CN113663527A - Preparation method of super-amphiphilic stainless steel net capable of adapting to wettability and used for emulsion on-demand separation - Google Patents
Preparation method of super-amphiphilic stainless steel net capable of adapting to wettability and used for emulsion on-demand separation Download PDFInfo
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- CN113663527A CN113663527A CN202110921829.5A CN202110921829A CN113663527A CN 113663527 A CN113663527 A CN 113663527A CN 202110921829 A CN202110921829 A CN 202110921829A CN 113663527 A CN113663527 A CN 113663527A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0039—Inorganic membrane manufacture
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/38—Liquid-membrane separation
- B01D61/40—Liquid-membrane separation using emulsion-type membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0039—Inorganic membrane manufacture
- B01D67/0044—Inorganic membrane manufacture by chemical reaction
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
Abstract
The invention discloses a preparation method of a super-amphiphilic stainless steel mesh which is used for emulsion separation as required and can adapt to wettability, and belongs to the technical field of preparation of emulsion separation membranes. The super-amphiphilic stainless steel mesh which can adapt to wettability is prepared by an all-water system construction strategy through an electrochemical method, and the oil-water emulsion is separated according to requirements. Compared with an intelligent response separation membrane and a Janus membrane, the method has the advantages of simple process, large-scale production, no secondary pollution, low production and manufacturing cost and the like. Greatly promoting the practical application of the emulsion separation membrane.
Description
Technical Field
The invention belongs to the technical field of preparation of emulsion separation membranes, and particularly relates to a preparation method of a super-amphiphilic stainless steel mesh which is used for separating emulsion as required and can adapt to wettability.
Background
Membrane separation technology is one of the main methods for treating oily wastewater. Oily wastewater generated in the industrial production process has the characteristics of diversity, complexity and the like, so that a separation membrane with single separation performance cannot meet the actual requirement. The existing on-demand separation membranes such as intelligent response separation membranes and Janus membranes have the defects of expensive materials, complex preparation process, easy secondary pollution and the like.
The super-amphiphilic stainless steel net is prepared by an electrochemical method. The construction strategy of the full water system is simple, the process is simple, the use of organic solvent is not involved, and the method is green, energy-saving and environment-friendly. The super-amphiphilic stainless steel mesh can be adapted to wettability so that emulsion can be separated as required, and meanwhile, the separation membrane has excellent antifouling performance and has huge practical application value in the aspect of oily sewage treatment.
Disclosure of Invention
The invention aims to provide a preparation method of a green, energy-saving and environment-friendly separation membrane. The emulsion can be separated according to the requirement by utilizing the adaptable wettability of the super-amphiphilic stainless steel mesh.
The technical scheme for realizing the purpose of the invention is as follows: the preparation method of the super-amphiphilic stainless steel net which is used for separating the emulsion according to the requirement and can adapt to the wettability is characterized by comprising the following steps:
A. cutting a stainless steel net: cutting the stainless steel net into a certain size by using scissors;
B. cleaning a stainless steel net: placing the cut stainless steel mesh in n-hexane for ultrasonic treatment for 1h, and removing impurities on the surface of the stainless steel mesh; washing two surfaces of the stainless steel mesh with ethanol and deionized water repeatedly in sequence to wash out residual n-hexane on the surfaces; finally, drying for 15min at room temperature;
C. copper plating on the surface of the stainless steel net: preparing a certain amount of blue vitriol CuSO4·5H2O, concentrated sulfuric acid H2SO4And distilled water H2Taking a piece of copper sheet as an anode, taking the stainless steel mesh obtained in the step B as a cathode, and plating copper on the surface of the cathode stainless steel mesh under the action of a direct-current power supply; taking out the copper-plated stainless steel mesh, washing with deionized water, and quickly drying;
D. preparing a super-amphiphilic stainless steel net: preparing a certain amount of sodium hydroxide NaOH as electrolyte, taking a piece of copper sheet as a cathode, taking the copper-plated stainless steel mesh obtained in the step C as an anode, and growing copper hydroxide Cu (OH) on the surface of the anode copper-plated stainless steel mesh under the action of a direct-current power supply2(ii) a Copper plated stainless steelAnd taking out the steel mesh, cleaning the steel mesh with deionized water, and quickly blow-drying.
