CN113082853A - Three-dimensional Janus stainless steel mesh capable of separating emulsified oil and water and preparation method thereof - Google Patents
Three-dimensional Janus stainless steel mesh capable of separating emulsified oil and water and preparation method thereof Download PDFInfo
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- CN113082853A CN113082853A CN202110352661.0A CN202110352661A CN113082853A CN 113082853 A CN113082853 A CN 113082853A CN 202110352661 A CN202110352661 A CN 202110352661A CN 113082853 A CN113082853 A CN 113082853A
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- 229910001220 stainless steel Inorganic materials 0.000 title claims abstract description 242
- 239000010935 stainless steel Substances 0.000 title claims abstract description 241
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 163
- 238000002360 preparation method Methods 0.000 title abstract description 36
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 claims abstract description 52
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 42
- 229920002873 Polyethylenimine Polymers 0.000 claims abstract description 27
- 229960003638 dopamine Drugs 0.000 claims abstract description 26
- 230000004048 modification Effects 0.000 claims abstract description 24
- 238000012986 modification Methods 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 8
- 230000003075 superhydrophobic effect Effects 0.000 claims abstract description 3
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims description 62
- 239000000243 solution Substances 0.000 claims description 54
- 239000008367 deionised water Substances 0.000 claims description 37
- 229910021641 deionized water Inorganic materials 0.000 claims description 37
- 238000001035 drying Methods 0.000 claims description 29
- 238000009210 therapy by ultrasound Methods 0.000 claims description 27
- 238000004140 cleaning Methods 0.000 claims description 23
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 20
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 20
- 239000002243 precursor Substances 0.000 claims description 20
- 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 claims description 18
- CTENFNNZBMHDDG-UHFFFAOYSA-N Dopamine hydrochloride Chemical compound Cl.NCCC1=CC=C(O)C(O)=C1 CTENFNNZBMHDDG-UHFFFAOYSA-N 0.000 claims description 18
- 229960001149 dopamine hydrochloride Drugs 0.000 claims description 18
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 15
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 14
- 239000007864 aqueous solution Substances 0.000 claims description 14
- 230000002209 hydrophobic effect Effects 0.000 claims description 14
- -1 perfluorosiloxane Chemical class 0.000 claims description 13
- 230000005661 hydrophobic surface Effects 0.000 claims description 10
- 230000005501 phase interface Effects 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 7
- NYIKUOULKCEZDO-UHFFFAOYSA-N triethoxy(3,3,4,4,5,5,6,6,6-nonafluorohexyl)silane Chemical group CCO[Si](OCC)(OCC)CCC(F)(F)C(F)(F)C(F)(F)C(F)(F)F NYIKUOULKCEZDO-UHFFFAOYSA-N 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 230000005660 hydrophilic surface Effects 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- MLXDKRSDUJLNAB-UHFFFAOYSA-N triethoxy(3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-heptadecafluorodecyl)silane Chemical compound CCO[Si](OCC)(OCC)CCC(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F MLXDKRSDUJLNAB-UHFFFAOYSA-N 0.000 claims description 2
- 238000000926 separation method Methods 0.000 abstract description 91
- 230000004907 flux Effects 0.000 abstract description 30
- 239000000839 emulsion Substances 0.000 abstract description 19
- 239000002184 metal Substances 0.000 abstract description 8
- 229910052751 metal Inorganic materials 0.000 abstract description 8
- 239000003921 oil Substances 0.000 description 49
- 235000019198 oils Nutrition 0.000 description 44
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 20
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 18
- 229910052802 copper Inorganic materials 0.000 description 16
- 239000010949 copper Substances 0.000 description 16
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 14
- 239000012528 membrane Substances 0.000 description 10
- 235000019441 ethanol Nutrition 0.000 description 9
- 239000000377 silicon dioxide Substances 0.000 description 9
- 235000012239 silicon dioxide Nutrition 0.000 description 9
- 239000011248 coating agent Substances 0.000 description 7
- 238000000576 coating method Methods 0.000 description 7
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 238000009736 wetting Methods 0.000 description 5
- 230000009471 action Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000005265 energy consumption Methods 0.000 description 4
- 235000019476 oil-water mixture Nutrition 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 239000002351 wastewater Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 239000000295 fuel oil Substances 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 238000012216 screening Methods 0.000 description 3
- ABTOQLMXBSRXSM-UHFFFAOYSA-N silicon tetrafluoride Chemical compound F[Si](F)(F)F ABTOQLMXBSRXSM-UHFFFAOYSA-N 0.000 description 3
- 239000007762 w/o emulsion Substances 0.000 description 3
- WSLDOOZREJYCGB-UHFFFAOYSA-N 1,2-Dichloroethane Chemical compound ClCCCl WSLDOOZREJYCGB-UHFFFAOYSA-N 0.000 description 2
- JJLJMEJHUUYSSY-UHFFFAOYSA-L Copper hydroxide Chemical compound [OH-].[OH-].[Cu+2] JJLJMEJHUUYSSY-UHFFFAOYSA-L 0.000 description 2
- 239000005750 Copper hydroxide Substances 0.000 description 2
- NHTMVDHEPJAVLT-UHFFFAOYSA-N Isooctane Chemical compound CC(C)CC(C)(C)C NHTMVDHEPJAVLT-UHFFFAOYSA-N 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 238000006482 condensation reaction Methods 0.000 description 2
- 229910001956 copper hydroxide Inorganic materials 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- JVSWJIKNEAIKJW-UHFFFAOYSA-N dimethyl-hexane Natural products CCCCCC(C)C JVSWJIKNEAIKJW-UHFFFAOYSA-N 0.000 description 2
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 230000009191 jumping Effects 0.000 description 2
- 239000002073 nanorod Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 1
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 241000282414 Homo sapiens Species 0.000 description 1
- 238000006845 Michael addition reaction Methods 0.000 description 1
- 239000002262 Schiff base Substances 0.000 description 1
- 150000004753 Schiff bases Chemical class 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- XQSFXFQDJCDXDT-UHFFFAOYSA-N hydroxysilicon Chemical compound [Si]O XQSFXFQDJCDXDT-UHFFFAOYSA-N 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- MCPLVIGCWWTHFH-UHFFFAOYSA-L methyl blue Chemical compound [Na+].[Na+].C1=CC(S(=O)(=O)[O-])=CC=C1NC1=CC=C(C(=C2C=CC(C=C2)=[NH+]C=2C=CC(=CC=2)S([O-])(=O)=O)C=2C=CC(NC=3C=CC(=CC=3)S([O-])(=O)=O)=CC=2)C=C1 MCPLVIGCWWTHFH-UHFFFAOYSA-L 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000007764 o/w emulsion Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229920005597 polymer membrane Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000009877 rendering Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 239000002569 water oil cream Substances 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D39/00—Filtering material for liquid or gaseous fluids
- B01D39/10—Filter screens essentially made of metal
- B01D39/12—Filter screens essentially made of metal of wire gauze; of knitted wire; of expanded metal
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/04—Additives and treatments of the filtering material
- B01D2239/0414—Surface modifiers, e.g. comprising ion exchange groups
- B01D2239/0421—Rendering the filter material hydrophilic
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/04—Additives and treatments of the filtering material
- B01D2239/0464—Impregnants
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/10—Filtering material manufacturing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/12—Special parameters characterising the filtering material
- B01D2239/1275—Stiffness
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/12—Special parameters characterising the filtering material
- B01D2239/1291—Other parameters
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Textile Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Organic Chemistry (AREA)
- Filtering Materials (AREA)
Abstract
The invention discloses a three-dimensional Janus stainless steel mesh capable of separating emulsified oil and water and a preparation method thereof. The Janus stainless steel mesh is formed by combining a super-hydrophilic stainless steel mesh obtained by treating a stainless steel mesh with the mesh number of 600-800 with a dopamine/polyethyleneimine ethanol solution and a two-dimensional Janus stainless steel mesh; the two-dimensional Janus stainless steel mesh is obtained by performing super-hydrophilic and super-hydrophobic modification treatment on a stainless steel mesh with the mesh number of 600-800, wherein one surface is a super-hydrophilic surface, and the other surface is a high-hydrophobic surface; and (3) superposing 15-20 super-hydrophilic stainless steel meshes and placing the superposed super-hydrophilic surfaces on the two-dimensional Janus stainless steel mesh. The separation efficiency of the Janus stainless steel mesh on emulsified oil-water is over 99 percent, and simultaneously, the separation flux is ensured to be 4000 L.m‑2·h‑1The method has the function of performing high-efficiency and high-flux oil-water separation on oil-in-water, water-in-oil and other emulsionsAnd the technical difficulty that the Janus metal filter screen is difficult to separate the emulsion is solved.
