CN102416269A - Micro/nano interface separation net as well as preparation method and application thereof - Google Patents
Micro/nano interface separation net as well as preparation method and application thereof Download PDFInfo
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- CN102416269A CN102416269A CN2011102436416A CN201110243641A CN102416269A CN 102416269 A CN102416269 A CN 102416269A CN 2011102436416 A CN2011102436416 A CN 2011102436416A CN 201110243641 A CN201110243641 A CN 201110243641A CN 102416269 A CN102416269 A CN 102416269A
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Abstract
The invention provides a micro/nano interface separation net as well as a preparation method and an application thereof. The micro/nano interface separation net comprises a metal fiber braided net and a conductive polymer layer covering the surface of the metal fiber braided net, wherein the conductive polymer layer is formed by a doped conductive polymer with redox reversibility. The micro/nano interface separation net has a simple manufacturing process, can transform between underwater super oleophobic property and underwater super lipophilic property and is suitable for different oil-water systems, thus realizing intelligent and controllable oil-water separation.
Description
Technical field
The invention belongs to chemical, technical field of function materials, be specifically related to a kind of micro-/ nano interface separating net and method for making and purposes.
Background technology
The free water that contains in the oil plant; Can influence the quality of oil plant; And plant equipment caused corrosion; The oil-polluted water of city and commercial production discharging is the severe contamination source of environment, thereby searching economy and durability, the oil-water separation method that efficient is good are the problems that commercial production, urban life need to be resolved hurrily.At present; What application was more in the oily water separation technique field is that equipment is complicated, the higher oil water separator of energy consumption; By comparison, emerging micro-/ nano interfacial separation material technology is not only a kind of environmentally friendly purification techniques, also has low energy consumption, advantage such as easy to operate.
For example; Application number is 01118387; Notification number is the Chinese invention patent of CN1239223C; Adopt the method for chemical vapour deposition (CVD) and heat cure, nanoscale low-surface-energy powder, dispersant are stirred in nano-photo catalytic binding agent and organic solvent mixed atmosphere resolve into emulsion, on 40-380 purpose metallic fiber braid; Obtain having the ultra lipophile/super-hydrophobicity nano-interface separating net of self-cleaning function successively with technologies such as spraying, dryness finalization processing, to be used for purifying the moisture of fluid.And for example; Put down in writing in the document; After fibrous braids such as 380-1500 purpose stainless steel, copper, iron, titanium, aluminium or terylene, nylon are carried out degreasing, pickling, washing, immerse in the perfluoroalkyl silicone gel colloidal sol behind the 3-30s, taking-up is dried; At 80-250 ℃ of following heat cure 10-120min, obtaining the surface coverage film thickness is the super-hydrophobic/super-oleophilic oil-water separating net of the perfluoroalkyl silicone film of 20-50nm again.But have following defective in the above-mentioned technology: one, the coat on fibrous braid surface adopts the method preparation of spraying or the dip-coating of gel colloidal sol; Need handle through super-dry or sintering typing; Complicated process of preparation; And the nethike embrane performance receives the influence of spraying/drying process easily, is difficult to guarantee the uniformity of separate mesh surface-coated thing; The 2nd, existing oil-water separating net function singlenessization fails to realize the water-oil separating that intelligence is controlled.
Summary of the invention
In view of this; Main purpose of the present invention is to provide a kind of micro-/ nano interface separating net; This micro-/ nano interface separating net, manufacture craft is simple, can ultra under water lipophile and ultra under water oleophobic property between transform each other; Be applicable to different profit systems, thereby realize the water-oil separating that intelligence is controlled.
In order to achieve the above object; The present invention provides a kind of micro-/ nano interface separating net; Said micro-/ nano interface separating net is made up of the conductive polymer coating of metallic fiber mesh grid and metallic fiber mesh grid surface coverage, and said conductive polymer coating is made up of the doping attitude conducting polymer with redox reversible property.
Further; Said doping attitude conducting polymer is through immersing the metallic fiber mesh grid in the electrolyte as working electrode; Control constant potential or constant current obtain, and said electrolyte is made up of the conducting polymer monomer of 0.01-1 weight portion, the adulterant of 0.02-2 weight portion and the distilled water of 10 weight portions.
Further, said metallic fiber mesh grid is the 40-300 order, and said metallic fiber mesh grid is stainless steel, copper, iron, aluminium or titanium net.
Further, said conducting polymer is the derivative of polypyrrole, polythiophene, polyaniline, polyparaphenylene or these polymer;
Said conducting polymer monomer is the derivative of pyrroles, thiophene, aniline, biphenyl or these monomers;
Said adulterant is anionic surfactant or the long chain organic acid with emulsifying property.
Further, said conducting polymer obtains through control constant potential 0.001-1.6V or control constant current 0.02-200mA.
Further, the thickness of said conductive polymer coating is 2-30 μ m.
Further, the fibre diameter of said micro-/ nano interface separating net is 45-150 μ m.
In order to achieve the above object, the present invention also provides a kind of preparation method of micro-/ nano interface separating net, and said preparation method may further comprise the steps:
Immersion contains in the electrolyte of conducting polymer monomer and adulterant as working electrode with the metallic fiber mesh grid; Pass through electrochemical reaction; Obtain being covered in the conductive polymer coating on metallic fiber mesh grid surface, said conductive polymer coating is made up of the doping attitude conducting polymer with redox reversible property.
Further, said doping attitude conducting polymer obtains through control constant potential or constant current, and said electrolyte is made up of the conducting polymer monomer of 0.01-1 weight portion, the adulterant of 0.02-2 weight portion and the distilled water of 10 weight portions.
Further, said metallic fiber mesh grid is the 40-300 order, and said metallic fiber mesh grid is stainless steel, copper, iron, aluminium or titanium net.