Further, in the step C, the concentration of the copper sulfate solution is 200 g/L.
Further, in the step C, the adding amount of concentrated sulfuric acid is: 50ml of H2SO4:1L H2O。
Further, in the step D, the concentration of the sodium hydroxide solution is 2mol/L.
Further, in the step C, when the direct current power supply works stably, the current in the copper electrodeposition process is 1A, and the deposition time is 5 min.
Further, in the step D, when the direct current power supply works stably, the current is 0.1A in the process of growing the copper hydroxide by anodic oxidation, and the deposition time is 7 min.
The invention has the beneficial effects that: compared with the prior art, the invention has the advantages that:
1. electrochemical preparation, simple process and easy large-scale preparation.
2. The full water system does not use any modifier and organic solvent, does not cause secondary pollution, and is green and environment-friendly.
3. The prepared super-amphiphilic stainless steel mesh has self-adaptive wettability and can realize the separation of emulsion according to requirements.
4. The prepared super-amphiphilic stainless steel mesh has good antifouling performance and can be used for multiple times.
Drawings
FIG. 1 is a scanning electron microscope image of the original stainless steel mesh, electrodeposited and anodized stainless steel mesh of example 1 of the present invention.
FIG. 2 is a graph showing the contact angle of water in air, the contact angle of oil under water, and the contact angle of water under oil in the stainless steel net according to example 2 of the present invention.
FIG. 3 is a separation test of three oil-in-water emulsions and three water-in-oil emulsions and an antifouling cycle test of a xylene-in-water emulsion and a xylene-in-water emulsion of the super-amphiphilic stainless steel mesh in example 3 of the present invention.
FIG. 4 is a sand impact test of the super-amphiphilic stainless steel net according to example 4 of the present invention to measure the mechanical properties of the separation membrane.
Detailed Description
In order to better understand the present invention, the following examples are further provided to illustrate the present invention, but the present invention is not limited to the following examples. Various changes or modifications may be effected therein by one skilled in the art and such equivalents are intended to be within the scope of the invention as defined by the claims appended hereto.
Example 1
1. Cutting a stainless steel net: the stainless steel net was cut into a size of 3X 3cm with scissors.
2. Cleaning a stainless steel net: and (3) placing the cut stainless steel net in n-hexane for ultrasonic treatment for 1h, and removing impurities such as oil stains on the surface of the stainless steel net. And (3) sequentially and repeatedly washing the two surfaces of the stainless steel mesh by using ethanol and deionized water, and washing off the residual n-hexane on the surface. Finally, it was dried at room temperature for 15 min.
3. Copper plating on the surface of the stainless steel net: preparing a certain amount of blue vitriol (CuSO)4·5H2O), concentrated sulfuric acid (H)2SO4) And distilled water (H)2O) as electrolyte, wherein the concentration of the copper sulfate solution is 200g/L, and the addition of concentrated sulfuric acid is as follows: 50ml of H2SO4:1L H2And O. And D, taking a piece of copper sheet as an anode, taking the stainless steel mesh obtained in the step B as a cathode, and plating copper on the surface of the cathode stainless steel mesh under the action of a direct-current power supply. When the direct current power supply works stably, the current in the copper electrodeposition process is 1A, and the deposition time is 5 min. And taking out the copper-plated stainless steel mesh, washing with deionized water, and quickly drying with a blower.
4. Preparing a super-amphiphilic stainless steel net: preparing a certain amount of sodium hydroxide (NaOH) as electrolyte, wherein the concentration of the sodium hydroxide solution is 2mol/L, taking a sheet of copper sheet as a cathode, taking the copper-plated stainless steel mesh obtained in the step C as an anode, and growing copper hydroxide (Cu (OH)) on the surface of the anode copper-plated stainless steel mesh under the action of a direct-current power supply2). When the direct current power supply works stably, the current in the process of growing the copper hydroxide by anodic oxidation is 0.1A, and the deposition time is 7 min. And taking out the copper-plated stainless steel mesh, washing with deionized water, and quickly drying with a blower.
