CN111871003A - Bionic mussel-based super-hydrophobic metal net and preparation method and application thereof - Google Patents
Bionic mussel-based super-hydrophobic metal net and preparation method and application thereof Download PDFInfo
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 123
- 239000002184 metal Substances 0.000 title claims abstract description 123
- 230000003075 superhydrophobic effect Effects 0.000 title claims abstract description 85
- 241000237536 Mytilus edulis Species 0.000 title claims abstract description 11
- 235000020638 mussel Nutrition 0.000 title claims abstract description 11
- 239000011664 nicotinic acid Substances 0.000 title claims abstract description 11
- 238000002360 preparation method Methods 0.000 title abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 71
- 239000000243 solution Substances 0.000 claims abstract description 63
- 238000001035 drying Methods 0.000 claims abstract description 31
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000000926 separation method Methods 0.000 claims abstract description 19
- 239000002253 acid Substances 0.000 claims abstract description 13
- 229960003638 dopamine Drugs 0.000 claims abstract description 11
- 239000003960 organic solvent Substances 0.000 claims abstract description 10
- 239000012266 salt solution Substances 0.000 claims abstract description 10
- -1 amino compound Chemical class 0.000 claims abstract description 7
- 239000004519 grease Substances 0.000 claims abstract description 7
- 150000003839 salts Chemical class 0.000 claims abstract description 6
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- 229910001220 stainless steel Inorganic materials 0.000 claims description 63
- 238000005406 washing Methods 0.000 claims description 18
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 17
- 238000004140 cleaning Methods 0.000 claims description 16
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- 229960001149 dopamine hydrochloride Drugs 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 12
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- 238000002791 soaking Methods 0.000 claims description 10
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- FJLUATLTXUNBOT-UHFFFAOYSA-N 1-Hexadecylamine Chemical compound CCCCCCCCCCCCCCCCN FJLUATLTXUNBOT-UHFFFAOYSA-N 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 6
- 239000011148 porous material Substances 0.000 claims description 3
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 3
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 3
- 239000003431 cross linking reagent Substances 0.000 claims description 2
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- QKNYBSVHEMOAJP-UHFFFAOYSA-N 2-amino-2-(hydroxymethyl)propane-1,3-diol;hydron;chloride Chemical compound Cl.OCC(N)(CO)CO QKNYBSVHEMOAJP-UHFFFAOYSA-N 0.000 description 18
- 239000007853 buffer solution Substances 0.000 description 18
- 239000010935 stainless steel Substances 0.000 description 18
- 235000019441 ethanol Nutrition 0.000 description 16
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 10
- 229910052709 silver Inorganic materials 0.000 description 10
- 239000004332 silver Substances 0.000 description 10
- 238000001291 vacuum drying Methods 0.000 description 10
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 8
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- 230000010355 oscillation Effects 0.000 description 7
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 5
- 239000002262 Schiff base Substances 0.000 description 5
- 150000004753 Schiff bases Chemical class 0.000 description 5
- 239000002585 base Substances 0.000 description 5
- 238000006845 Michael addition reaction Methods 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000003502 gasoline Substances 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
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- 230000008569 process Effects 0.000 description 4
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 230000003373 anti-fouling effect Effects 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 229910052731 fluorine Inorganic materials 0.000 description 3
- 239000011737 fluorine Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 3
- 229940012189 methyl orange Drugs 0.000 description 3
- 235000019476 oil-water mixture Nutrition 0.000 description 3
- 238000006722 reduction reaction Methods 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
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- 229910021645 metal ion Inorganic materials 0.000 description 2
- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 description 2
- 229960000907 methylthioninium chloride Drugs 0.000 description 2
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- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000006399 behavior Effects 0.000 description 1
- YCIMNLLNPGFGHC-UHFFFAOYSA-N catechol Chemical group OC1=CC=CC=C1O YCIMNLLNPGFGHC-UHFFFAOYSA-N 0.000 description 1
- 239000011538 cleaning material Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
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- 125000000524 functional group Chemical group 0.000 description 1
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- 125000001165 hydrophobic group Chemical group 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
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- 239000002082 metal nanoparticle Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical group CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
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- 230000002940 repellent Effects 0.000 description 1
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Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
- B01D17/0202—Separation of non-miscible liquids by ab- or adsorption
Landscapes
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
Abstract
The invention discloses a super-hydrophobic metal net based on bionic mussels and a preparation method and application thereof, and belongs to the technical field of oil-water separation materials. The preparation method of the invention comprises the following steps: pretreating the metal net to remove oxides and grease on the surface; and immersing the metal net in a dopamine solution, a metal salt solution and a long-chain amino compound solution with certain concentration in sequence for reaction, and finally drying. The preparation method provided by the invention is simple, environment-friendly, low in energy consumption and low in cost, and is beneficial to large-scale production; the wire mesh is covered with a layer of rough metal nanocluster, has higher acid resistance, alkali resistance, salt resistance, organic solvent resistance and antibacterial performance, can realize the high-efficiency separation of heavy oil and light oil mixtures in the oily wastewater under the action of gravity, is applied to the treatment of the oily wastewater, and has the separation efficiency as high as 99.8 percent.