Further, said conducting polymer is the derivative of polypyrrole, polythiophene, polyaniline, polyparaphenylene or these polymer;
Said conducting polymer monomer is the derivative of pyrroles, thiophene, aniline, biphenyl or these monomers;
Said adulterant is anionic surfactant or the long chain organic acid with emulsifying property.
Further, control constant potential 0.001-1.6V or control constant current 0.02-200mA among the said preparation method.
Further, control constant potential 10-120min or control constant current 10-120min among the said preparation method.
In order to achieve the above object, the present invention also provides a kind of purposes of micro-/ nano interface separating net, and said micro-/ nano interface separating net is used for water-oil separating.
Compared with prior art; Micro-/ nano interface separating net of the present invention; Have the following advantages: (1) the present invention is immersed the metallic fiber mesh grid and is contained in the electrolyte liquid of adulterant and conducting polymer monomer as working electrode, adopt the method for constant potential or constant current polymerization to prepare the micro-/ nano interface separating net, and preparation technology is simple; Need not handle through super-dry/sintering typing; Avoided the nethike embrane performance to receive the influence of spraying/drying process, and preparation method of the present invention accurately control easily, can guarantee that micro-/ nano interface separating net surface texture is even; (2) because the doping attitude conducting polymer that covers on the wire netting of micro-/ nano interface separating net of the present invention has good redox reversible property; Make mode that micro-/ nano interface separating net of the present invention can be through electrochemical oxidation/reduction at the ultra oleophobic property under the oxidation state and go back reversible transition between the ultra lipophile under the ortho states under water under water; And response speed is fast; So applicable to different profit systems, functional diversities, thereby the intelligent controlled separation of realization profit; (3) electrolyte of using among the preparation method of the present invention is the dispersion system of adulterant/polymer monomer, and environmental pollution is less.
Description of drawings
Fig. 1 is the scanning electron microscope diagram one of micro-/ nano interface separating net of the present invention;
Fig. 2 is the scanning electron microscope diagram two of micro-/ nano interface separating net of the present invention;
Fig. 3 is the lubricant nature of the oil immersion under water sketch map under the micro-/ nano interface separating net oxidation state of the present invention;
Fig. 4 is the also lubricant nature of the oil immersion under water sketch map under the ortho states of micro-/ nano interface separating net of the present invention.
The specific embodiment
Below in conjunction with accompanying drawing and embodiment to micro-/ nano interface separating net of the present invention and its production and use specify.
Micro-/ nano interface separating net provided by the invention is made up of the conductive polymer coating of metallic fiber mesh grid of 40-300 purpose and metallic fiber mesh grid surface coverage; Said conductive polymer coating is made up of the doping attitude conducting polymer with redox reversible property; Said doping attitude conducting polymer is through immersing the metallic fiber mesh grid in the electrolyte as working electrode; With the platinized platinum is auxiliary electrode; Silver-silver chloride electrode is that reference electrode makes up three-electrode system, and control constant potential or constant current obtain; Wherein, said electrolyte is made up of the conducting polymer monomer of 0.01-1 weight portion, the adulterant of 0.02-2 weight portion and the distilled water of 10 weight portions.
Above-mentionedly be used for metallic fiber mesh grid of the present invention and can be metallic fiber mesh grids such as stainless steel, copper, iron, aluminium or titanium; Said conducting polymer can be the derivative of polypyrrole, polythiophene, polyaniline, polyparaphenylene or these polymer, as gathers (1-methylene-2-methyl naphthalene)-N-pyrroles, gathers the enedioxy thiophene, gathers the 3-hexyl thiophene or gather 2,5-dimethoxyaniline etc.; Said conducting polymer monomer can be the derivative of pyrroles, thiophene, aniline, biphenyl or these monomers, like (1-methylene-2-methyl naphthalene)-N-pyrroles, 3,4-enedioxy thiophene, 3-hexyl thiophene or 2,5-dimethoxyaniline etc.; Said adulterant can be multiple anionic surfactant (like higher fatty acid salt, alkyl sulfate, alkylsulfonate or alkylbenzenesulfonate etc.) or the long chain organic acid (like alkyl benzene sulphonate, alkyl sulfonic acid or perfluorocarboxylic acid etc.) with emulsifying property, for example odium stearate, lauryl sodium sulfate/potassium/ammonium/magnesium/lithium salts, dodecyl sodium sulfonate potassium/sodium/ammonium salt, perfluorooctane sulfonate, perfluorooctane sulfonate potassium/sodium/ammonium salt, perfluoro octyl sulfonic acid tetraethyl amine, DBSA, neopelex/calcium/ammonium/triethanolamine salt, perfluor decanedioic acid, perfluoro caprylic acid or perfluoro-pelargonic acid etc.
Because the doping attitude conducting polymer that covers on the wire netting of micro-/ nano interface separating net of the present invention has good redox reversible property, make the ultra oleophobic property that micro-/ nano interface separating net of the present invention can be under oxidation state under water and go back reversible transition between the ultra lipophile under the ortho states under water.Be specially and place electrolyte (like LiClO as working electrode micro-/ nano interface separating net of the present invention
4Solution) in, as auxiliary electrode, (saturated) calomel electrode is as reference electrode with platinized platinum; Control current potential (as 0.25 to 0.5V); Make the doping attitude conducting polymer generation oxidation reaction of micro-/ nano interfacial separation net surface, form the micro-/ nano interface separating net under the oxidation state, this moment, micro-/ nano interface separating net of the present invention presented the ultra oleophobic property under the oxidation state under water; Fig. 3 is the lubricant nature of the oil immersion under water sketch map under the micro-/ nano interface separating net oxidation state of the present invention; As can be seen from Figure 3, oil droplet is nonwetting basically on the net in the micro-/ nano interfacial separation of oxidation state of the present invention, shows ultra oleophobic property under water; In addition; Also can control current potential (as-0.8V to-0.5V); Make the doping attitude conducting polymer generation reduction reaction of micro-/ nano interfacial separation net surface of the present invention, form and go back the micro-/ nano interface separating net under the ortho states, this moment, micro-/ nano interface separating net of the present invention presented the ultra lipophile of going back under the ortho states under water; Fig. 4 is the lubricant nature of the oil immersion under water sketch map of micro-/ nano interface separating net of the present invention; As can be seen from Figure 4, oil droplet leaks down from the micro-/ nano interfacial separation that the present invention goes back ortho states on the net, shows ultra lipophile under water.Therefore micro-/ nano interface separating net of the present invention is applicable to different profit systems, functional diversities.