5. And (3) morphology characterization: the SEM electron microscope image shows that the surface morphology of the stainless steel mesh is remarkably changed after electrodeposition and anodic oxidation. After electrodeposition, the smooth stainless steel wire is formed with copper with a protruding structure, as shown in fig. 1 a-b; after anodic oxidation, acicular copper hydroxide grows on the protruded copper, as shown in fig. 1 c-d.
Example 2
1. Cutting a stainless steel net: the stainless steel net was cut into a size of 3X 3cm with scissors.
2. Cleaning a stainless steel net: and (3) placing the cut stainless steel net in n-hexane for ultrasonic treatment for 1h, and removing impurities such as oil stains on the surface of the stainless steel net. And (3) sequentially and repeatedly washing the two surfaces of the stainless steel mesh by using ethanol and deionized water, and washing off the residual n-hexane on the surface. Finally, it was dried at room temperature for 15 min.
3. Copper plating on the surface of the stainless steel net: preparing a certain amount of blue vitriol (CuSO)4·5H2O), concentrated sulfuric acid (H)2SO4) And distilled water (H)2O) as electrolyte, wherein the concentration of the copper sulfate solution is 200g/L, and the addition of concentrated sulfuric acid is as follows: 50ml of H2SO4:1L H2And O. And D, taking a piece of copper sheet as an anode, taking the stainless steel mesh obtained in the step B as a cathode, and plating copper on the surface of the cathode stainless steel mesh under the action of a direct-current power supply. When the direct current power supply works stably, the current in the copper electrodeposition process is 1A, and the deposition time is 5 min. And taking out the copper-plated stainless steel mesh, washing with deionized water, and quickly drying with a blower.
4. Preparing a super-amphiphilic stainless steel net: preparing a certain amount of sodium hydroxide (NaOH) as electrolyte, wherein the concentration of the sodium hydroxide solution is 2mol/L, taking a sheet of copper sheet as a cathode, taking the copper-plated stainless steel mesh obtained in the step C as an anode, and growing copper hydroxide (Cu (OH)) on the surface of the anode copper-plated stainless steel mesh under the action of a direct-current power supply2). When the direct current power supply works stably, the current in the process of growing the copper hydroxide by anodic oxidation is 0.1A, and the deposition time is 7 min. And taking out the copper-plated stainless steel mesh, washing with deionized water, and quickly drying with a blower.
5. And (3) wettability characterization: the wettability of the separation membrane is a prerequisite for the ability to separate emulsions and the performance of emulsion separation. The water contact angle and the oil contact angle in the air, the underwater oil contact angle and the underwater oil contact angle in the prepared stainless steel mesh are measured. As fig. 2a shows the contact angle of water in the air, the stainless steel net shows super-hydrophilicity. As shown in fig. 2b, which is the contact angle of oil in air, the stainless steel mesh shows super lipophilicity. As shown in fig. 2c, the contact angles of the stainless steel mesh in water for three kinds of oil, i.e., p-xylene, ethyl oleate and n-octane, are shown, and the stainless steel mesh shows underwater lipophobicity. For example, fig. 2d shows the contact angle of the stainless steel net to water in three kinds of oil, i.e. xylene, n-hexane and isooctane, the stainless steel net shows hydrophobicity under oil.
Example 3
1. Cutting a stainless steel net: the stainless steel net was cut into a size of 3X 3cm with scissors.
2. Cleaning a stainless steel net: and (3) placing the cut stainless steel net in n-hexane for ultrasonic treatment for 1h, and removing impurities such as oil stains on the surface of the stainless steel net. And (3) sequentially and repeatedly washing the two surfaces of the stainless steel mesh by using ethanol and deionized water, and washing off the residual n-hexane on the surface. Finally, it was dried at room temperature for 15 min.