Description
Technical Field
The invention belongs to the technical field of oil-water separation materials, and particularly relates to a super-hydrophobic metal net based on a bionic mussel, and a preparation method and application thereof.
Background
The oil-water separation is an interface phenomenon, and the special wetting material shows opposite wetting behaviors to an oil phase and a water phase in a mixture, so that the high-efficiency separation of various oil-water mixtures can be realized. The first super-wetting material found is super-hydrophobic, the contact angle of the surface of the super-wetting material to water in air is more than 150 degrees, the surface of the super-wetting material has extremely low surface energy, and the super-wetting material is an oil-water separation material with excellent performance. At present, the super-wetting material is mainly prepared by two methods, namely, a rough structure is constructed on the surface of the material, and a low-surface-energy reagent (long-chain alkyl or fluorine-containing reagent) is used for modifying the surface. The rapid development of the super-hydrophobic material has important application in the fields of oil-water separation, solar cells, sensors and the like. The superhydrophobic material is selectively wettable and repellent to achieve separation. The current super-hydrophobic materials mainly have the following problems:
(1) the stability of the rough structure on the surface of the super-hydrophobic material is poor, the fluorine-containing compound is expensive and has poor environmental protection, and the development and the application of the super-hydrophobic material are limited to a certain extent.
(2) Long manufacturing period, complex process, high preparation cost, single performance and poor antifouling performance.
(3) Some super-hydrophobic materials have poor chemical stability and single performance and are difficult to be applied to complicated and severe working environments.
In recent years, the application of the super-hydrophobic metal mesh material in oil-water separation is more and more extensive. The metal net has the characteristics of strong mechanical property and adjustable aperture, and can separate an oil-water mixture from an emulsion without secondary pollution. In addition, the oil-water separator can integrate anti-pollution, anti-corrosion, fire prevention and photocatalytic performances, can solve the pollution problem of oil products with different densities to a certain extent, and has great application value in the fields of oil-water separation, self-cleaning materials, intelligent responsiveness and the like. Luo et al (ACSOmega, 2019,4, 20486-. Khosravi et al [ Sep. Purif. Technol,2019,215,573-581] prepared CuS and Cu2S nanoparticles on a copper mesh by an in situ growth method, further modified with stearic acid to obtain a superhydrophobic material. The prepared metal mesh has super-hydrophobic or super-hydrophilic performance, but uses a fluorine-containing toxic solvent and a coating material, possibly causes secondary pollution, and the preparation method has high energy consumption and a complex preparation process, needs special instruments and equipment, and greatly reduces the application value of the metal mesh. In addition, patent CN201310100511.6 discloses a super-hydrophobic membrane, in which a dopamine polymer layer, a silver particle layer, and a thiol group bonded to silver particles are sequentially disposed on the surface of a metal substrate, and this patent uses 1H, 2H-perfluorododecanethiol for low surface energy modification, which is highly toxic and environmentally friendly, and the thiol group is bonded to the silver particles through a chemical bond, which is not highly stable.
In summary, the current oil-water separation materials need to be improved in the aspects of environmental protection, stability, tolerance and the like.
Disclosure of Invention
The invention aims to provide a bionic mussel-based super-hydrophobic metal net which is prepared from green raw materials and has high antifouling performance, self-cleaning performance and tolerance performance. The purpose is realized by the following technical scheme:
the super-hydrophobic metal net based on the bionic mussel is characterized in that a two-dimensional stainless steel wire net is used as a base body, dopamine is used as a cross-linking agent on the surface of the base body, a micro-nano rough structure and a long-chain amino compound are densely covered on the surface of the base body, and the micro-nano rough structure is a metal nanocluster structure.