Fig. 1 and Fig. 2 are respectively the scanning electron microscope diagram of micro-/ nano interface separating net of the present invention, wherein adopt SEM (FE-SEMJEOL JSM-6700F) amplify respectively 300 times (as shown in Figure 1, test condition: HV 20.00kV; WD 11.1mm) and 5000 times (as shown in Figure 2; Test condition: HV 20.00kV, WD 11.0mm) surface topography of observation micro-/ nano interface separating net of the present invention is found out from Fig. 1 and Fig. 2; Cover the layer of even conductive polymer coating in the metallic fiber mesh grid of the present invention; Micro-/ nano interfacial separation net surface is coarse pleated structure (like Fig. 1), has a micron projection (like Fig. 2) on the fold, adopts SEM; Observe the about 45-150 μ of the fibre diameter m of micro-/ nano interface separating net of the present invention, the about 2-30 μ of the thickness m of doping attitude conductive polymer coating.
Like Fig. 1 and shown in Figure 2; Micro-/ nano interface separating net of the present invention has the grid concaveconvex structure; The doping attitude conducting polymer of growing on the metallic fiber surface demonstrates multistage micro; Micro-/ nano interface separating net surface roughness of the present invention is increased, thereby make micro-/ nano interface separating net of the present invention show the ultra oleophobic property of oxidation state under water; This micro-/ nano interface separating net is carried out in the process of electrochemical reduction; Doping attitude conducting polymer is to the anion dedoping; Cause conducting polymer surface free energy, surface microstructure to change; Even change near the oil water interfacial tension the micro-/ nano interface separating net, and under the effect of certain kalimeris lattice Buddhist nun effect, the micro-/ nano interface separating net is appeared go back the ultra lipophile under the ortho states under water.
Micro-/ nano interface separating net of the present invention can be used for water-oil separating, specifically can be applicable to moisture oil plant purification, oil-polluted water processing and be used for microfluidic device.
The present invention also provides a kind of preparation method of above-mentioned micro-/ nano interface separating net, specifically comprises the steps:
(1) mesh grid of 40-300 purpose metallic fiber is alternately immersed carries out ultrasonic cleaning in absolute ethyl alcohol, the deionized water, dry under the last normal temperature;
(2) preparation contains the electrolyte of adulterant/conducting polymer monomer, and this electrolyte specifically is made up of the conducting polymer monomer of 0.01-1 weight portion, the adulterant of 0.02-2 weight portion and the distilled water of 10 weight portions, with the ultrasonic emulsion that is dispersed into of electrolyte;
(3) with metallic fiber mesh grid, platinized platinum, and silver-silver chloride electrode immerse in the above-mentioned emulsion, wherein the metallic fiber mesh grid is a working electrode, platinized platinum is an auxiliary electrode, silver-silver chloride electrode is a reference electrode, constitutes three-electrode system, carries out polymerisation;
In this step, can adopt the method for control constant potential or constant current to carry out polymerisation, specifically can control constant potential 0.001-1.6V, reaction 10-120min, or control constant current 0.02-200mA, reaction 10-120min.
(4) reaction finishes the mesh grid of back taking-up metallic fiber, with the alternately flushing of absolute ethyl alcohol, deionized water, obtains micro-/ nano interface separating net of the present invention.
Below for the specific embodiment of micro-/ nano interface separating net of the present invention.
One, the preparation of micro-/ nano interface separating net in the embodiment of the invention
Embodiment 1
(1) (2.5cm * 1cm) alternately immerses and carries out ultrasonic cleaning in absolute ethyl alcohol, the deionized water, dries under the last normal temperature with 40 purpose stainless steel fibre mesh grids;
(2) preparation contains the electrolyte of adulterant/conducting polymer monomer, and this electrolyte is specifically by 3 of 0.01 gram, and the lauryl sodium sulfate of 4-enedioxy thiophene, 0.05 gram and the distilled water of 10 grams are formed, with the ultrasonic emulsion that is dispersed into of electrolyte;
(3) with stainless steel fibre mesh grid, smooth platinized platinum (2cm * 1cm), and silver-silver chloride electrode (concentration of electrolyte is 3M) immerse in the emulsion of step 2; Wherein the stainless steel fibre mesh grid is a working electrode; Platinized platinum is an auxiliary electrode, and silver-silver chloride electrode is a reference electrode, constitutes three-electrode system; Control constant potential 1.6V, reaction 10min;
(4) reaction finishes the mesh grid of back taking-up stainless steel fibre, with the alternately flushing of absolute ethyl alcohol, deionized water, obtains micro-/ nano interface separating net 1 of the present invention.
Embodiment 2
(1) (2.5cm * 1cm) alternately immerses and carries out ultrasonic cleaning in absolute ethyl alcohol, the deionized water, dries under the last normal temperature with 100 purpose stainless steel fibre mesh grids;
(2) preparation contains the electrolyte of adulterant/conducting polymer monomer, and this electrolyte specifically is made up of the 3-hexyl thiophene of 0.05 gram, the neopelex of 0.5 gram and the distilled water of 10 grams, with the ultrasonic emulsion that is dispersed into of electrolyte;
(3) with stainless steel fibre mesh grid, smooth platinized platinum (2cm * 1cm), and silver-silver chloride electrode (concentration of electrolyte is 3M) immerse in the emulsion of step 2; Wherein the stainless steel fibre mesh grid is a working electrode; Platinized platinum is an auxiliary electrode, and silver-silver chloride electrode is a reference electrode, constitutes three-electrode system; Control constant potential 1.4V, reaction 90min;
(4) reaction finishes the mesh grid of back taking-up stainless steel fibre, with the alternately flushing of absolute ethyl alcohol, deionized water, obtains micro-/ nano interface separating net 2 of the present invention.
