

[0042] Figure 9 (b) Tafel curves of the conductive filter material TiSe2 / TF and the original foamed titanium prepared in the embodiments provided by the present invention;

[0043] Figure 9 (c) The overpotentials of the conductive filter material TiSe2 / TF and the original foamed titanium prepared in the embodiments provided by the present invention at currents of 100mA and 500mA, respectively;

[0044] Figure 9 (d) is a real-world image showing the aeration rate of the conductive filter material TiSe2 / TF and the original foamed titanium prepared in the embodiments provided by the present invention;

[0045] Figure 10 (a) A performance comparison diagram of the conductive filter material TiSe2 / TF prepared in the embodiments provided by the present invention;

[0046] Figure 10 (b) is a flux recovery diagram of the conductive filter material TiSe2 / TF prepared in the embodiments provided by the present invention;

[0047] Figure 11 The conductive filter material TiSe2 / TF prepared in the embodiments provided by the present invention has a filtration cycle performance diagram of 100 cycles.

[0048] Figure 12 The filtration performance of the conductive filter material TiSe2 / TF prepared in the embodiments provided by the present invention under extreme conditions is shown in the figure.

[0049] Figure 13 The antifouling performance diagram of the conductive filter material TiSe2 / TF prepared in the embodiments provided by the present invention;

[0050] Figure 14 A diagram illustrating the potential antifouling mechanism (in-situ aeration and dielectric force) of the conductive filter material TiSe2 / TF prepared in the embodiments provided by the present invention. Detailed Implementation

[0051] Exemplary embodiments of the present disclosure will now be described in more detail with reference to the accompanying drawings. While exemplary embodiments of the present disclosure are shown in the drawings, it should be understood that the present disclosure may be implemented in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the disclosure to those skilled in the art.

[0052] Given that the dielectric force in an electric field environment can act on particles to achieve active particle displacement, this lays the theoretical foundation for developing an antifouling material that is dominated by both in-situ aeration and dielectric force in an electric field environment.

[0053] In this invention, the antifouling method that uses the driving force generated by the filter material to actively move oil droplets away from the membrane surface is called "active antifouling".

[0054] Currently, traditional membranes have a limited lifespan under the influence of an electric field, making it impossible to achieve both "active antifouling" and long service life.

[0055] In order to obtain a conductive filter material with active anti-fouling capability, a first aspect of the present invention provides a conductive filter material.

[0056] The conductive filter material of the present invention includes titanium foam and TiSe2 nanoparticles grown in situ on at least a portion of the surface of a titanium foam substrate.

[0057] Among them, TiSe2 nanoparticles are spherical and protruding.

[0058] In the embodiments of the present invention, the average particle size of TiSe2 nanoparticles is 300 nm to 1 μm.

[0059] In an embodiment of the present invention, TiSe2 nanoparticles are arranged discontinuously on the surface of a foamed titanium substrate.

[0060] In the embodiments of the present invention, the pore size of the foamed titanium is ≤5μm and the pore size is controllable, and it has excellent electrical conductivity.

[0061] In this invention, foamed titanium is used as the substrate material, which can extend the service life of the membrane while maintaining high separation efficiency.

[0062] It should be noted that the pore size of the foamed titanium is greater than 0 to achieve better filtration.

[0063] This invention achieves the first growth of superhydrophilic TiSe2 nanoparticles on the surface of titanium foam using a one-step hydrothermal method. The resulting conductive filter material TiSe2 / TF exhibits both superhydrophilicity and underwater superoleophobicity, and can be used simultaneously as a filter material and a cathode electrode.

[0064] Microbubbles generated by in-situ aeration via the hydrogen evolution reaction (HER) spontaneously bind to oil deposits, increasing their buoyancy. Simultaneously, the reduction in interfacial and potential energy of these bubbles leads to spontaneous coalescence, increasing the kinetic energy of the oil contaminants. Subsequently, under the electric field generated by the conductive filter material TiSe2 / TF, the emulsion droplets are subjected to dielectric electrophoretic forces, spontaneously detaching from the filter material's surface, achieving an "active antifouling" effect. Calculations and tests show that this antifouling mechanism reduces membrane fouling by over 90% with the conductive filter material TiSe2 / TF. Furthermore, the separation efficiency consistently exceeds 99% in 100 manual cycle tests.