3. Copper plating on the surface of the stainless steel net: preparing a certain amount of blue vitriol (CuSO)4·5H2O), concentrated sulfuric acid (H)2SO4) And distilled water (H)2O) as electrolyte, wherein the concentration of the copper sulfate solution is 200g/L, and the addition of concentrated sulfuric acid is as follows: 50ml of H2SO4:1L H2And O. And D, taking a piece of copper sheet as an anode, taking the stainless steel mesh obtained in the step B as a cathode, and plating copper on the surface of the cathode stainless steel mesh under the action of a direct-current power supply. When the direct current power supply works stably, the current in the copper electrodeposition process is 1A, and the deposition time is 5 min. And taking out the copper-plated stainless steel mesh, washing with deionized water, and quickly drying with a blower.
4. Preparing a super-amphiphilic stainless steel net: preparing a certain amount of sodium hydroxide (NaOH) as electrolyte, wherein the concentration of the sodium hydroxide solution is 2mol/L, taking a sheet of copper sheet as a cathode, taking the copper-plated stainless steel mesh obtained in the step C as an anode, and growing the NaOH on the surface of the anode copper-plated stainless steel mesh under the action of a direct-current power supplyCopper (Cu (OH)2). When the direct current power supply works stably, the current in the copper electrodeposition process is 1A, and the deposition time is 5 min. When the direct current power supply works stably, the current in the process of growing the copper hydroxide by anodic oxidation is 0.1A, and the deposition time is 7 min. And taking out the copper-plated stainless steel mesh, washing with deionized water, and quickly drying with a blower.
5. Separation performance: to evaluate the emulsion separation performance of the stainless steel mesh, emulsion separation experiments were performed on three oil-in-water emulsions and three water-in-oil emulsions. FIG. 3a shows the separation flux and separation efficiency of three emulsions of stainless steel mesh p-xylene in water, ethyl oleate in water and n-octane in water. FIG. 3b shows the separation flux and separation efficiency of three emulsions of p-xylene-in-water, n-hexane-in-water and isooctane-in-water in stainless steel mesh. FIGS. 3c-d are antifouling cycle tests of stainless steel mesh against xylene in water and xylene in water emulsions.
Example 4
1. Cutting a stainless steel net: the stainless steel net was cut into a size of 3X 3cm with scissors.
2. Cleaning a stainless steel net: and (3) placing the cut stainless steel net in n-hexane for ultrasonic treatment for 1h, and removing impurities such as oil stains on the surface of the stainless steel net. And (3) sequentially and repeatedly washing the two surfaces of the stainless steel mesh by using ethanol and deionized water, and washing off the residual n-hexane on the surface. Finally, it was dried at room temperature for 15 min.
3. Copper plating on the surface of the stainless steel net: preparing a certain amount of blue vitriol (CuSO)4·5H2O), concentrated sulfuric acid (H)2SO4) And distilled water (H)2O) as electrolyte, wherein the concentration of the copper sulfate solution is 200g/L, and the addition of concentrated sulfuric acid is as follows: 50ml of H2SO4:1L H2And O. And D, taking a piece of copper sheet as an anode, taking the stainless steel mesh obtained in the step B as a cathode, and plating copper on the surface of the cathode stainless steel mesh under the action of a direct-current power supply. When the direct current power supply works stably, the current in the copper electrodeposition process is 1A, and the deposition time is 5 min. And taking out the copper-plated stainless steel mesh, washing with deionized water, and quickly drying with a blower.
4. Preparing a super-amphiphilic stainless steel net: preparing a certain amount of sodium hydroxide (NaOH) as electrolyte,the concentration of the sodium hydroxide solution is 2mol/L, a piece of copper sheet is taken as a cathode, the copper-plated stainless steel mesh obtained in the step C is taken as an anode, and copper hydroxide (Cu (OH) grows on the surface of the anode copper-plated stainless steel mesh under the action of a direct current power supply2). When the direct current power supply works stably, the current in the process of growing the copper hydroxide by anodic oxidation is 0.1A, and the deposition time is 7 min. And taking out the copper-plated stainless steel mesh, washing with deionized water, and quickly drying with a blower.