Embodiment 3
(1) (2.5cm * 1cm) alternately immerses and carries out ultrasonic cleaning in absolute ethyl alcohol, the deionized water, dries under the last normal temperature with 200 purpose stainless steel fibre mesh grids;
(2) preparation contains the electrolyte of adulterant/conducting polymer monomer, and this electrolyte specifically is made up of the thiophene of 0.1 gram, the DBSA of 0.25 gram and the distilled water of 10 grams, with the ultrasonic emulsion that is dispersed into of electrolyte;
(3) with stainless steel fibre mesh grid, smooth platinized platinum (2cm * 1cm), and silver-silver chloride electrode (concentration of electrolyte is 3M) immerse in the emulsion of step 2; Wherein the stainless steel fibre mesh grid is a working electrode; Platinized platinum is an auxiliary electrode, and silver-silver chloride electrode is a reference electrode, constitutes three-electrode system; Control constant current 20mA, reaction 30min;
(4) reaction finishes the mesh grid of back taking-up stainless steel fibre, with the alternately flushing of absolute ethyl alcohol, deionized water, obtains micro-/ nano interface separating net 3 of the present invention.
Embodiment 4
(1) (2.5cm * 1cm) alternately immerses and carries out ultrasonic cleaning in absolute ethyl alcohol, the deionized water, dries under the last normal temperature with 300 purpose stainless steel fibre mesh grids;
(2) preparation contains the electrolyte of adulterant/conducting polymer monomer, and this electrolyte is specifically by 3 of 0.2 gram, and the ammonium lauryl sulfate of 4-enedioxy thiophene, 0.35 gram and the distilled water of 10 grams are formed, with the ultrasonic emulsion that is dispersed into of electrolyte;
(3) with stainless steel fibre mesh grid, smooth platinized platinum (2cm * 1cm), and silver-silver chloride electrode (concentration of electrolyte is 3M) immerse in the emulsion of step 2; Wherein the stainless steel fibre mesh grid is a working electrode; Platinized platinum is an auxiliary electrode, and silver-silver chloride electrode is a reference electrode, constitutes three-electrode system; Control constant current 10mA, reaction 44min;
(4) reaction finishes the mesh grid of back taking-up stainless steel fibre, with the alternately flushing of absolute ethyl alcohol, deionized water, obtains micro-/ nano interface separating net 4 of the present invention.
Embodiment 5
(1) (2.5cm * 1cm) alternately immerses and carries out ultrasonic cleaning in absolute ethyl alcohol, the deionized water, dries under the last normal temperature with 40 purpose copper fiber knitted nets;
(2) preparation contains the electrolyte of adulterant/conducting polymer monomer, and this electrolyte is specifically by 3 of 0.5 gram, and the perfluoro-pelargonic acid of 4-enedioxy thiophene, 2 grams and the distilled water of 10 grams are formed, with the ultrasonic emulsion that is dispersed into of electrolyte;
(3) with copper fiber knitted net, smooth platinized platinum (2cm * 1cm), and silver-silver chloride electrode (concentration of electrolyte is 3M) immerse in the emulsion of step 2; Wherein the copper fiber knitted net is a working electrode; Platinized platinum is an auxiliary electrode, and silver-silver chloride electrode is a reference electrode, constitutes three-electrode system; Control constant voltage 1.3V, reaction 120min;
(4) reaction finishes back taking-up copper fiber knitted net, with the alternately flushing of absolute ethyl alcohol, deionized water, obtains micro-/ nano interface separating net 5 of the present invention.
Embodiment 6
(1) (2.5cm * 1cm) alternately immerses and carries out ultrasonic cleaning in absolute ethyl alcohol, the deionized water, dries under the last normal temperature with 200 purpose copper fiber knitted nets;
(2) preparation contains the electrolyte of adulterant/conducting polymer monomer, and this electrolyte specifically is made up of the pyrroles of 0.02 gram, the perfluoro octyl sulfonic acid tetraethyl amine of 0.05 gram and the distilled water of 10 grams, with the ultrasonic emulsion that is dispersed into of electrolyte;
(3) with copper fiber knitted net, smooth platinized platinum (2cm * 1cm), and silver-silver chloride electrode (concentration of electrolyte is 3M) immerse in the emulsion of step 2; Wherein the copper fiber knitted net is a working electrode; Platinized platinum is an auxiliary electrode, and silver-silver chloride electrode is a reference electrode, constitutes three-electrode system; Control constant current 0.02mA, reaction 120min;
(4) reaction finishes back taking-up copper fiber knitted net, with the alternately flushing of absolute ethyl alcohol, deionized water, obtains micro-/ nano interface separating net 6 of the present invention.
Embodiment 7
(1) (2.5cm * 1cm) alternately immerses and carries out ultrasonic cleaning in absolute ethyl alcohol, the deionized water, dries under the last normal temperature with 100 purpose iron fiber mesh grids;
(2) preparation contains the electrolyte of adulterant/conducting polymer monomer, and this electrolyte specifically is made up of the pyrroles of 0.01 gram, the dodecyl sodium sulfate of 0.02 gram and the distilled water of 10 grams, with the ultrasonic emulsion that is dispersed into of electrolyte;
(3) with iron fiber mesh grid, smooth platinized platinum (2cm * 1cm), and silver-silver chloride electrode (concentration of electrolyte is 3M) immerse in the emulsion of step 2; Wherein the iron fiber mesh grid is a working electrode; Platinized platinum is an auxiliary electrode, and silver-silver chloride electrode is a reference electrode, constitutes three-electrode system; Control constant voltage 0.001V, reaction 20min;
(4) reaction finishes the mesh grid of back taking-up iron fiber, with the alternately flushing of absolute ethyl alcohol, deionized water, obtains micro-/ nano interface separating net 7 of the present invention.