[0065] Therefore, the conductive filter material with active anti-fouling capability provided in this invention has important application value and academic significance.

[0066] A second aspect of the present invention provides a method for preparing the conductive filter material described in the first aspect of the present invention.

[0067] like Figure 1 As shown, the preparation of the conductive filter material in this invention is carried out according to the following steps.

[0068] (1) Pre-treat the foamed titanium to obtain clean foamed titanium.

[0069] The pretreatment process includes: first, ultrasonic cleaning of the foamed titanium with acetone and hydrochloric acid solutions in sequence to remove lipophilic impurities and oxide layers from the surface of the foamed titanium; then, repeated rinsing with deionized water to remove excess cleaning solution; and finally, a first drying process to obtain clean foamed titanium.

[0070] In an embodiment of the present invention, the foamed titanium is ultrasonically cleaned in acetone for 10 to 15 minutes to remove fat-soluble impurities from the surface of the foamed titanium.

[0071] For example, the ultrasonic cleaning time of foamed titanium in acetone is 10 min, 11 min, 12 min, 13 min, 14 min, and 15 min, but it is not limited to the listed values. Other unlisted values ​​within this range are also applicable.

[0072] In an embodiment of the present invention, the foamed titanium is ultrasonically cleaned in hydrochloric acid solution for 10 to 15 minutes to remove the oxide layer on the surface of the foamed titanium.

[0073] For example, the ultrasonic cleaning time of foamed titanium in hydrochloric acid solution is 10 min, 11 min, 12 min, 13 min, 14 min, and 15 min, but it is not limited to the listed values. Other unlisted values ​​within this range are also applicable.

[0074] In one embodiment of the present invention, the concentration of the hydrochloric acid solution is 3 mol / L.

[0075] Of course, you can also choose a hydrochloric acid solution of appropriate concentration according to actual needs for effective cleaning.

[0076] It should be noted that, in order to ensure efficient cleaning, the foamed titanium after ultrasonic cleaning with acetone is rinsed with deionized water before ultrasonic cleaning with hydrochloric acid solution to remove residual acetone from the surface of the foamed titanium.

[0077] In an embodiment of the present invention, the foamed titanium, after being ultrasonically cleaned with acetone and hydrochloric acid, is repeatedly washed with deionized water to remove residual cleaning solution, and then placed in an oven for drying.

[0078] It should be noted that deionized water can be used for ultrasonic cleaning to achieve better cleaning results.

[0079] In an embodiment of the present invention, the temperature of the first drying process is 60-65°C, for example, drying can be carried out in an oven at 60°C.

[0080] (2) The pretreated clean foam titanium and the reaction solution are transferred to a stainless steel reactor for hydrothermal reaction to obtain a conductive filter material; wherein the reaction solution contains selenium.

[0081] In an embodiment of the present invention, the reaction solution is a dispersion solution of selenium powder.

[0082] In some embodiments of the present invention, the reaction solution contains ethylenediamine, for example, an aqueous solution of ethylenediamine.

[0083] In this process, selenium powder is dispersed in an ethylenediamine solution.

[0084] In the embodiments of the present invention, the mass percentages of selenium powder and ethylenediamine in the reaction solution are (1-3%) and (45-50%), respectively.

[0085] In some embodiments of the present invention, the mass percentages of selenium powder, ethylenediamine, and deionized water in the reaction solution are (1-3%), (45-50%), and (45-55%), respectively.

[0086] In some embodiments of the present invention, the mass percentages of selenium powder, ethylenediamine, and deionized water in the reaction solution are 1.5%, 48%, and 50.5%, respectively.

[0087] In some embodiments of the present invention, the amounts of each substance added to the reaction solution are as follows:

[0088] The solution contains 4–5 mL of ethylenediamine (C2H8N2), 0.1 g of selenium powder, and 6–8 mL of deionized water.