Preferably, the metal nanocluster structure is composed of Au particles, Ag particles, or Pt particles.
Preferably, the amino compounds are hexadecylamine and octadecylamine.
Preferably, the aperture of the stainless steel wire mesh is 200-400 meshes.
The invention also aims to provide a preparation method of the bionic mussel-based super-hydrophobic metal net, which is used for preparing the super-hydrophobic metal net. Aiming at the defects of complex preparation method, high energy consumption, poor environmental protection and the like of the existing super-hydrophobic metal mesh material, the preparation method is simple, environment-friendly, cheap and easy to obtain. The purpose is realized by the following technical scheme:
a preparation method of a super-hydrophobic metal net based on bionic mussels comprises the following steps:
s1, preprocessing the metal net: respectively soaking the stainless steel wire mesh in an organic solvent, an HCl solution and deionized water for ultrasonic cleaning to remove oxides and grease on the surface, taking out the stainless steel wire mesh, cleaning with pure water, and drying for later use;
s2, putting the stainless steel wire mesh prepared in the step S1 into a dopamine hydrochloride solution, adjusting the pH value to 7-9, reacting at 40-60 ℃ for 20-24 h, repeatedly cleaning with pure water until the water is clear, and drying for later use;
s3, preparing the surface of the metal nanocluster: soaking the stainless steel wire mesh prepared in the step S2 in a metal salt solution, stirring and reacting for 10-14 hours at 30-60 ℃, washing with pure water for multiple times after the reaction is finished, and drying for later use; the metal salt is one of salt solutions of silver nitrate, chloroauric acid and platinum;
s4, preparing a super-hydrophobic metal net: and (4) placing the metal net prepared in the step S3 in an ethanol solution of a long-chain amino compound for reacting for 24 hours, washing for multiple times, and drying, wherein the drying mode can be vacuum drying or drying by a blast drier.
Preferably, the organic solvent is one of acetone, ethanol and methanol, and the concentration of the HCl solution is 0.1 mol/L.
Preferably, the concentration of the dopamine hydrochloride solution is 1.0 mg/mL-3.0 mg/mL.
Preferably, the concentration of the metal salt solution is 3 mM-15 mM.
The invention further aims to apply the super-hydrophobic metal net to oil-water separation, especially to complex working conditions with high salt content or high acid-base property.
The method forms a stable adhesion layer on the surface of the metal mesh by utilizing the self-polymerization of the catechol group and the amino functional group in dopamine molecules, and then reduces metal ions into metal nano particles through reduction, thereby forming a rough structure of the metal nanocluster on the surface of the metal mesh. Meanwhile, because dopamine has secondary reaction activity, long-chain hydrophobic groups are grafted to the dopamine through Michael addition/Schiff base reaction, so that low-surface-energy modification is realized, and the stable and durable super-hydrophobic metal mesh is obtained.
Tests show that the super-hydrophobic metal net has strong self-cleaning performance, and the metal net can keep a clean state and is not polluted after colored reagents such as potassium permanganate or dye and the like scattered on the surface of the metal net are washed by water flow or soaked in organic wastewater for 20 to 24 hours. The surface of the metal net forms an even, stable and compact rough structure, the pure water contact angle of the super-hydrophobic metal net is more than 150 degrees, the rolling angle is less than 5 degrees, and the condition of the super-hydrophobic material is achieved. Meanwhile, the material can still keep the super-hydrophobic performance after being soaked in strong acid, strong base, high salt and organic solution for a certain time and irradiated by ultraviolet light for a certain time. In addition, the super-hydrophobic metal net has high reusability.
Compared with the prior art, the invention has the advantages that:
(1) according to the preparation method, a layer of uniformly distributed and stable metal nanocluster rough structure is prepared on the surface of a metal mesh through the reduction effect of dopamine hydrochloride, the metal nanocluster rough structure has super-hydrophobic performance, meanwhile, the super-hydrophobic performance is further enhanced through grafting an environment-friendly fluorine-free amino compound through the secondary reaction activity of dopamine through Michael addition/Schiff base reaction, and the stability of the amino compound grafted on dopamine is higher.