Embodiment 8
(1) (2.5cm * 1cm) alternately immerses and carries out ultrasonic cleaning in absolute ethyl alcohol, the deionized water, dries under the last normal temperature with 300 purpose iron fiber mesh grids;
(2) preparation contains the electrolyte of adulterant/conducting polymer monomer, and this electrolyte specifically is made up of (1-methylene-2-the methyl naphthalene)-N-pyrroles of 0.05 gram, the perfluorooctane sulfonate of 0.5 gram and the distilled water of 10 grams, with the ultrasonic emulsion that is dispersed into of electrolyte;
(3) with iron fiber mesh grid, smooth platinized platinum (2cm * 1cm), and silver-silver chloride electrode (concentration of electrolyte is 3M) immerse in the emulsion of step 2; Wherein the iron fiber mesh grid is a working electrode; Platinized platinum is an auxiliary electrode, and silver-silver chloride electrode is a reference electrode, constitutes three-electrode system; Control constant voltage 0.5V, reaction 30min;
(4) reaction finishes the mesh grid of back taking-up iron fiber, with the alternately flushing of absolute ethyl alcohol, deionized water, obtains micro-/ nano interface separating net 8 of the present invention.
Embodiment 9
(1) (2.5cm * 1cm) alternately immerses and carries out ultrasonic cleaning in absolute ethyl alcohol, the deionized water, dries under the last normal temperature with 40 purpose titanium fiber knitted nets;
(2) preparation contains the electrolyte of adulterant/conducting polymer monomer, and this electrolyte specifically is made up of the aniline of 0.01 gram, the DBSA triethanolamine sodium of 0.025 gram and the distilled water of 10 grams, with the ultrasonic emulsion that is dispersed into of electrolyte;
(3) with titanium fiber knitted net, smooth platinized platinum (2cm * 1cm), and silver-silver chloride electrode (concentration of electrolyte is 3M) immerse in the emulsion of step 2; Wherein the titanium fiber knitted net is a working electrode; Platinized platinum is an auxiliary electrode, and silver-silver chloride electrode is a reference electrode, constitutes three-electrode system; Control constant current 3mA, reaction 10min;
(4) reaction finishes back taking-up titanium fiber knitted net, with the alternately flushing of absolute ethyl alcohol, deionized water, obtains micro-/ nano interface separating net 9 of the present invention.
Embodiment 10
(1) (2.5cm * 1cm) alternately immerses and carries out ultrasonic cleaning in absolute ethyl alcohol, the deionized water, dries under the last normal temperature with 100 purpose titanium fiber knitted nets;
(2) preparation contains the electrolyte of adulterant/conducting polymer monomer, and this electrolyte specifically is made up of the aniline of 0.05 gram, the perfluorooctane sulfonate potassium of 0.25 gram and the distilled water of 10 grams, with the ultrasonic emulsion that is dispersed into of electrolyte;
(3) with titanium fiber knitted net, smooth platinized platinum (2cm * 1cm), and silver-silver chloride electrode (concentration of electrolyte is 3M) immerse in the emulsion of step 2; Wherein the titanium fiber knitted net is a working electrode; Platinized platinum is an auxiliary electrode, and silver-silver chloride electrode is a reference electrode, constitutes three-electrode system; Control constant current 200mA, reaction 30min;
(4) reaction finishes back taking-up titanium fiber knitted net, with the alternately flushing of absolute ethyl alcohol, deionized water, obtains micro-/ nano interface separating net 10 of the present invention.
Embodiment 11
(1) (2.5cm * 1cm) alternately immerses and carries out ultrasonic cleaning in absolute ethyl alcohol, the deionized water, dries under the last normal temperature with 40 purpose aluminum fiber mesh grids;
(2) preparation contains the electrolyte of adulterant/conducting polymer monomer, and this electrolyte specifically is made up of the aniline of 0.1 gram, the odium stearate of 0.5 gram and the distilled water of 10 grams, with the ultrasonic emulsion that is dispersed into of electrolyte;
(3) with aluminum fiber mesh grid, smooth platinized platinum (2cm * 1cm), and silver-silver chloride electrode (concentration of electrolyte is 3M) immerse in the emulsion of step 2; Wherein the aluminum fiber mesh grid is a working electrode; Platinized platinum is an auxiliary electrode, and silver-silver chloride electrode is a reference electrode, constitutes three-electrode system; Control constant voltage 0.1V, reaction 44min;
(4) reaction finishes the mesh grid of back taking-up aluminum fiber, with the alternately flushing of absolute ethyl alcohol, deionized water, obtains micro-/ nano interface separating net 11 of the present invention.
Embodiment 12
(1) (2.5cm * 1cm) alternately immerses and carries out ultrasonic cleaning in absolute ethyl alcohol, the deionized water, dries under the last normal temperature with 100 purpose aluminum fiber mesh grids;
(2) preparation contains the electrolyte of adulterant/conducting polymer monomer, and this electrolyte is specifically by 2 of 0.5 gram, and the perfluor decanedioic acid of 5-dimethoxyaniline, 0.1 gram and the distilled water of 10 grams are formed, with the ultrasonic emulsion that is dispersed into of electrolyte;
(3) with aluminum fiber mesh grid, smooth platinized platinum (2cm * 1cm), and silver-silver chloride electrode (concentration of electrolyte is 3M) immerse in the emulsion of step 2; Wherein the aluminum fiber mesh grid is a working electrode; Platinized platinum is an auxiliary electrode, and silver-silver chloride electrode is a reference electrode, constitutes three-electrode system; Control constant voltage 1V, reaction 20min;
(4) reaction finishes the mesh grid of back taking-up aluminum fiber, with the alternately flushing of absolute ethyl alcohol, deionized water, obtains micro-/ nano interface separating net 12 of the present invention.