[0089] In one specific embodiment of the present invention, the amounts of each substance added to the reaction solution are as follows:

[0090] 0.1 g of selenium powder, 4 mL of ethylenediamine, and 6 mL of deionized water.

[0091] In embodiments of the present invention, the temperature of the hydrothermal reaction is 180–200°C, for example, 180°C; and the reaction time is 4–6 hours, for example, 5 hours.

[0092] In some embodiments of the present invention, the hydrothermal reaction temperature is 180°C and the reaction time is 5 hours.

[0093] (3) The obtained conductive filter material is washed and then dried.

[0094] The prepared conductive filter material needs to be repeatedly rinsed and washed with deionized water to remove excess hydrothermal reaction solution; then the washed conductive filter material undergoes a second drying process.

[0095] In an embodiment of the present invention, the temperature of the second drying process is 60-65°C, for example, drying can be carried out in an oven at a temperature of 60°C.

[0096] It is worth mentioning that the first and second drying processes in this invention can be carried out under a protective atmosphere, such as nitrogen, to prevent oxidation.

[0097] A third aspect of the present invention provides an application of a conductive filter material in the treatment of oily wastewater.

[0098] The conductive filter material is either the conductive filter material provided in the first aspect of the present invention, or the conductive filter material prepared by the method provided in the second aspect of the present invention.

[0099] In embodiments of the present invention, the oily wastewater is an oil-in-water emulsion and / or an oil-water mixture.

[0100] The conductive filter material, its preparation method, and its application in this invention will be described in detail below through specific embodiments.

[0101] Example 1:

[0102] Adopting such Figure 1 The preparation method process is shown.

[0103] First, the cut titanium foam sheets (27mm × 27mm × 1mm, pore size greater than 0 and less than or equal to 5μm) were immersed in 50mL of 3mol / L hydrochloric acid solution and ultrasonically cleaned for 15 minutes to remove the oxide layer on the surface of the titanium foam. Next, the cleaned titanium foam was rinsed with deionized water to remove any residual hydrochloric acid solution. Then, it was immersed in 30mL of acetone solution and ultrasonically cleaned for 15 minutes to remove soluble lipid impurities on the surface of the titanium foam. After cleaning, the titanium foam was repeatedly rinsed, soaked, and ultrasonicated with deionized water to ensure no residual hydrochloric acid and acetone remained. Finally, the cleaned titanium foam was dried in an oven at 60℃ for later use.

[0104] Next, weigh 0.1g of selenium powder and add 6mL of deionized water and 4mL of ethylenediamine. Sonicate the mixture until homogeneous, ensuring the selenium powder is evenly dispersed.

[0105] Third, the mixed solution was transferred together with the prepared clean titanium foam to a reactor and reacted in an oven at 180°C for 5 hours to obtain a conductive filter material TiSe2 / TF with TiSe2 nanoparticles grown in situ on the surface of the titanium foam. The obtained conductive filter material TiSe2 / TF was then rinsed to remove excess reaction solution.

[0106] In this invention, the conductive filter material TiSe2 / TF prepared in Example 1 was subjected to SEM testing to observe the morphological changes after TiSe2 nanoparticles were grown on the surface of the titanium foam. The results are as follows: Figure 2 As shown.

[0107] from Figure 2 (a)- Figure 2 As can be seen in (c), the modified titanium foam surface is uniformly distributed with TiSe2 nanospheres and TiSe2 nanoprotrusions at different magnifications, proving that TiSe2 nanoparticles have been successfully grown on the surface of titanium foam.

[0108] also, Figure 2 (d) The cross-sectional view proves that the nanoparticles are complete spheres.

[0109] In this invention, the filtration performance of the conductive filter material TiSe2 / TF prepared in Example 1 was tested. The test emulsions included four different oil-in-water emulsions, and the test conditions included filtration under both electric field and no electric field conditions. The results are as follows: Figures 3-6 As shown.

[0110] The results show that, without applying a DC electric field, the retention rate of the conductive filter material TiSe2 / TF can reach about 95% for oil-in-water emulsions composed of four different oils. At the same time, it can be clearly observed that the flux decreases from 2094 LMH in pure water to about 600 LMH.