(2) The stainless steel wire mesh has super-hydrophobic and super-oleophilic properties, the contact angle of the super-hydrophobic metal mesh to pure water is more than 150 degrees, the rolling angle is less than 5 degrees, and the separation performance to the mixed liquid of heavy oil and light oil is higher than 98 percent.
(3) The super-hydrophobic metal mesh has good tolerance performance, and can keep super-hydrophobic performance in strong acid, strong alkali, high salt and various organic solvents; after being irradiated by ultraviolet light, the paint still can keep higher super-hydrophobicity and has strong antifouling property, and can be used for treating oily wastewater in complex environment.
(4) The preparation method provided by the invention is simple, low in energy consumption and environment-friendly in reagent, special equipment and instruments are not needed, a stainless steel wire mesh is used, and the method is low in cost, easy to obtain and high in mechanical stability.
Drawings
FIG. 1 is an SEM image of a superhydrophobic stainless steel mesh and an original stainless steel mesh;
FIG. 2 is an XRD pattern of a superhydrophobic stainless steel mesh and an original stainless steel mesh;
FIG. 3 is a graph of the contact angles of a superhydrophobic stainless steel mesh and an original stainless steel mesh for pure water and gasoline, respectively, in air;
FIG. 4 is a representation of a silver mirror of a superhydrophobic stainless steel mesh in water;
FIG. 5 is a diagram of a process of self-cleaning methyl orange dye by a super-hydrophobic stainless steel wire mesh;
FIG. 6 is a diagram of the separation process of the petroleum ether/water mixture by the super-hydrophobic stainless steel wire net;
FIG. 7 is a graph of the separation effect of a superhydrophobic stainless steel mesh on different oil/water mixtures;
FIG. 8 is a graph of pure water contact angles of a superhydrophobic stainless steel screen after being irradiated by an ultraviolet lamp for different times;
FIG. 9 is a graph of pure water contact angle of a superhydrophobic metal mesh after being soaked in a pH solution for 24 h;
FIG. 10 is a graph of pure water contact angles of the superhydrophobic metal mesh after being soaked in different organic solvents and salt solutions for 24 h.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A super-hydrophobic metal net and a preparation method thereof are as follows:
(1) and (4) pretreating the metal mesh. Cutting a 300-mesh stainless steel wire net into square blocks of 40 x 40mm, sequentially soaking the square blocks in a dilute hydrochloric acid solution and absolute ethyl alcohol, ultrasonically cleaning for 20 minutes to remove surface oxides and grease, taking out the square blocks, cleaning the square blocks with pure water for multiple times, and drying the square blocks in a vacuum drying oven for later use.
(2) Preparation of Tris-HCl (0.01mol/L) buffer solution: 1.576g of Tris-HCl was dissolved in 1L of the solution to prepare a 10mM buffer solution.
(3) And (2) placing the metal mesh obtained in the step (1) in 1.5mg/mL dopamine hydrochloride solution, adjusting the pH value of the solution to 8.5 by using Tris-HCl buffer solution, stirring the solution in a water bath kettle for reaction for 24 hours at the temperature of 60 ℃, washing the solution for multiple times by using pure water, and drying the solution at 60 ℃ for later use.
(4) And (4) placing the metal net obtained in the step (3) in a 12mM silver nitrate solution, reacting for 12 hours on a magnetic stirrer at the reaction temperature of 60 ℃ and the rotating speed of 120r/min, washing for many times by using pure water after reaction, and placing in a vacuum drying oven to dry at 60 ℃ for later use.
(5) And (3) placing the metal mesh obtained in the step (4) in an ethanol solution of octadecylamine (1% vt), carrying out oscillation reaction for 24h, taking out, washing with absolute ethanol for multiple times, and drying in a vacuum drying oven at the temperature of 60 ℃ to obtain the super-hydrophobic metal mesh.
Fig. 1 is SEM images of the superhydrophobic stainless steel mesh prepared in this example and the original stainless steel mesh, wherein a is the original stainless steel mesh, and b is the superhydrophobic stainless steel mesh prepared in this example. As can be seen from the figure, the original stainless steel wire mesh has a smooth surface and no roughness structure. After modification, the surface of the stainless steel wire mesh is uniformly coated with a layer of rough structure, the nano rough structure is composed of silver nanoclusters, and meanwhile, the particle size and the shape of particles are irregular, so that the surface of the stainless steel wire mesh has large roughness, and the hydrophobic property of the stainless steel wire mesh is improved.