Embodiment 13
(1) (2.5cm * 1cm) alternately immerses and carries out ultrasonic cleaning in absolute ethyl alcohol, the deionized water, dries under the last normal temperature with 200 purpose aluminum fiber mesh grids;
(2) preparation contains the electrolyte of adulterant/conducting polymer monomer, and this electrolyte specifically is made up of the biphenyl of 1 gram, the perfluorooctane sulfonate sodium of 0.45 gram and the distilled water of 10 grams, with the ultrasonic emulsion that is dispersed into of electrolyte;
(3) with aluminum fiber mesh grid, smooth platinized platinum (2cm * 1cm), and silver-silver chloride electrode (concentration of electrolyte is 3M) immerse in the emulsion of step 2; Wherein the aluminum fiber mesh grid is a working electrode; Platinized platinum is an auxiliary electrode, and silver-silver chloride electrode is a reference electrode, constitutes three-electrode system; Control constant voltage 1.5V, reaction 60min;
(4) reaction finishes the mesh grid of back taking-up aluminum fiber, with the alternately flushing of absolute ethyl alcohol, deionized water, obtains micro-/ nano interface separating net 13 of the present invention.
Two, the lubricant nature of oil immersion under water of micro-/ nano interface separating net test in the embodiment of the invention
Embodiment 1 test
As working electrode, platinized platinum is as auxiliary electrode with the micro-/ nano interface separating net 1 that makes in the foregoing description 1, and saturated calomel electrode immerses the LiClO of 0.1M as reference electrode
4In the solution, control current potential 0.3V, reaction time 45s obtains the micro-/ nano interface separating net 1 under the oxidation state, adopts contact angle measurement (TBU90E, German DATAPHYSICS company) to measure the contact angle of micro-/ nano interface separating net 1 and oil under the oxidation state;
In addition, control current potential-0.8V, reaction time 45s obtains going back the micro-/ nano interface separating net 1 ortho states under, adopts contact angle measurement (TBU90E, German DATAPHYSICS company) to measure micro-/ nano interface separating net 1 and the oily contact angle gone back ortho states under.
Embodiment 2 tests
As working electrode, platinized platinum is as auxiliary electrode with the micro-/ nano interface separating net 2 that makes in the foregoing description 2, and saturated calomel electrode immerses the LiClO of 0.1M as reference electrode
4In the solution, control current potential 0.35V, reaction time 45s obtains the micro-/ nano interface separating net 2 under the oxidation state, adopts contact angle measurement (TBU90E, German DATAPHYSICS company) to measure the contact angle of micro-/ nano interface separating net 2 and oil under the oxidation state;
In addition, control current potential-0.7V, reaction time 45s obtains going back the micro-/ nano interface separating net 2 ortho states under, adopts contact angle measurement (TBU90E, German DATAPHYSICS company) to measure micro-/ nano interface separating net 2 and the oily contact angle gone back ortho states under.
Embodiment 3 tests
As working electrode, platinized platinum is as auxiliary electrode with the micro-/ nano interface separating net 3 that makes in the foregoing description 3, and saturated calomel electrode immerses the LiClO of 0.1M as reference electrode
4In the solution, control current potential 0.5V, reaction time 45s obtains the micro-/ nano interface separating net 3 under the oxidation state, adopts contact angle measurement (TBU90E, German DATAPHYSICS company) to measure the contact angle of micro-/ nano interface separating net 3 and oil under the oxidation state;
In addition, control current potential-0.6V, reaction time 45s obtains going back the micro-/ nano interface separating net 3 ortho states under, adopts contact angle measurement (TBU90E, German DATAPHYSICS company) to measure micro-/ nano interface separating net 3 and the oily contact angle gone back ortho states under.
Embodiment 4 tests
As working electrode, platinized platinum is as auxiliary electrode with the micro-/ nano interface separating net 4 that makes in the foregoing description 4, and saturated calomel electrode immerses the LiClO of 0.1M as reference electrode
4In the solution, control current potential 0.3V, reaction time 45s obtains the micro-/ nano interface separating net 4 under the oxidation state, adopts contact angle measurement (TBU90E, German DATAPHYSICS company) to measure the contact angle of micro-/ nano interface separating net 4 and oil under the oxidation state;
In addition, control current potential-0.8V, reaction time 45s obtains going back the micro-/ nano interface separating net 4 ortho states under, adopts contact angle measurement (TBU90E, German DATAPHYSICS company) to measure micro-/ nano interface separating net 4 and the oily contact angle gone back ortho states under.
Embodiment 5 tests
As working electrode, platinized platinum is as auxiliary electrode with the micro-/ nano interface separating net 5 that makes in the foregoing description 5, and saturated calomel electrode immerses the LiClO of 0.1M as reference electrode
4In the solution, control current potential 0.45V, reaction time 45s obtains the micro-/ nano interface separating net 5 under the oxidation state, adopts contact angle measurement (TBU90E, German DATAPHYSICS company) to measure the contact angle of micro-/ nano interface separating net 5 and oil under the oxidation state;
In addition, control current potential-0.5V, reaction time 45s obtains going back the micro-/ nano interface separating net 5 ortho states under, adopts contact angle measurement (TBU90E, German DATAPHYSICS company) to measure micro-/ nano interface separating net 5 and the oily contact angle gone back ortho states under.
Embodiment 6 tests
As working electrode, platinized platinum is as auxiliary electrode with the micro-/ nano interface separating net 6 that makes in the foregoing description 6, and saturated calomel electrode immerses the LiClO of 0.1M as reference electrode
4In the solution, control current potential 0.3V, reaction time 45s obtains the micro-/ nano interface separating net 6 under the oxidation state, adopts contact angle measurement (TBU90E, German DATAPHYSICS company) to measure the contact angle of micro-/ nano interface separating net 6 and oil under the oxidation state;
In addition, control current potential-0.7V, reaction time 45s obtains going back the micro-/ nano interface separating net 6 ortho states under, adopts contact angle measurement (TBU90E, German DATAPHYSICS company) to measure micro-/ nano interface separating net 6 and the oily contact angle gone back ortho states under.