[0111] After applying a DC electric field to the filtration system, it was found that the retention rate of all oils by the conductive filter material TiSe2 / TF increased to over 99%.

[0112] Subsequently, the liquids before and after filtration were further examined using a microscope, confirming that almost no small oil droplets were found within the microscope lens after filtration under a DC electric field. Particle size analysis also supported this result (e.g., Figure 7 (As shown).

[0113] It should be noted that the potential performance improvement mechanism has already been included. Figure 8 Inside.

[0114] In this invention, the electrochemical properties of foamed titanium before and after modification were tested, and the results are as follows: Figure 9 As shown.

[0115] Hydrogen evolution reaction (HER) tests were performed using a three-electrode system on an electrochemical workstation.

[0116] like Figure 9 (a)- Figure 9 As shown in (b), by comparing the linear sweep voltammetry (LSV) curve and the Tafel plot, it can be found that the modified conductive filter material TiSe2 / TF has better electrochemical performance than the original foamed titanium.

[0117] The conductive filter material TiSe2 / TF exhibits significantly better hydrogen evolution performance under high current than the original material (e.g., Figure 9 (c)- Figure 9 (d) As shown, it is hoped that filtration separation will be the main method in the entire experimental process, and HER will only be used as an auxiliary means of separation. Therefore, the appropriate amount of hydrogen evolution can avoid the large amount of water loss caused by water electrolysis.

[0118] The durability of filter materials is one of the criteria for industrial-scale promotion.

[0119] In this invention, the durability and tolerance to extreme environments of the conductive filter material TiSe2 / TF were tested.

[0120] like Figure 11 As shown, the separation performance of the conductive filter material TiSe2 / TF did not decrease during 100 cycles of testing.

[0121] like Figure 12 As shown, the filtration performance of the conductive filter material TiSe2 / TF was not affected in strong acid and strong alkali environments.

[0122] At the same time, such as Figure 10As shown in (a), the conductive filter material TiSe2 / TF, prepared 4 months after completion, still achieves a separation efficiency of over 99%, demonstrating the superiority of the preparation method in this invention. Meanwhile... Figure 10 (b) shows that the flux recovery of the conductive filter material TiSe2 / TF is above 90% during 180 minutes of uninterrupted filtration.

[0123] In this invention, the antifouling performance of the conductive filter material TiSe2 / TF under an active antifouling mechanism was tested, and the results are as follows: Figure 13 As shown.

[0124] After filtration under both electric field and non-electric field conditions, the conductive filter material TiSe2 / TF was ultrasonically cleaned with anhydrous ethanol to fully dissolve residual oil droplets in the membrane pores. The image clearly shows that the cleaning solution was colorless and transparent after filtration under the electric field condition, while the cleaning solution after ordinary filtration turned completely red. Measurement of the oil content using a UV spectrophotometer revealed that applying an electric field reduced membrane pore fouling by more than 90%.

[0125] like Figure 14 As shown, under the dual mechanism of dielectric electrophoresis and in-situ aeration, oil droplets spontaneously leave the filter surface, achieving an active anti-fouling effect.

[0126] This invention modifies titanium foam, enabling the modified foam to achieve active antifouling performance when filtering oily wastewater through a dual mechanism of in-situ aeration and dielectric electrophoresis in conjunction with an external electric field. This results in a separation efficiency of over 99% while exhibiting superior antifouling and durability.

[0127] The preparation method of this invention is simple to operate, low in cost, and easy to implement for industrial application, and is of great significance in the application of oily wastewater.

[0128] It should be noted that the term "comprising" and any variations thereof in the specification and claims of this invention are intended to cover non-exclusive inclusion, for example, including a series of components that are not necessarily limited to those explicitly listed, but may include other components that are not explicitly listed or that are inherent to the component.

[0129] In this invention, the terms "upper," "lower," "bottom," "top," "left," "right," "inner," and "outer," etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. These terms are primarily for the purpose of better describing the invention and its embodiments, and are not intended to limit the indicated device, element, or component to having a specific orientation, or to be constructed and operated in a specific orientation.