Fig. 2 is an XRD pattern of the superhydrophobic stainless steel mesh and the original stainless steel mesh obtained in this example. As can be seen from the figure, the SSM/Ag/ODA of the super-hydrophobic stainless steel wire mesh has obvious diffraction peaks of Fe at 43.5 degrees, 50.8 degrees and 74.6 degrees, and compared with the original SSM, the modification process does not damage the original structure of the metal mesh, but the diffraction intensity of the peaks is reduced, so that the surface structure is changed. Obvious characteristic diffraction peaks of Ag can be observed from an SSM/Ag/ODA spectrum, and the grain size of the rough structure on the surface can be presumed to be smaller according to the intensity and the width of the diffraction peaks.
Pure water and gasoline are respectively used as liquid phases, and the contact angle values of the super-hydrophobic stainless steel wire mesh and the original stainless steel wire mesh obtained in the embodiment to different liquid phases are measured by a full-automatic contact angle measuring instrument, and the result is shown in fig. 3. As can be seen from the figure, the pure water contact angle of the original stainless steel wire mesh is 105.4 degrees, the pure water contact angle of the super-hydrophobic stainless steel wire mesh is 165.7 degrees, and the contact angles of the original stainless steel wire mesh and the super-hydrophobic stainless steel wire mesh to gasoline are both 0 degrees, which shows that the super-hydrophobic property of the modified stainless steel wire mesh is obviously enhanced, and the super-lipophilicity is still maintained.
Fig. 4 is a silver mirror image of the superhydrophobic stainless steel mesh obtained in the embodiment in water. Ag+The metal silver is reduced into the metal silver by the dopamine, and the generated metal silver is attached to the surface of the metal mesh and is as bright as a mirror, which shows that the surface of the stainless steel mesh has a layer of dense and rough silver nano structure.
The stainless steel wire net is fixed on a glass slide, the stainless steel wire net is inclined at 45 degrees, then methyl orange dye particles are scattered on the metal net, pure water is absorbed by a rubber head dropper to wash the metal net, and the experimental process is shown in figure 5. As can be seen from the figure, when the surface of the stainless steel wire mesh is polluted by methyl orange and washed by water flow, the stainless steel wire mesh is not dyed, the clean surface can still be kept, and the self-cleaning performance is better.
The metal mesh was fixed between two microcysts, the oil-water mixture (sudan dyed the oil phase red, the water phase blue methylene blue solution for distinction) was poured in from the upper filter cup, and the separated liquid was received at the lower end with a beaker, the experimental procedure is shown in fig. 6. As can be seen from the figure, petroleum ether can rapidly pass through the super-hydrophobic stainless steel wire mesh, while the aqueous solution is retained on the mesh and cannot pass through the mesh, which illustrates the super-hydrophobicity and super-oleophylic property of the metal mesh.
The water phase and the oil phase are mixed according to the volume ratio of 1:1, the water phase is dyed by methylene blue, the oil phase is dyed by Sudan II, so that the oil-water separation process can be conveniently observed, and the experimental result is shown in figure 7. As can be seen from the figure, the separation efficiency of the super-hydrophobic stainless steel wire mesh on the mixed liquid of petroleum ether, gasoline, dichloromethane, toluene, chloroform and water is higher than 98%.
The contact angle of pure water of the superhydrophobic stainless steel mesh obtained in this example was measured after irradiating the mesh under an ultraviolet lamp (λ 254nm,15w) for various times, and the result is shown in fig. 8. As can be seen from the figure, the contact angle of the stainless steel wire mesh is reduced with the increase of the ultraviolet irradiation time, but after 12 hours of ultraviolet irradiation, the water contact angle is still more than 150 degrees, and the super-hydrophobic property is maintained.
The super-hydrophobic stainless steel wire mesh obtained in this example was immersed in hydrochloric acid and sodium hydroxide solutions of different pH values for 24 hours, and then the contact angle of pure water was measured, and the result is shown in fig. 9. As can be seen from the figure, after the material is soaked in strong acid and strong alkali solution for 24 hours, the contact angles are both measured to be larger than 150 degrees, and the super-hydrophobic property can still be maintained, thereby proving the acid resistance and alkali resistance of the material.