Embodiment 7 tests
As working electrode, platinized platinum is as auxiliary electrode with the micro-/ nano interface separating net 7 that makes in the foregoing description 7, and saturated calomel electrode immerses the LiClO of 0.1M as reference electrode
4In the solution, control current potential 0.5V, reaction time 45s obtains the micro-/ nano interface separating net 7 under the oxidation state, adopts contact angle measurement (TBU90E, German DATAPHYSICS company) to measure the contact angle of micro-/ nano interface separating net 7 and oil under the oxidation state;
In addition, control current potential-0.65V, reaction time 45s obtains going back the micro-/ nano interface separating net 7 ortho states under, adopts contact angle measurement (TBU90E, German DATAPHYSICS company) to measure micro-/ nano interface separating net 7 and the oily contact angle gone back ortho states under.
Embodiment 8 tests
As working electrode, platinized platinum is as auxiliary electrode with the micro-/ nano interface separating net 8 that makes in the foregoing description 8, and saturated calomel electrode immerses the LiClO of 0.1M as reference electrode
4In the solution, control current potential 0.35V, reaction time 45s obtains the micro-/ nano interface separating net 8 under the oxidation state, adopts contact angle measurement (TBU90E, German DATAPHYSICS company) to measure the contact angle of micro-/ nano interface separating net 8 and oil under the oxidation state;
In addition, control current potential-0.75V, reaction time 45s obtains going back the micro-/ nano interface separating net 8 ortho states under, adopts contact angle measurement (TBU90E, German DATAPHYSICS company) to measure micro-/ nano interface separating net 8 and the oily contact angle gone back ortho states under.
Embodiment 9 tests
As working electrode, platinized platinum is as auxiliary electrode with the micro-/ nano interface separating net 9 that makes in the foregoing description 9, and saturated calomel electrode immerses the LiClO of 0.1M as reference electrode
4In the solution, control current potential 0.4V, reaction time 45s obtains the micro-/ nano interface separating net 9 under the oxidation state, adopts contact angle measurement (TBU90E, German DATAPHYSICS company) to measure the contact angle of micro-/ nano interface separating net 9 and oil under the oxidation state;
In addition, control current potential-0.8V, reaction time 45s obtains going back the micro-/ nano interface separating net 9 ortho states under, adopts contact angle measurement (TBU90E, German DATAPHYSICS company) to measure micro-/ nano interface separating net 9 and the oily contact angle gone back ortho states under.
Embodiment 10 tests
As working electrode, platinized platinum is as auxiliary electrode with the micro-/ nano interface separating net 10 that makes in the foregoing description 10, and saturated calomel electrode immerses the LiClO of 0.1M as reference electrode
4In the solution, control current potential 0.35V, reaction time 45s obtains the micro-/ nano interface separating net 10 under the oxidation state, adopts contact angle measurement (TBU90E, German DATAPHYSICS company) to measure the contact angle of micro-/ nano interface separating net 10 and oil under the oxidation state;
In addition, control current potential-0.65V, reaction time 45s obtains going back the micro-/ nano interface separating net 10 ortho states under, adopts contact angle measurement (TBU90E, German DATAPHYSICS company) to measure micro-/ nano interface separating net 10 and the oily contact angle gone back ortho states under.
Embodiment 11 tests
As working electrode, platinized platinum is as auxiliary electrode with the micro-/ nano interface separating net 11 that makes in the foregoing description 11, and saturated calomel electrode immerses the LiClO of 0.1M as reference electrode
4In the solution, control current potential 0.3V, reaction time 45s obtains the micro-/ nano interface separating net 11 under the oxidation state, adopts contact angle measurement (TBU90E, German DATAPHYSICS company) to measure the contact angle of micro-/ nano interface separating net 11 and oil under the oxidation state;
In addition, control current potential-0.75V, reaction time 45s obtains going back the micro-/ nano interface separating net 11 ortho states under, adopts contact angle measurement (TBU90E, German DATAPHYSICS company) to measure micro-/ nano interface separating net 11 and the oily contact angle gone back ortho states under.
Embodiment 12 tests
As working electrode, platinized platinum is as auxiliary electrode with the micro-/ nano interface separating net 12 that makes in the foregoing description 12, and saturated calomel electrode immerses the LiClO of 0.1M as reference electrode
4In the solution, control current potential 0.3V, reaction time 45s obtains the micro-/ nano interface separating net 12 under the oxidation state, adopts contact angle measurement (TBU90E, German DATAPHYSICS company) to measure the contact angle of micro-/ nano interface separating net 12 and oil under the oxidation state;
In addition, control current potential-0.7V, reaction time 45s obtains going back the micro-/ nano interface separating net 12 ortho states under, adopts contact angle measurement (TBU90E, German DATAPHYSICS company) to measure micro-/ nano interface separating net 12 and the oily contact angle gone back ortho states under.
Embodiment 13 tests
As working electrode, platinized platinum is as auxiliary electrode with the micro-/ nano interface separating net 13 that makes in the foregoing description 13, and saturated calomel electrode immerses the LiClO of 0.1M as reference electrode
4In the solution, control current potential 0.25V, reaction time 45s obtains the micro-/ nano interface separating net 13 under the oxidation state, adopts contact angle measurement (TBU90E, German DATAPHYSICS company) to measure the contact angle of micro-/ nano interface separating net 13 and oil under the oxidation state;
In addition, control current potential-0.5V, reaction time 45s obtains going back the micro-/ nano interface separating net 13 ortho states under, adopts contact angle measurement (TBU90E, German DATAPHYSICS company) to measure micro-/ nano interface separating net 13 and the oily contact angle gone back ortho states under.