[0130] Furthermore, in addition to indicating location or positional relationship, some of the aforementioned terms may also have other meanings. For example, the term "above" may also be used in certain situations to indicate a dependency or connection relationship. Those skilled in the art can understand the specific meaning of these terms in this invention based on the specific circumstances.

[0131] Furthermore, the descriptions of "first," "second," etc., involved in this invention are for descriptive purposes only and should not be construed as indicating or implying their relative importance or implicitly specifying the number of technical features indicated. Therefore, a feature defined with "first" or "second" may explicitly or implicitly include at least one of those features.

[0132] Furthermore, the technical solutions of the various embodiments can be combined with each other, but only if they are feasible for those skilled in the art. If the combination of technical solutions is contradictory or cannot be implemented, it should be considered that such combination of technical solutions does not exist and is not within the scope of protection claimed by this invention.

[0133] The above description is merely a preferred embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any variations or substitutions that can be easily conceived by those skilled in the art within the technical scope disclosed in the present invention should be included within the scope of protection of the present invention. Therefore, the scope of protection of the present invention should be determined by the scope of the claims.

Claims

1. A conductive filter material, characterized in that, The conductive filter material includes titanium foam and TiSe2 nanoparticles grown in situ on at least a portion of the surface of the titanium foam. The TiSe2 nanoparticles are protruding and have an average particle size of 300 nm to 1 μm. The TiSe2 nanoparticles are discontinuously arranged on the surface of the titanium foam. The pore size of the titanium foam is less than or equal to 5 μm and greater than 0.

2. The conductive filter material as described in claim 1, characterized in that, The TiSe2 nanoparticles are spherical.

3. A method for preparing the conductive filter material according to claim 1 or 2, characterized in that, Includes the following steps: Pretreatment of foamed titanium; The pretreated foamed titanium is subjected to a hydrothermal reaction with a reaction solution to obtain the conductive filter material; wherein the reaction solution contains selenium.

4. The method for preparing the conductive filter material as described in claim 3, characterized in that, The pretreatment process includes: firstly, ultrasonically cleaning the foamed titanium with acetone and hydrochloric acid solutions in sequence, then rinsing with deionized water, and finally performing a first drying process.

5. The method for preparing the conductive filter material as described in claim 4, characterized in that, The foamed titanium was ultrasonically cleaned in acetone and hydrochloric acid solutions for 10-15 minutes each.

6. The method for preparing the conductive filter material as described in claim 4, characterized in that, The temperature of the first drying process is 60~65℃.

7. The method for preparing the conductive filter material as described in claim 3, characterized in that, The reaction solution is a dispersion of selenium powder.

8. The method for preparing the conductive filter material as described in claim 7, characterized in that, The reaction solution contains ethylenediamine.

9. The method for preparing the conductive filter material as described in claim 8, characterized in that, The mass percentages of the selenium powder and the ethylenediamine in the reaction solution are (1~3%) and (45~50%), respectively.

10. The method for preparing the conductive filter material according to claim 3, characterized in that, The hydrothermal reaction is carried out at a temperature of 180-200℃ for 4-6 hours.

11. The method for preparing the conductive filter material according to claim 10, characterized in that, The hydrothermal reaction was carried out at a temperature of 180°C for 5 hours.

12. The method for preparing the conductive filter material as described in claim 3, characterized in that, Also includes: The obtained conductive filter material is then washed and subjected to a second drying process.

13. The method for preparing the conductive filter material according to claim 12, characterized in that, The washing process involves repeated rinsing with deionized water.

14. The method for preparing the conductive filter material according to claim 12, characterized in that, The temperature for the second drying process is 60~65℃.

15. The application of a conductive filter material according to claim 1 or 2, or a conductive filter material prepared by the method according to any one of claims 3-14, in the treatment of oily wastewater.

16. The application as described in claim 15, characterized in that, The oily wastewater is an oil-in-water emulsion.

Citation Information

Patent Citations

  • Oil-water separation device

    CN114524492A