Description
Technical Field
The invention relates to the field of oily wastewater treatment, in particular to a three-dimensional Janus stainless steel mesh for efficiently separating layered oil water and emulsified oil water at high flux, and a preparation method and application thereof.
Background
With the continuous development of industrial science and technology, the discharge of oily wastewater is also increased, which brings great pressure to the environment and threatens the survival of human beings, therefore, how to treat oily wastewater efficiently is urgent. The traditional oil-water separation means mainly comprises: centrifugal method, gravity separation method, etc., but these traditional separation methods have the disadvantages of high energy consumption, complex operation, high cost, etc. The super-wetting surface separation membrane is a hot material for oil-water separation by virtue of the advantages of high efficiency, low cost, low energy consumption, no toxicity and the like. However, the super-wetting surface separation membrane can only remove water or oil, and has a single function and limited oil-water separation treatment efficiency. Therefore, the development of a multifunctional separation material capable of removing water and oil is a research focus of people.
The Janus separation membrane refers to the fact that two surfaces of the membrane have opposite properties, including opposite wetting performance, opposite charges and the like, wherein the Janus separation membrane with the opposite wetting performance has a selective oil-water separation effect, oil and water can be removed, the processing capacity of an oil-water separation process is greatly improved, and therefore the separation membrane has a certain application prospect in the oil-water separation field. The Janus separation membrane using the metal filter screen as the base material can better adapt to the actual industrial environment by virtue of the advantages of low price, easiness in processing, high temperature resistance, good mechanical property and the like of the metal filter screen.
Chinese patent application CN110038569A discloses Janus Cu (OH)2@Cu2O-copper net and its preparation method and application. The preparation method comprisesPutting the pre-cleaned copper net into sodium hydroxide aqueous solution for anodic oxidation to obtain the copper net full of needle-shaped copper hydroxide nano rods, then immersing the copper net into normal hexane solution containing silane coupling agent, standing, washing, drying, heat treating, irradiating by ultraviolet light, and then carrying out vapor phase reduction on hydrazine hydrate aqueous solution to obtain Janus Cu (OH)2@Cu2O-copper mesh, which can be applied to the separation of immiscible oil-water mixtures and can degrade methyl blue in the aqueous phase under visible light. However, the application is only for immiscible oil-water mixtures, the particle size of emulsified oil-water is usually in the range of 10nm-100 mu m, the pore size of the copper mesh is generally far larger than that of emulsion, the size sieving effect does not exist, the copper mesh is thin, and the separation channel is extremely short, so that the copper mesh has no demulsification capability, cannot separate the emulsified oil-water, and has complex preparation process, large time consumption and large energy consumption.
Chinese invention patent application CN110755887A discloses a super-hydrophilic-super-hydrophobic Janus copper mesh and a preparation method and application thereof. The preparation method comprises the steps of firstly etching a copper net by using a sodium persulfate/sodium hydroxide solution, growing needle-shaped copper hydroxide nanorods on the surface of the copper net, performing hydrophobic modification by using gas molecules of a dimethyl siloxane mixed solution, and adding water to control the wetting distance of hydrophobic molecules so as to obtain the super-hydrophilic-super-hydrophobic Janus copper net. Although the technology successfully prepares the Janus copper mesh with super-wettability, the application of the technology is still limited to separating immiscible oil-water mixtures, and similarly, the aperture of the Janus copper mesh of the technology is far larger than the particle size of the emulsion, so that the Janus copper mesh cannot play a role in size screening of the emulsion, and the Janus copper mesh is a straight-through hole and has no demulsification capability, so that emulsified oil-water cannot be separated, and the actual oily wastewater also comprises emulsified oil-water, so that the technology cannot be well adapted to the actual oil-water separation environment.
Disclosure of Invention
Aiming at the defect that the Janus metal filter screen in the prior art cannot separate emulsified oil and water, the invention provides the preparation method which has the advantages of mild reaction conditions, readily available reaction equipment, low energy consumption in the preparation process, high bonding strength of the coating and the substrate, and two performances of water removal and oil removal, and can realize the separation of emulsified oil and waterThe three-dimensional Janus stainless steel mesh for realizing the efficient separation of emulsions such as light oil, heavy oil, even oil-in-water and water-in-oil and the like and the preparation method thereof, the separation efficiency of the Janus stainless steel mesh on the emulsified oil and water exceeds 99 percent, and simultaneously, the separation flux is ensured to be 4000 L.m-2·h-1The above.
According to the invention, the stainless steel mesh with larger pore diameter is used as a substrate, and the three-dimensional Janus stainless steel mesh is assembled by superposing a plurality of super-hydrophilic stainless steel meshes on the super-hydrophilic side of the Janus stainless steel mesh. Super hydrophilic stainless steel mesh of stack is equivalent to the super hydrophilic side's of enlarging two-dimentional Janus stainless steel mesh thickness, has constructed random and have certain length's capillary passage, though do not possess size screening effect, but oil drop or water drop when emulsified oil water intercept water drop or oil drop through can receiving strong capillary action, have obtained the breakdown of emulsion ability to successfully separate emulsified oil water, solved the shortcoming that prior art Janus metal filter screen can't separate emulsified oil water.