Table 1: embodiment of the invention 1-12 prepares constituent content and conditional parameter in the process
Table 2: embodiment of the invention 1-12 contact angle test
Table 1 shows embodiment of the invention micro-/ nano interface separating net 1-13 and prepares constituent content and conditional parameter in the process, and table 2 shows micro-/ nano interface separating net 1-13 of the present invention respectively in oxidation state and go back the contact angle test result under the ortho states.Find out from table 1 and table 2; The micro-/ nano interface separating net of embodiment of the invention preparation is 128.3 °-154.3 ° at the micro-/ nano interface separating net of the oxidation state that different oxidizing potentials (0.25V to 0.5V) form down with oily contact angle, shows that micro-/ nano interface separating net of the present invention has ultra oleophobic property under water under oxidation state; With micro-/ nano interface separating net of the present invention different reduction potentials (0.8V to-0.5V) under; The micro-/ nano interface separating net of ortho states is gone back in formation; When contacting with oil; Oil droplet all leaks down from the micro-/ nano interface separating net, shows that micro-/ nano interface separating net of the present invention has ultra lipophile under water going back under the ortho states.
The above is merely preferred embodiment of the present invention, is not to be used to limit protection scope of the present invention, and all equivalent variations of being done according to the present invention and modification, all within the scope of the present invention.
Claims (14)
1. micro-/ nano interface separating net; It is characterized in that; Said micro-/ nano interface separating net is made up of the conductive polymer coating of metallic fiber mesh grid and metallic fiber mesh grid surface coverage, and said conductive polymer coating is made up of the doping attitude conducting polymer with redox reversible property.
2. micro-/ nano interface separating net as claimed in claim 1; It is characterized in that; Said doping attitude conducting polymer is through immersing the metallic fiber mesh grid in the electrolyte as working electrode; Control constant potential or constant current obtain, and said electrolyte is made up of the conducting polymer monomer of 0.01-1 weight portion, the adulterant of 0.02-2 weight portion and the distilled water of 10 weight portions.
3. micro-/ nano interface separating net as claimed in claim 1 is characterized in that, said metallic fiber mesh grid is the 40-300 order, and said metallic fiber mesh grid is stainless steel, copper, iron, aluminium or titanium net.
4. micro-/ nano interface separating net as claimed in claim 2 is characterized in that, said conducting polymer is the derivative of polypyrrole, polythiophene, polyaniline, polyparaphenylene or these polymer;
Said conducting polymer monomer is the derivative of pyrroles, thiophene, aniline, biphenyl or these monomers;
Said adulterant is anionic surfactant or the long chain organic acid with emulsifying property.
5. micro-/ nano interface separating net as claimed in claim 2 is characterized in that, said conducting polymer obtains through control constant potential 0.001-1.6V or control constant current 0.02-200mA.
6. micro-/ nano interface separating net as claimed in claim 1 is characterized in that, the thickness of said conductive polymer coating is 2-30 μ m.
7. micro-/ nano interface separating net as claimed in claim 1 is characterized in that, the fibre diameter of said micro-/ nano interface separating net is 45-150 μ m.
8. the preparation method of a micro-/ nano interface separating net is characterized in that, said preparation method may further comprise the steps:
Immersion contains in the electrolyte of conducting polymer monomer and adulterant as working electrode with the metallic fiber mesh grid; Pass through electrochemical reaction; Obtain being covered in the conductive polymer coating on metallic fiber mesh grid surface, said conductive polymer coating is made up of the doping attitude conducting polymer with redox reversible property.
9. preparation method as claimed in claim 8; It is characterized in that; Said doping attitude conducting polymer obtains through control constant potential or constant current, and said electrolyte is made up of the conducting polymer monomer of 0.01-1 weight portion, the adulterant of 0.02-2 weight portion and the distilled water of 10 weight portions.
10. preparation method as claimed in claim 8 is characterized in that, said metallic fiber mesh grid is the 40-300 order, and said metallic fiber mesh grid is stainless steel, copper, iron, aluminium or titanium net.
11. preparation method as claimed in claim 8 is characterized in that, said conducting polymer is the derivative of polypyrrole, polythiophene, polyaniline, polyparaphenylene or these polymer;
Said conducting polymer monomer is the derivative of pyrroles, thiophene, aniline, biphenyl or these monomers;
Said adulterant is anionic surfactant or the long chain organic acid with emulsifying property.
12. preparation method as claimed in claim 9 is characterized in that, control constant potential 0.001-1.6V or control constant current 0.02-200mA among the said preparation method.
13. preparation method as claimed in claim 12 is characterized in that, control constant potential 10-120min or control constant current 10-120min among the said preparation method.
14. the purposes like each described micro-/ nano interface separating net among the claim 1-7 is characterized in that, said micro-/ nano interface separating net is used for water-oil separating.
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| CN102728104A (en) * | 2012-07-12 | 2012-10-17 | 北京航空航天大学 | Corrosion-resistant oil-water separation mesh membrane as well as preparation method and applications thereof |
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| CN103952853B (en) * | 2014-05-19 | 2015-08-26 | 华东理工大学 | A kind of X-type fibrage method being applicable to water-oil separating |
| CN104906827A (en) * | 2015-05-15 | 2015-09-16 | 清华大学 | Solution response oil and water separation net membrane based on electrostatic self-assembly, preparation method and applications |
| CN105582693B (en) * | 2015-12-22 | 2018-09-11 | 北京航空航天大学 | A kind of T-type oily water separating equipment integrating two kinds of special wellability materials |
| CN105582693A (en) * | 2015-12-22 | 2016-05-18 | 北京航空航天大学 | T-type oil-water separation equipment integrating two special wettable materials |
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| CN111266018B (en) * | 2020-02-12 | 2021-05-11 | 中国科学院生态环境研究中心 | Polymer film with adjustable wettability as well as preparation method and application thereof |
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Application publication date: 20120418 |