The superhydrophobic stainless steel wire mesh obtained in this example was immersed in different organic solvents (cyclohexane, ethanol, petroleum ether, DMF and acetone) and a high-salt solution of sodium chloride for 24 hours, and then the contact angle of pure water was measured, and the result is shown in fig. 10. According to the detection result, the water contact angle of the metal mesh treated by the organic solvent and the high-salt solution is still maintained to be more than 150 degrees, the super-hydrophobic property is maintained, and the excellent organic solvent and high-salt resistance is proved.
Example 2
A super-hydrophobic metal net and a preparation method thereof are as follows:
(1) and (4) pretreating the metal mesh. Cutting a 400-mesh stainless steel wire net into square blocks of 40 x 40mm, sequentially soaking in acetone and absolute ethyl alcohol, ultrasonically cleaning for 20 minutes to remove surface oxides and grease, taking out, cleaning with pure water for multiple times, and drying in a vacuum drying oven for later use.
(2) Preparation of Tris-HCl (0.01mol/L) buffer solution: 1.576g of Tris-HCl was dissolved in 1L of the solution to prepare a 10mM buffer solution.
(3) And (2) placing the metal net obtained in the step (1) in 1.5mg/mL dopamine hydrochloride solution, adjusting the pH of the solution to 8.5, and adjusting by using Tris-HCl buffer solution. The reaction mixture was stirred at 30 ℃ for 24 hours, washed repeatedly with pure water, and dried for future use (60 ℃).
(4) And (4) placing the metal mesh obtained in the step (3) in a 12mM silver nitrate solution, reacting for 12 hours at the reaction temperature of 30 ℃ and the rotation speed of 120r/min, washing with pure water, and then placing in a vacuum drying oven to dry at 60 ℃ for later use.
(5) And (3) placing the metal mesh obtained in the step (4) in an ethanol solution of octadecylamine (1% vt), carrying out Schiff base reaction in a constant-temperature shaking table, taking out after 24 hours of reaction, placing in absolute ethanol for washing for multiple times, and drying at 60 ℃ to obtain the super-hydrophobic metal mesh.
The difference between this example and example 1 is that the pore diameter of the stainless steel wire mesh is changed from 300 mesh to 400 mesh, and the temperature of the reduction reaction and the Michael addition/Schiff base reaction of dopamine hydrochloride is adjusted to 30 ℃. Compared with the superhydrophobic stainless steel wire mesh prepared in example 1, the nanostructured clusters on the surface of the superhydrophobic metal wire mesh prepared in example 2 are more uniform, and the contact angle of pure water is still more than 150 °.
Example 3
A super-hydrophobic metal net and a preparation method thereof are as follows:
(1) and (4) pretreating the metal mesh. Cutting a 200-mesh stainless steel wire net into squares of 40 multiplied by 40mm, sequentially soaking in acetone and absolute ethyl alcohol, ultrasonically cleaning for 20 minutes to remove surface oxides and grease, taking out, cleaning for multiple times by pure water, and drying in a vacuum drying oven for later use.
(2) Preparation of Tris-HCl (0.01mol/L) buffer solution: 1.576g of Tris-HCl was dissolved in 1L of the solution to prepare a 10mM buffer solution.
(3) And (2) placing the metal mesh obtained in the step (1) in 1.5mg/mL dopamine hydrochloride solution, adjusting the pH value to 8.5 by using Tris-HCl buffer solution, stirring and reacting in a water bath kettle for 24 hours at the temperature of 60 ℃, washing for multiple times by using pure water, and drying at 60 ℃ for later use.
(4) And (4) placing the metal net obtained in the step (3) in a 15mM silver nitrate solution, and stirring and reacting for 12 hours at the temperature of 60 ℃ at the rotating speed of 120 r/min. The metal net prepared by the reaction is washed for a plurality of times by pure water and dried for standby at the temperature of 60 ℃.
(5) And (3) placing the metal net obtained in the step (4) in an ethanol solution of octadecylamine (1% vt), carrying out oscillation reaction for 24 hours, taking out the metal net, washing the metal net with absolute ethanol for multiple times, and drying the metal net in a vacuum drying oven at the temperature of 60 ℃ to obtain the super-hydrophobic metal net.