The purpose of the invention is realized by the following technical scheme:
a three-dimensional Janus stainless steel mesh capable of separating emulsified oil and water is formed by combining a super-hydrophilic stainless steel mesh and a two-dimensional Janus stainless steel mesh, wherein the mesh number of the stainless steel mesh is 600-800, and the super-hydrophilic stainless steel mesh is obtained by processing the stainless steel mesh with a dopamine/polyethyleneimine ethanol solution; the two-dimensional Janus stainless steel mesh is obtained by performing super-hydrophilic and super-hydrophobic modification treatment on a stainless steel mesh with the mesh number of 600-800, wherein one surface is a super-hydrophilic surface, and the other surface is a high-hydrophobic surface; and (3) superposing 15-20 super-hydrophilic stainless steel meshes and placing the superposed super-hydrophilic surfaces on the two-dimensional Janus stainless steel mesh.
To further achieve the object of the present invention, preferably, the super-hydrophilic stainless steel net is obtained by the following method: cleaning a stainless steel net, drying, soaking in a precursor solution, cleaning with deionized water, and drying; the precursor solution is prepared by adding 1-4 parts of dopamine hydrochloride, 1-4 parts of polyethyleneimine, 2-6 parts of Tris-HCl and 40-60 parts of water, 10-30 parts of ammonia water, 300-600 parts of ethanol, carrying out ultrasonic treatment until the materials are fully dissolved, and then adding 3-6 parts of ethyl orthosilicate in parts by mass.
Preferably, the ultrasonic treatment time is 30-60 min, and the stainless steel net cleaning is to clean the stainless steel net with acetone, ethanol and deionized water respectively.
Preferably, the two-dimensional Janus stainless steel mesh is obtained by placing the weak hydrophobic side of the high-hydrophobic/weak-hydrophobic stainless steel mesh on the liquid surface of dopamine aqueous solution, performing ultrasonic treatment, performing single-side super-hydrophilic modification, and then washing and drying with deionized water; the high-hydrophobicity/weak-hydrophobicity stainless steel mesh is obtained by placing a super-hydrophilic stainless steel mesh on a phase interface of a carbon tetrachloride solution of perfluorosiloxane and water for modification, wherein one side of the high-hydrophobicity/weak-hydrophobicity stainless steel mesh close to the carbon tetrachloride solution has high hydrophobicity, and one side of the high-hydrophobicity/weak-hydrophobicity stainless steel mesh close to the water has weak hydrophobicity.
Preferably, the perfluorosiloxane carbon tetrachloride solution consists of 50-150 parts of carbon tetrachloride and 1-4 parts of perfluorosiloxane by mass, the heating condition is water bath, the temperature is 35-45 ℃, and the reaction time is 60-90 min.
Preferably, the perfluorosiloxane is 1H,1H,2H, 2H-perfluorohexyltriethoxysilane, 1H,2H, 2H-perfluoroheptyltriethoxysilane or 1H,1H,2H, 2H-perfluorodecyltriethoxysilane.
Preferably, the stainless steel net is a twill net; the contact angle of the highly hydrophobic surface in water in air is larger than 130 degrees.
Preferably, the contact angle of the super hydrophilic surface with water in the air is equal to 0 degrees.
The preparation method of the three-dimensional Janus stainless steel mesh capable of separating emulsified oil and water comprises the following steps:
1) cleaning the stainless steel net, and drying for later use;
2) preparing a precursor solution: adding 1-4 parts of dopamine hydrochloride, 1-4 parts of polyethyleneimine, 2-6 parts of Tris-HCl and 40-60 parts of water 10-30 parts of ammonia water into 300-600 parts of ethanol by mass, and carrying out ultrasonic treatment until the dopamine hydrochloride, the polyethyleneimine, the Tris-HCl and the ammonia water are fully dissolved; adding 3-6 parts of tetraethoxysilane into the obtained solution to obtain a precursor solution;
3) putting the stainless steel mesh obtained in the step 1) into the precursor solution obtained in the step 2), shaking by using a shaking table, washing by using deionized water for a plurality of times, and drying to obtain a super-hydrophilic stainless steel mesh;
4) placing the super-hydrophilic stainless steel mesh obtained in the step 3) on a phase interface of a carbon tetrachloride solution of perfluorosiloxane and water for single-side modification to obtain a high-hydrophobicity/weak-hydrophobicity stainless steel mesh, wherein one side of the high-hydrophobicity/weak-hydrophobicity stainless steel mesh close to the carbon tetrachloride solution has high hydrophobicity, and one side of the high-hydrophobicity/weak-hydrophobicity stainless steel mesh close to the water has weak hydrophobicity;
5) preparing a dopamine solution: placing the weak hydrophobic side of the high-hydrophobic/weak-hydrophobic stainless steel mesh obtained in the step 4) on the liquid surface of the dopamine aqueous solution, performing ultrasonic treatment, performing single-side super-hydrophilic modification, washing with deionized water, and drying to obtain a two-dimensional Janus stainless steel mesh; the dopamine aqueous solution is obtained by adding 1-4 parts of dopamine hydrochloride, 1-4 parts of polyethyleneimine, 2-6 parts of Tris-HCl and 10-30 parts of ammonia water into 300-600 parts of deionized water in parts by mass, mixing and then carrying out ultrasonic treatment;
6) and (3) superposing 15-20 pieces of the super-hydrophilic stainless steel mesh obtained in the step 3) on the super-hydrophilic side of the two-dimensional Janus stainless steel mesh obtained in the step 5), and combining to obtain the three-dimensional Janus stainless steel mesh capable of separating the emulsified oil and the water.
Preferably, the rotating speed of the shaking table in the step 3) is 90-120 rpm, and the shaking time is 6-12 h; the single-side super-hydrophilic modification time in the step 5) is 10-60 min.
The formation of the super-hydrophilic coating is that under the action of ammonia water, ethyl orthosilicate is hydrolyzed and condensed to generate silicon dioxide containing hydroxyl groups, and the silicon dioxide containing the hydroxyl groups are stacked to form a micron structure; the PDA and PEI are subjected to Schiff base reaction and Michael addition reaction under the action of oxygen and ammonia water to generate a coating full of hydroxyl groups, the coating and hydroxyl silicon dioxide particles are subjected to hydrolytic condensation reaction and are adhered to the substrate, and the hydroxyl-rich PDA/PEI coating and the micro-nano-grade silicon dioxide stainless steel mesh are obtained after drying.