5. And (3) testing mechanical properties: an impact test was performed on a stainless steel net with 20g of sand at a height of 15 cm. The separation performance test was performed on the stainless steel net after each 10 impacts to measure the mechanical properties of the separation membrane, and the results are shown in fig. 4.
To summarize: the invention adopts a full water system construction strategy, prepares the super-amphiphilic stainless steel mesh which can adapt to the wettability by an electrochemical method, and realizes the separation of oil-water emulsion according to the requirement. Compared with an intelligent response separation membrane and a Janus membrane, the method has the advantages of simple process, large-scale production, no secondary pollution, low production and manufacturing cost and the like. Greatly promoting the practical application of the emulsion separation membrane.
Finally, it should be noted that the above-mentioned contents are only used for illustrating the technical solutions of the present invention, and not for limiting the protection scope of the present invention, and that the simple modifications or equivalent substitutions of the technical solutions of the present invention by those of ordinary skill in the art can be made without departing from the spirit and scope of the technical solutions of the present invention.
Claims (6)
1. The preparation method of the super-amphiphilic stainless steel net which is used for separating the emulsion according to the requirement and can adapt to the wettability is characterized by comprising the following steps:
A. cutting a stainless steel net: cutting the stainless steel net into a certain size by using scissors;
B. cleaning a stainless steel net: placing the cut stainless steel mesh in n-hexane for ultrasonic treatment for 1h, and removing impurities on the surface of the stainless steel mesh; washing two surfaces of the stainless steel mesh with ethanol and deionized water repeatedly in sequence to wash out residual n-hexane on the surfaces; finally, drying for 15min at room temperature;
C. copper plating on the surface of the stainless steel net: is configured toAmount of copper sulfate pentahydrate CuSO4·5H2O, concentrated sulfuric acid H2SO4And distilled water H2Taking a piece of copper sheet as an anode, taking the stainless steel mesh obtained in the step B as a cathode, and plating copper on the surface of the cathode stainless steel mesh under the action of a direct-current power supply; taking out the copper-plated stainless steel mesh, washing with deionized water, and quickly drying;
D. preparing a super-amphiphilic stainless steel net: preparing a certain amount of sodium hydroxide NaOH as electrolyte, taking a piece of copper sheet as a cathode, taking the copper-plated stainless steel mesh obtained in the step C as an anode, and growing copper hydroxide Cu (OH) on the surface of the anode copper-plated stainless steel mesh under the action of a direct-current power supply2(ii) a And taking out the copper-plated stainless steel mesh, washing with deionized water, and quickly blow-drying.
2. The method of preparing a conformable wetting stainless steel mesh for emulsion on-demand separation according to claim 1, wherein: in the step C, the concentration of the copper sulfate solution is 200 g/L.
3. The method of preparing a conformable wetting stainless steel mesh for emulsion on-demand separation according to claim 1, wherein: in the step C, the adding amount of concentrated sulfuric acid is as follows: 50ml of H2SO4:1L H2O。
4. The method of preparing a conformable wetting stainless steel mesh for emulsion on-demand separation according to claim 1, wherein: in the step D, the concentration of the sodium hydroxide solution is 2mol/L.
5. The method of preparing a conformable wetting stainless steel mesh for emulsion on-demand separation according to claim 1, wherein: in the step C, when the direct current power supply works stably, the current in the copper electrodeposition process is 1A, and the deposition time is 5 min.
6. The method of preparing a conformable wetting stainless steel mesh for emulsion on-demand separation according to claim 1, wherein: in the step D, when the direct current power supply works stably, the current in the process of growing the copper hydroxide by anodic oxidation is 0.1A, and the deposition time is 7 min.
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CN114917621A (en) * | 2022-03-25 | 2022-08-19 | 湖北大学 | Preparation method of super-amphiphilic stainless steel net for emulsion separation |
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