The difference between this example and example 2 is that the temperature at which dopamine hydrochloride is reduced and Michael addition/Schiff base reaction is carried out is adjusted to 60 ℃, the pore size of the metal mesh is changed to 200 mesh, and the concentration of silver nitrate solution is changed to 15 mM.
Example 4
A super-hydrophobic metal net and a preparation method thereof are as follows:
(1) and (4) pretreating the metal mesh. Cutting a stainless steel wire mesh of 300 meshes into square blocks of 40 multiplied by 40mm, sequentially soaking in acetone, absolute ethyl alcohol and pure water, ultrasonically cleaning for 20 minutes, removing surface impurities, and drying for later use under the condition of 60 ℃.
(2) Preparation of Tris-HCl (0.01mol/L) buffer solution: 1.576g of Tris-HCl was dissolved in 1L of the solution to prepare a 10mM buffer solution.
(3) And (2) placing the metal mesh obtained in the step (1) in 1.0mg/mL dopamine hydrochloride solution, adjusting the pH value to 8.5 by using Tris-HCl buffer solution, reacting in a constant-temperature water bath kettle for 24 hours at the temperature of 60 ℃, washing for multiple times by using pure water, and drying at 60 ℃ for later use.
(4) And (4) placing the metal mesh obtained in the step (3) in a 15mM silver nitrate solution, carrying out oscillation reaction for 12 hours at the temperature of 60 ℃ and the rotating speed of 120r/min, washing the metal mesh for multiple times by using pure water after the reaction, and drying the metal mesh at the temperature of 60 ℃ for later use.
(5) And (3) placing the metal net obtained in the step (4) in an ethanol solution (1% vt) of hexadecylamine, soaking for 24 hours, taking out, washing with absolute ethanol, and drying at 60 ℃ to obtain the super-hydrophobic metal net.
The difference between the embodiment and the embodiment 3 is that the aperture of the metal mesh is changed to 300 meshes, the concentration of the dopamine hydrochloride solution is changed to 1.5mg/mL and 1.0mg/mL, and the ethanol solution of octadecylamine is changed to the ethanol solution of hexadecylamine, and the volume fraction is 1%.
Example 5
A super-hydrophobic metal net and a preparation method thereof are as follows:
(1) and (4) pretreating the metal mesh. Cutting a stainless steel wire mesh of 300 meshes into square blocks of 40 multiplied by 40mm, sequentially soaking in acetone, absolute ethyl alcohol and pure water, ultrasonically cleaning for 20 minutes, removing surface oxides and grease, and drying for later use under the condition of 60 ℃.
(2) Preparation of Tris-HCl (0.01mol/L) buffer solution: 1.576g of Tris-HCl was dissolved in 1L of the solution to prepare a 10mM buffer solution.
(3) And (2) placing the metal mesh obtained in the step (1) in 1.5mg/mL dopamine hydrochloride solution, adjusting the pH value to 8.5 by using Tris-HCl buffer solution, stirring and reacting in a water bath kettle for 24 hours at the temperature of 60 ℃, washing for multiple times by using pure water, and drying at 60 ℃ for later use.
(4) And (4) placing the metal mesh obtained in the step (3) in a 15mM chloroauric acid solution, placing the solution system in a constant-temperature gas bath oscillation reactor, reacting for 12 hours at the temperature of 80 ℃ and the rotating speed of 80r/min, and drying the reacted metal mesh at the temperature of 60 ℃ for later use.
(5) And (3) placing the metal net obtained in the step (4) in an ethanol solution of octadecylamine (1% vt), carrying out oscillation reaction for 24 hours, taking out the metal net, washing the metal net with absolute ethanol for multiple times, and drying the metal net in a vacuum drying oven at the temperature of 60 ℃ to obtain the super-hydrophobic metal net.
The difference between the example and the example 4 is that 15mM silver nitrate solution is changed to 15mM chloroauric acid solution, the temperature of dopamine reducing metal ion is changed to 80 ℃ at 60 ℃, and the ethanol solution of hexadecylamine is changed to the ethanol solution of octadecylamine, and the volume fraction is 1%.
Example 6
A super-hydrophobic metal net and a preparation method thereof are as follows:
(1) and (4) pretreating the metal mesh. Cutting a stainless steel wire mesh with the size of 400 meshes into round pieces with the size of 40 multiplied by 40mm, sequentially carrying out ultrasonic cleaning for 20 minutes in acetone, absolute ethyl alcohol and pure water, removing surface impurities, and drying for later use at 60 ℃.