The perfluorosiloxane and the hydroxyl of the silicon dioxide and PDA/PEI coating are subjected to hydrolysis condensation reaction for hydrophobic modification, and the reaction principle is as follows: under the action of a solvent, perfluorosiloxane is rapidly hydrolyzed to form perfluorosilane with hydroxyl, the perfluorosilane is condensed with hydroxyl on the coating of silicon dioxide and PDA/PEI, and a long fluorine-containing chain is connected to the surface of the stainless steel net, so that the surface energy of the surface of the stainless steel net is reduced, and the surface obtains high hydrophobicity. The PDA of the present invention reacts with PEI and, by virtue of its strong adhesion, covers a weakly hydrophobic surface, rendering it superhydrophilic.
Compared with the prior art, the invention has the following advantages and technical effects:
1. according to the invention, by superposing the super-hydrophilic stainless steel mesh, the thickness of the super-hydrophilic layer of the Janus stainless steel mesh is increased, and meanwhile, a plurality of irregular capillary channels with wettability are formed, so that oil drops or water drops can be subjected to obvious capillary force and adhesive force generated by the capillary channels and the wettability after entering the capillary channels, so that the oil drops are continuously intercepted and gradually gathered, demulsification is finally completed, oil and water are layered, and the emulsified oil and water are successfully separated. The three-dimensional Janus stainless steel mesh obtained by the invention has the one-way conductivity of water, has the function of selectively separating oil and water, realizes high-efficiency separation of oil-water mixture of light oil and heavy oil, and simultaneously realizes high-flux high-efficiency separation of emulsified oil-water. The emulsion separation efficiency is higher than 99%, and the flux for separating oil-in-water and water-in-oil exceeds 4241.92 L.m-2·h-1，7072.11L·m-2·h-1The defect that the Janus metal filter screen cannot separate emulsified oil and water and the defect that the Janus polymer membrane separation flux is too low are solved.
2. The three-dimensional Janus stainless steel mesh obtained by the invention has excellent chemical stability and mechanical properties, and can still keep stable under extreme acid-base salt conditions and sand impact conditions.
3. According to the invention, the super-hydrophilic stainless steel mesh is prepared by directly covering the stainless steel mesh with dopamine/polyethyleneimine and silicon dioxide particles to construct active sites, the Janus stainless steel mesh is prepared by utilizing hydrophobic modification of a phase interface and dopamine deposition on a single surface, and the three-dimensional Janus stainless steel mesh is obtained by superposing and combining the super-hydrophilic stainless steel mesh and the Janus stainless steel mesh. The reactants and the substrate are firstly combined through the super-strong adhesion of PDA and then are mutually connected with the silicon dioxide through chemical bonds, so that the silicon dioxide/silicon.
4. The three-dimensional Janus stainless steel mesh prepared by the method is simple in process, mild in reaction condition and easy to operate.
Drawings
FIG. 1 is a Scanning Electron Microscope (SEM) image of a cleaned stainless steel net in preparation example 1;
FIG. 2 is a Scanning Electron Microscope (SEM) image of the super-hydrophilic stainless steel net prepared in preparation example 1;
FIG. 3 is a partial magnified Scanning Electron Microscope (SEM) image of the hydrophobic surface of the three-dimensional Janus stainless steel mesh prepared in preparation example 1;
FIG. 4 is a partial magnified Scanning Electron Microscope (SEM) image of the superhydrophilic surface of the three-dimensional Janus stainless steel mesh prepared in preparation example 1;
FIG. 5 is a photograph of a contact angle of a hydrophobic surface of a three-dimensional Janus stainless steel mesh prepared in preparation example 1 with deionized water;
FIG. 6 is a photograph of a contact angle of a superhydrophilic surface to deionized water of the three-dimensional Janus stainless steel mesh prepared in preparation example 1;
FIG. 7 is a photograph showing the contact angle of the super hydrophilic surface of the three-dimensional Janus stainless steel net prepared in preparation example 1 with isooctane under water;
FIG. 8 is a photograph showing the contact angle of the super hydrophilic surface of the three-dimensional Janus stainless steel net prepared in preparation example 1 with 1, 2-dichloroethane under water;
FIG. 9 is an energy dispersive X-ray spectroscopy of the hydrophobic surface of the three-dimensional Janus stainless steel mesh prepared in preparation example 1;
fig. 10 is an X-ray photoelectron spectrum of both faces of the three-dimensional Janus stainless steel mesh prepared in preparation example 1.
Detailed Description
For a better understanding of the present invention, the present invention will be further described with reference to the following examples and the accompanying drawings, but the scope of the present invention as claimed is not limited to the scope of the examples.
Preparation of example 1
1) Ultrasonically cleaning a stainless steel net (with size of 2.5cm × 2.5cm, 800 meshes) with acetone, ethanol and deionized water for 15min, and drying at 60 deg.C;
2) adding 0.2g of dopamine hydrochloride, 0.2g of polyethyleneimine, 0.6g of Tris-HCl, 10ml of deionized water and 5ml of ammonia water into 100ml of absolute ethyl alcohol, and dissolving by ultrasonic treatment for 30 min; adding 0.68ml of Tetraethoxysilane (TEOS) to obtain a precursor solution;
3) putting the stainless steel mesh obtained in the step 1) into the precursor solution, shaking for 6h by using a shaking table under the condition of 120rpm, cleaning by using deionized water, and drying to obtain a super-hydrophilic stainless steel mesh;
4) and (3) placing the super-hydrophilic stainless steel mesh obtained in the step (3) on a phase interface of a carbon tetrachloride/perfluorosiloxane solution and water, and reacting for 60min under a water bath condition of 35 ℃, wherein the carbon tetrachloride/perfluorosiloxane solution consists of 20g of carbon tetrachloride and 0.04g of 1H,1H,2H, 2H-perfluorohexyltriethoxysilane, so that the high-hydrophobic/weak-hydrophobic stainless steel mesh is obtained, wherein one side close to the carbon tetrachloride/perfluorosiloxane solution is a high-hydrophobic surface, and one side close to the water is a weak-hydrophobic surface.
5) Preparing a dopamine solution: adding 0.2g of dopamine hydrochloride, 0.2g of polyethyleneimine, 0.6g of Tris-HCl and 5ml of ammonia water into 100ml of deionized water, mixing, and performing ultrasonic treatment for 30min for later use; and (3) placing the weak hydrophobic side of the stainless steel mesh obtained in the step (4) on the liquid surface of the dopamine aqueous solution for ultrasonic treatment for 60min, carrying out super-hydrophilic modification, cleaning and drying by using deionized water to obtain the two-dimensional high-hydrophobic/super-hydrophilic Janus stainless steel mesh, wherein the side close to the dopamine aqueous solution is a super-hydrophilic surface, and the side close to the air is a high-hydrophobic surface.
6) Respectively overlapping the super-hydrophilic stainless steel nets obtained in the step 3) on the super-hydrophilic surface of the two-dimensional Janus stainless steel net by using 0, 5, 10, 15, 20, 25 and 30 pieces of super-hydrophilic stainless steel nets to obtain six three-dimensional Janus stainless steel nets;
FIG. 1 is a Scanning Electron Microscope (SEM) image of a stainless steel net cleaned in step 1) of preparation example 1. As can be seen in fig. 1, the unreacted stainless steel mesh surface was smooth, free of particles and roughness.
Fig. 2 is a Scanning Electron Microscope (SEM) image of the superhydrophilic stainless steel mesh prepared in preparation example 1. As can be seen from FIG. 2, the super-hydrophilic stainless steel mesh obtained in this example has a plurality of spherical silica particles and layered dopamine deposited on the surface. Fig. 3 is a partially enlarged view of a Scanning Electron Microscope (SEM) image of the hydrophobic surface of the three-dimensional Janus stainless steel mesh prepared in preparation example 1, and fig. 3 shows that the branched perfluorosilane makes the connection between silica particles tighter, there is an agglomeration phenomenon, and the roughness is reduced. FIG. 4 is a partial enlarged view of a Scanning Electron Microscope (SEM) image of the super-hydrophilic surface of the three-dimensional Janus stainless steel mesh prepared in this example, which can be seen that a dopamine coating layer is covered on the surface; EDS analysis is carried out on the hydrophobic surface of the three-dimensional Janus stainless steel mesh in the example 1, EDS data can also indicate that the mesh contains F element, and the success of hydrophobic modification is verified; furthermore, XPS surface element analysis was performed on both sides of the three-dimensional Janus stainless steel net of example 1, and it can be known that the three-dimensional Janus stainless steel net can be prepared by preset steps by analyzing the difference of the relative contents of various elements on both sides, as shown in detail in fig. 9 and 10.
FIG. 5 is a photograph showing the contact angle of the hydrophobic surface of the three-dimensional Janus stainless steel net prepared in the preparation example 1 facing deionized water (surface tension 72.8mN/m), respectively, and it can be seen that the contact angle is 135 deg., which indicates that it has high hydrophobicity; FIG. 6 is a photograph showing the contact angle of the superhydrophilic surface of the three-dimensional Janus stainless steel mesh prepared in this example 1 to deionized water, where a water drop spreads rapidly when contacting the surface, the contact angle is 0 DEG, and the surface has superhydrophilic properties; fig. 7 is a photograph of a contact angle of the super-hydrophilic surface to light oil (isooctane) under water, the contact angle is 151 °, and fig. 8 is a photograph of a contact angle of the super-hydrophilic surface to heavy oil (1, 2-dichloroethane) under water, the contact angle is 152 °, which shows that the super-hydrophilic surface of the three-dimensional Janus stainless steel mesh prepared in preparation example 1 has the underwater super-oleophobic property.
Preparation of example 2
Ultrasonically cleaning a stainless steel mesh (with size of 2.5cm × 2.5cm, 600 meshes) with acetone, ethanol and deionized water for 15min, and drying at 60 deg.C; adding 0.2g of dopamine hydrochloride, 0.2g of polyethyleneimine, 0.6g of Tris-HCl, 10ml of ionized water and 5ml of ammonia water into 100ml of absolute ethyl alcohol, and dissolving by ultrasonic treatment for 30 min; adding 0.68ml of Tetraethoxysilane (TEOS) under the condition of stirring to obtain a precursor solution; putting the cleaned stainless steel mesh into the precursor solution, shaking for 6h at 120rpm by using a shaking table, cleaning by using deionized water, and drying to obtain a super-hydrophilic stainless steel mesh; placing the obtained super-hydrophilic stainless steel mesh on a phase interface of a carbon tetrachloride/perfluorosiloxane solution and water, and reacting for 60min under a water bath condition of 35 ℃, wherein the carbon tetrachloride solution consists of 20g of carbon tetrachloride and 0.04g of 1H,1H,2H, 2H-perfluorohexyltriethoxysilane to obtain a high-hydrophobic/weak-hydrophobic stainless steel mesh (one side close to the carbon tetrachloride/perfluorosiloxane is a high-hydrophobic surface, and one side close to the water is a weak-hydrophobic side); adding 0.2g of dopamine hydrochloride, 0.2g of polyethyleneimine, 0.6g of Tris-HCl and 5ml of ammonia water into 100ml of deionized water, mixing, and performing ultrasonic treatment for 30min for later use; placing the weak hydrophobic side of the obtained high-hydrophobic/weak-hydrophobic stainless steel mesh on the liquid surface of the dopamine aqueous solution for ultrasonic treatment for 60min, performing super-hydrophilic modification, and cleaning and drying the modified stainless steel mesh by using deionized water to obtain a two-dimensional Janus stainless steel mesh (one side close to the dopamine solution is a super-hydrophilic surface, and the other side close to the air is a high-hydrophobic surface); and respectively superposing 0, 10, 15, 20, 25 and 30 pieces of super-hydrophilic stainless steel nets on the super-hydrophilic surface of the two-dimensional Janus stainless steel net to obtain six three-dimensional Janus stainless steel nets.
Preparation example 3: comparative example 1
Ultrasonically cleaning a stainless steel mesh (with size of 2.5cm × 2.5cm, 200 meshes) with acetone, ethanol and deionized water for 15min, and drying at 60 deg.C; adding 0.2g of dopamine hydrochloride, 0.2g of polyethyleneimine, 0.6g of Tris-HCl, 10ml of ionized water and 5ml of ammonia water into 100ml of absolute ethyl alcohol, and dissolving by ultrasonic treatment for 30 min; adding 0.68ml of Tetraethoxysilane (TEOS) under the condition of stirring to obtain a precursor solution; putting the cleaned stainless steel mesh into the precursor solution, shaking for 6h at 120rpm by using a shaking table, cleaning by using deionized water, and drying to obtain a super-hydrophilic stainless steel mesh; placing the obtained super-hydrophilic stainless steel mesh on a phase interface of a carbon tetrachloride/perfluorosiloxane solution and water, and reacting for 60min under a water bath condition of 35 ℃, wherein the carbon tetrachloride solution consists of 20g of carbon tetrachloride and 0.04g of 1H,1H,2H, 2H-perfluorohexyltriethoxysilane to obtain a high-hydrophobic/weak-hydrophobic stainless steel mesh (one side close to the carbon tetrachloride/perfluorosiloxane is a high-hydrophobic surface, and one side close to the water is a weak-hydrophobic side); adding 0.2g of dopamine hydrochloride, 0.2g of polyethyleneimine, 0.6g of Tris-HCl and 5ml of ammonia water into 100ml of deionized water, mixing, and performing ultrasonic treatment for 30min for later use; placing the weak hydrophobic side of the obtained high-hydrophobic/weak-hydrophobic stainless steel mesh on the liquid surface of the dopamine aqueous solution for ultrasonic treatment for 60min, performing super-hydrophilic modification, and cleaning and drying the modified stainless steel mesh by using deionized water to obtain a two-dimensional Janus stainless steel mesh (one side close to the dopamine solution is a super-hydrophilic surface, and the other side close to the air is a high-hydrophobic surface); and respectively superposing 0, 10, 15, 20, 25 and 30 pieces of super-hydrophilic stainless steel nets on the super-hydrophilic surface of the two-dimensional Janus stainless steel net to obtain six three-dimensional Janus stainless steel nets.