(2) Preparation of Tris-HCl (0.01mol/L) buffer solution: 1.576g of Tris-HCl was accurately weighed and dispensed into a 1L volumetric flask to obtain a 10mM buffer solution.
(3) And (2) placing the metal mesh obtained in the step (1) in a dopamine hydrochloride solution of 3.0mg/mL, adjusting the pH value to 9 by using a Tris-HCl buffer solution, stirring and reacting in a water bath kettle for 20 hours at the temperature of 60 ℃, washing for multiple times by using pure water, and drying at 60 ℃ for later use.
(4) And (4) placing the metal mesh obtained in the step (3) in a 3mM chloroauric acid solution, placing the solution system in a constant-temperature gas bath oscillation reactor, reacting for 12 hours at the temperature of 60 ℃ and the rotating speed of 80r/min, and drying the reacted metal mesh at the temperature of 60 ℃ for later use.
(5) And (3) placing the metal net obtained in the step (4) in an ethanol solution of hexadecylamine (2% vt), carrying out oscillation reaction for 24 hours, washing with ethanol for multiple times, and drying in a vacuum drying oven at 60 ℃ to obtain the super-hydrophobic metal net.
This example is different from example 5 in that a 15mM chloroauric acid solution was changed to a 3.0mM chloroauric acid solution, a concentration of 1.5mg/mL dopamine hydrochloride solution was changed to 3.0mg/mL, and a reaction temperature of the chloroauric acid solution was changed to 60 ℃ at 80 ℃. The ethanol solution of octadecylamine is changed into the ethanol solution of hexadecylamine, and the volume fraction of 1 percent is changed into 2 percent.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (9)
1. The super-hydrophobic metal net based on the bionic mussel is characterized in that the super-hydrophobic metal net takes a two-dimensional stainless steel wire net as a base body, dopamine is taken as a cross-linking agent on the surface of the base body, a dense micro-nano coarse structure and a long-chain amino compound are covered on the surface of the base body, and the micro-nano coarse structure is a metal nano-cluster structure.
2. The superhydrophobic metal mesh according to claim 1, wherein the metal nanocluster structure is comprised of Au particles, Ag particles, or Pt particles.
3. The superhydrophobic metal mesh according to claim 1, wherein the amino compounds are hexadecylamine and octadecylamine.
4. The superhydrophobic metal mesh according to claim 1, wherein the stainless steel wire mesh has a pore size of 200-400 mesh.
5. A method for preparing a super-hydrophobic metal net based on a bionic mussel, which is used for preparing the super-hydrophobic metal net of claim 1, and is characterized by comprising the following steps:
s1, preprocessing the metal net: respectively soaking the stainless steel wire mesh in an organic solvent, an HCl solution and deionized water for ultrasonic cleaning to remove oxides and grease on the surface, taking out the stainless steel wire mesh, cleaning with pure water, and drying for later use;
s2, putting the stainless steel wire mesh prepared in the step S1 into a dopamine hydrochloride solution, adjusting the pH value to 7-9, reacting at 40-60 ℃ for 20-24 h, repeatedly cleaning with pure water until the water is clear, and drying for later use;
s3, preparing the surface of the metal nanocluster: soaking the stainless steel wire mesh prepared in the step S2 in a metal salt solution, stirring and reacting for 10-14 h at 30-60 ℃, washing with pure water for multiple times after the reaction is finished, and drying for later use; the metal salt is one of salt solutions of silver nitrate, chloroauric acid and platinum;
s4, preparing a super-hydrophobic metal net: and (4) placing the metal net prepared in the step S3 in an ethanol solution of a long-chain amino compound for reaction for 20-24 hours, washing for multiple times and drying.
6. The method according to claim 5, wherein the organic solvent is one of acetone, ethanol and methanol, and the concentration of the HCl solution is 0.1 mol/L.
7. The method of claim 5, wherein the concentration of the dopamine hydrochloride solution is 1.0mg/mL to 3.0 mg/mL.
8. The method according to claim 5, wherein the concentration of the metal salt solution is 3mM to 15 mM.
9. The use of the bionic mussel-based superhydrophobic metal mesh of claim 1 in oil-water separation.
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