Preparation example 4 (comparative example 2)
Ultrasonically cleaning a stainless steel net (with size of 2.5cm × 2.5cm, 400 meshes) with acetone, ethanol and deionized water for 15min, and drying at 60 deg.C; adding 0.2g of dopamine hydrochloride, 0.2g of polyethyleneimine, 0.6g of Tris-HCl, 10ml of ionized water and 5ml of ammonia water into 100ml of absolute ethyl alcohol, and dissolving by ultrasonic treatment for 30 min; adding 0.68ml of Tetraethoxysilane (TEOS) under the condition of stirring to obtain a precursor solution; putting the cleaned stainless steel mesh into the precursor solution, shaking for 6h at 120rpm by using a shaking table, cleaning by using deionized water, and drying to obtain a super-hydrophilic stainless steel mesh; placing the obtained super-hydrophilic stainless steel mesh on a phase interface of a carbon tetrachloride/perfluorosiloxane solution and water, and reacting for 60min under a water bath condition of 35 ℃, wherein the carbon tetrachloride solution consists of 20g of carbon tetrachloride and 0.04g of 1H,1H,2H, 2H-perfluorohexyltriethoxysilane to obtain a high-hydrophobic/weak-hydrophobic stainless steel mesh (one side close to the carbon tetrachloride/perfluorosiloxane is a high-hydrophobic surface, and one side close to the water is a weak-hydrophobic side); adding 0.2g of dopamine hydrochloride, 0.2g of polyethyleneimine, 0.6g of Tris-HCl and 5ml of ammonia water into 100ml of deionized water, mixing, and performing ultrasonic treatment for 30min for later use; placing the weak hydrophobic side of the obtained high-hydrophobic/weak-hydrophobic stainless steel mesh on the liquid surface of the dopamine aqueous solution for ultrasonic treatment for 60min, performing super-hydrophilic modification, and cleaning and drying the modified stainless steel mesh by using deionized water to obtain a two-dimensional Janus stainless steel mesh (one side close to the dopamine solution is a super-hydrophilic surface, and the other side close to the air is a high-hydrophobic surface); and respectively superposing 0, 10, 15, 20, 25 and 30 pieces of super-hydrophilic stainless steel nets on the super-hydrophilic surface of the two-dimensional Janus stainless steel net to obtain six three-dimensional Janus stainless steel nets.
Preparation of example 5 (comparative example 3)
Ultrasonically cleaning a stainless steel mesh (with size of 2.5cm × 2.5cm, 1000 meshes) with acetone, ethanol and deionized water for 15min, and drying at 60 deg.C; adding 0.2g of dopamine hydrochloride, 0.2g of polyethyleneimine, 0.6g of Tris-HCl, 10ml of ionized water and 5ml of ammonia water into 100ml of absolute ethyl alcohol, and dissolving by ultrasonic treatment for 30 min; adding 0.68ml of Tetraethoxysilane (TEOS) under the condition of stirring to obtain a precursor solution; putting the cleaned stainless steel mesh into the precursor solution, shaking for 6h at 120rpm by using a shaking table, cleaning by using deionized water, and drying to obtain a super-hydrophilic stainless steel mesh; placing the obtained super-hydrophilic stainless steel mesh on a phase interface of a carbon tetrachloride/perfluorosiloxane solution and water, and reacting for 60min under a water bath condition of 35 ℃, wherein the carbon tetrachloride solution consists of 20g of carbon tetrachloride and 0.04g of 1H,1H,2H, 2H-perfluorohexyltriethoxysilane to obtain a high-hydrophobic/weak-hydrophobic stainless steel mesh (one side close to the carbon tetrachloride/perfluorosiloxane is a high-hydrophobic surface, and one side close to the water is a weak-hydrophobic side); adding 0.2g of dopamine hydrochloride, 0.2g of polyethyleneimine, 0.6g of Tris-HCl and 5ml of ammonia water into 100ml of deionized water, mixing, and performing ultrasonic treatment for 30min for later use; placing the weak hydrophobic side of the obtained high-hydrophobic/weak-hydrophobic stainless steel mesh on the liquid surface of the dopamine aqueous solution for ultrasonic treatment for 60min, performing super-hydrophilic modification, and cleaning and drying the modified stainless steel mesh by using deionized water to obtain a two-dimensional Janus stainless steel mesh (one side close to the dopamine solution is a super-hydrophilic surface, and the other side close to the air is a high-hydrophobic surface); and respectively superposing 0, 10, 15, 20, 25 and 30 pieces of super-hydrophilic stainless steel nets on the super-hydrophilic surface of the two-dimensional Janus stainless steel net to obtain six three-dimensional Janus stainless steel nets.
Application examples
Although the Janus metal filter screen can be prepared in the prior art, but the emulsified oil and water cannot be separated, the invention discovers that the combination of the super-hydrophilic stainless steel mesh and the two-dimensional Janus stainless steel mesh can realize the separation of the emulsified oil and water by the Janus metal filter screen, and particularly, the invention discovers that when the number of the stainless steel meshes is 600-800 and the number of the super-hydrophilic stainless steel meshes is 15-20, the efficient separation and the high separation flux of the emulsified oil and water can be realized, the separation efficiency of the oil-water emulsion exceeds 99%, wherein the separation efficiency of the water-in-oil emulsion exceeds 99.36%, and the separation efficiency of the water-in-oil emulsion exceeds 99.53%; the separation flux is all 4000L·m-2·h-1Above, wherein the oil-in-water emulsion separation flux exceeds 4241.92 L.m-2·h-1The separation flux of the water-in-oil emulsion exceeds 7072.11 L.m-2·h-1(ii) a And the separation efficiency and the separation flux of the emulsified oil and water are increased in a jumping way compared with the number of the close stainless steel meshes and the number of the close super-hydrophilic stainless steel meshes, so that the problem of contradiction that the separation efficiency and the separation flux are difficult to consider is effectively solved.
Because industrial oily wastewater containing toluene is common, toluene is taken as an oil phase as an example when the emulsified oil-water separation capacity of the three-dimensional Janus layered membrane is tested, and for emulsified oil-water of other oil phases, the separation efficiency is slightly different according to different properties of the oil phase, but the separation efficiency can still be maintained to be more than 99.5%, and the separation flux is higher than 4000 L.m-2·h-1. In the existing technology of adopting membrane separation emulsified oil water, the emulsified oil water is mostly separated by utilizing size screening to break emulsion, which means that the aperture of the membrane is small enough, so that the flux is correspondingly reduced, and the separation efficiency and the separation flux are difficult to be considered. As for the separation flux for separating the emulsified oil and water, the flux of most materials is very low, several hundreds or more than one thousand, and basically less than two thousand, and the separation flux is higher only under the pressurized condition, but the pressurization operation complicates the practical application thereof.
To verify the findings of the present invention, the present invention was subjected to the following specific tests:
and (3) testing of emulsified oil-water separation: the application test of the emulsified oil-water separation capability was performed on six different three-dimensional Janus stainless steel meshes obtained in different preparation examples, and the application test of the emulsified oil-water separation capability was performed on the multifunctional three-dimensional Janus stainless steel meshes with different mesh numbers and different numbers of super-hydrophilic sheets obtained in preparation examples 1 to 5. The oil-in-water emulsions (O/W) in the tests are exemplified by toluene-in-water emulsions and the water-in-oil emulsions (W/O) by water-in-toluene emulsions.
The specific test method is as follows: when the toluene emulsion in the water pocket is separated, the hydrophobic surface of the three-dimensional Janus stainless steel net is upward, the super-hydrophilic surface of the three-dimensional Janus stainless steel net is firstly wetted by water, the three-dimensional Janus stainless steel net is placed between two glass tubes and clamped by a clamp, the device is vertically placed, the toluene emulsion in the water pocket is poured, the water can rapidly pass through the separation device, oil drops are intercepted and gathered in the stainless steel net, and the filtrate is collected; when the water-in-toluene emulsion is separated, the super-hydrophilic surface of the three-dimensional Janus stainless steel net faces upwards and is placed in the separating device, the device is vertically placed, the water-in-toluene emulsion is poured, toluene can rapidly pass through the separating device, water drops are intercepted in the stainless steel net, and filtrate is collected. In the separation process, separation is carried out only by gravity without external acting force; the separation efficiency and the separation flux of the two emulsion separation processes were calculated, and the specific results are shown in tables 1 and 2. The result shows that the multifunctional three-dimensional Janus stainless steel mesh prepared by the invention has excellent emulsified oil-water separation capability. Table 1 shows the separation efficiency of the three-dimensional Janus stainless steel mesh separation oil-in-water (O/W) and water-in-oil (W/O) emulsions assembled from different stainless steel meshes and different super-hydrophilic stainless steel meshes in examples 1-5.
TABLE 1
As can be seen from table 1, when the mesh number of the stainless steel mesh is too small (200, 400 meshes), no matter how many sheets of super-hydrophilic stainless steel mesh are stacked, the separation efficiency is very low, and the emulsified oil and water cannot be well separated, and the emulsified oil and water separation capability is not provided. When the mesh number of the stainless steel net is higher than 600 meshes (600 meshes, 800 meshes, 1000 meshes), it can be seen from the table that the separation efficiency can reach more than 99% by increasing the number of the super-hydrophilic stainless steel net, therefore, the mesh number of the stainless steel net must be more than or equal to 600 in order to reach more than 99%. When the mesh number is larger than or equal to 600, the separation efficiency of the three-dimensional Janus stainless steel mesh is gradually increased along with the number of super-hydrophilic superposed sheets, when the number of the super-hydrophilic stainless steel meshes is close to 15 sheets, the oil-in-water and oil-in-water separation efficiency is increased to about 99.5%, and compared with the separation efficiency (40-60%) of 10 super-hydrophilic stainless steels, the three-dimensional Janus stainless steel mesh has jumping increase, has demulsification capability and can separate emulsified oil and water. This is probably because when the aperture reaches a certain requirement, the length of the capillary channel needs to reach a certain value to enable the three-dimensional Janus stainless steel net to have the demulsification capability, but when the number of the super-hydrophilic stainless steel nets stacked exceeds 15 (excluding 15), the separation efficiency of the three-dimensional Janus stainless steel net is slowly increased and is basically not changed. It can be determined that in order to improve the separation efficiency of emulsified oil and water of the assembled three-dimensional Janus stainless steel mesh to more than 99.5%, the number of the super-hydrophilic stainless steel meshes needs to be more than or equal to 15, and the mesh number of the stainless steel meshes needs to be more than or equal to 600.
Table 2 shows the separation flux test conditions of three-dimensional Janus stainless steel mesh separation oil-in-water (O/W) and water-in-oil (W/O) emulsions assembled by different stainless steel mesh numbers and different super-hydrophilic stainless steel mesh numbers in preparation examples 1-5.
TABLE 2
Table 2 shows the separation flux of the three-dimensional Janus stainless steel mesh for separating emulsified oil and water, which is obtained by assembling different stainless steel mesh numbers and different super-hydrophilic stainless steel mesh numbers. It can be seen from table 2 that the separation flux gradually decreases as the number of the stainless steel meshes increases, and similarly, the separation flux gradually decreases as the number of the super-hydrophilic stainless steel meshes increases. As discussed above, it is known that the separation efficiency is sufficiently high, the number of stacked sheets is not less than 15, and the mesh number of stainless steel is not less than 600, and therefore, even if the separation flux is high in the case where the mesh number is less than 600 and the number of stacked sheets is less than 15, the separation flux and the separation efficiency cannot be considered in these cases because of the low separation efficiency, and thus these cases are not considered. When the superposed number of the super-hydrophilic stainless steel nets is the same, the mesh number of the stainless steel nets is 1000, and the separation flux under the condition that the superposed number is more than or equal to 15 is far smaller than that of the three-dimensional Janus stainless steel nets with the mesh number of 600 and 800, for example, when the superposed number is 15, the mesh number is increased from 800 to 1000, and the separation fluxes are respectively 4956.71L m-2·h-1And 7572.11L · m-2·h-1Quickly reduced to 1643.15L m-2·h-1And 2067.34L · m-2·h-1However, the separation efficiency between them is not very different, so it is not reasonable to choose a 1000 mesh stainless steel net. Similarly, when the number of super-hydrophilic sheets is 25 and 30, the separation flux is far smaller than that of the three-dimensional Janus stainless steel net stacked with 15 and 20 super-hydrophilic stainless steel nets, for example, when the number of sheets is increased from 20 to 25 and the number of sheets is 800, the separation flux is rapidly reduced from 4241.92 and 7072.11 to 1536.77 L.m.-2·h-1And 2342.34L · m-2·h-1Likewise, their separation efficiencies are not very different, so it is not reasonable to choose to stack more than 25 sheets of super-hydrophilic stainless steel mesh. Therefore, on the premise of obtaining the demulsification capacity, the requirement that the mesh number of the stainless steel is 600-800 and the super-hydrophilic stainless steel is overlapped by 15-20 needs to be met while high separation efficiency and high separation flux are kept. Therefore, for the three-dimensional Janus stainless steel mesh, when the number of the stainless steel mesh is 600-800 and the super-hydrophilic stainless steel is overlapped by 15-20, the separation efficiency is as high as 99.5%, and the separation flux is 4000 L.m-2·h-1Above, the three-dimensional Janus stainless steel net has excellent ability to separate emulsified oil and water.
It should be noted that the present invention is not limited by the above-mentioned embodiments, and various changes and modifications can be made in the present invention without departing from the spirit and scope of the present invention, and these changes and modifications fall into the protection scope of the claimed invention; the scope of the invention is defined by the following claims.
Claims (10)
1. The utility model provides a three-dimensional Janus stainless steel net of separable emulsified oil water which characterized in that: the super-hydrophilic stainless steel mesh is formed by combining a two-dimensional Janus stainless steel mesh and a super-hydrophilic stainless steel mesh which is obtained by treating a stainless steel mesh with the mesh number of 600-800 with a dopamine/polyethyleneimine ethanol solution; the two-dimensional Janus stainless steel mesh is obtained by performing super-hydrophilic and super-hydrophobic modification treatment on a stainless steel mesh with the mesh number of 600-800, wherein one surface is a super-hydrophilic surface, and the other surface is a high-hydrophobic surface; and (3) superposing 15-20 super-hydrophilic stainless steel meshes and placing the superposed super-hydrophilic surfaces on the two-dimensional Janus stainless steel mesh.
2. The three-dimensional Janus stainless steel mesh capable of separating emulsified oil and water as claimed in claim 1, wherein: the super-hydrophilic stainless steel net is obtained by the following method: cleaning a stainless steel net, drying, soaking in a precursor solution, cleaning with deionized water, and drying; the precursor solution is prepared by adding 1-4 parts of dopamine hydrochloride, 1-4 parts of polyethyleneimine, 2-6 parts of Tris-HCl and 40-60 parts of water, 10-30 parts of ammonia water, 300-600 parts of ethanol, carrying out ultrasonic treatment until the materials are fully dissolved, and then adding 3-6 parts of ethyl orthosilicate in parts by mass.
3. The three-dimensional Janus stainless steel mesh capable of separating emulsified oil and water as claimed in claim 2, wherein: the ultrasonic treatment time is 30-60 min, and the stainless steel net is cleaned by respectively using acetone, ethanol and deionized water.
4. The three-dimensional Janus stainless steel mesh capable of separating emulsified oil and water as claimed in claim 1, wherein: the two-dimensional Janus stainless steel mesh is obtained by placing the weak hydrophobic side of a high-hydrophobic/weak-hydrophobic stainless steel mesh on the liquid surface of a dopamine aqueous solution, performing ultrasonic treatment, performing single-side super-hydrophilic modification, and then cleaning and drying with deionized water; the high-hydrophobicity/weak-hydrophobicity stainless steel mesh is obtained by placing a super-hydrophilic stainless steel mesh on a phase interface of a carbon tetrachloride solution of perfluorosiloxane and water for modification, wherein one side of the high-hydrophobicity/weak-hydrophobicity stainless steel mesh close to the carbon tetrachloride solution has high hydrophobicity, and one side of the high-hydrophobicity/weak-hydrophobicity stainless steel mesh close to the water has weak hydrophobicity.
5. The three-dimensional Janus stainless steel mesh capable of separating emulsified oil and water as claimed in claim 4, wherein: the perfluorosiloxane carbon tetrachloride solution is composed of 50-150 parts of carbon tetrachloride and 1-4 parts of perfluorosiloxane by mass, and the heating condition is water bath, the temperature is 35-45 ℃, and the reaction time is 60-90 min.
6. The three-dimensional Janus stainless steel mesh capable of separating emulsified oil and water as claimed in claim 5, wherein: the perfluorosiloxane is 1H,1H,2H, 2H-perfluorohexyltriethoxysilane, 1H,2H, 2H-perfluoroheptyltriethoxysilane or 1H,1H,2H, 2H-perfluorodecyltriethoxysilane.
7. The three-dimensional Janus stainless steel mesh capable of separating emulsified oil and water as claimed in claim 1, wherein: the stainless steel net is a twill net; the contact angle of the highly hydrophobic surface in water in air is larger than 130 degrees.
8. The three-dimensional Janus stainless steel mesh capable of separating emulsified oil and water as claimed in claim 1, wherein: the contact angle of the super hydrophilic surface with water in the air is equal to 0 degree.
9. The method for preparing the three-dimensional Janus stainless steel mesh capable of separating the emulsified oil and the water as claimed in any one of claims 1 to 8, which is characterized by comprising the following steps:
1) cleaning the stainless steel net, and drying for later use;
2) preparing a precursor solution: adding 1-4 parts of dopamine hydrochloride, 1-4 parts of polyethyleneimine, 2-6 parts of Tris-HCl and 40-60 parts of water 10-30 parts of ammonia water into 300-600 parts of ethanol by mass, and carrying out ultrasonic treatment until the dopamine hydrochloride, the polyethyleneimine, the Tris-HCl and the ammonia water are fully dissolved; adding 3-6 parts of tetraethoxysilane into the obtained solution to obtain a precursor solution;
3) putting the stainless steel mesh obtained in the step 1) into the precursor solution obtained in the step 2), shaking by using a shaking table, washing by using deionized water for a plurality of times, and drying to obtain a super-hydrophilic stainless steel mesh;
4) placing the super-hydrophilic stainless steel mesh obtained in the step 3) on a phase interface of a carbon tetrachloride solution of perfluorosiloxane and water for single-side modification to obtain a high-hydrophobicity/weak-hydrophobicity stainless steel mesh, wherein one side of the high-hydrophobicity/weak-hydrophobicity stainless steel mesh close to the carbon tetrachloride solution has high hydrophobicity, and one side of the high-hydrophobicity/weak-hydrophobicity stainless steel mesh close to the water has weak hydrophobicity;
5) preparing a dopamine solution: placing the weak hydrophobic side of the high-hydrophobic/weak-hydrophobic stainless steel mesh obtained in the step 4) on the liquid surface of the dopamine aqueous solution, performing ultrasonic treatment, performing single-side super-hydrophilic modification, washing with deionized water, and drying to obtain a two-dimensional Janus stainless steel mesh; the dopamine aqueous solution is obtained by adding 1-4 parts of dopamine hydrochloride, 1-4 parts of polyethyleneimine, 2-6 parts of Tris-HCl and 10-30 parts of ammonia water into 300-600 parts of deionized water in parts by mass, mixing and then carrying out ultrasonic treatment;
6) and (3) superposing 15-20 pieces of the super-hydrophilic stainless steel mesh obtained in the step 3) on the super-hydrophilic side of the two-dimensional Janus stainless steel mesh obtained in the step 5), and combining to obtain the three-dimensional Janus stainless steel mesh capable of separating the emulsified oil and the water.
10. The method for preparing the three-dimensional Janus stainless steel mesh capable of separating the emulsified oil and the water according to claim 9, wherein the three-dimensional Janus stainless steel mesh comprises the following steps: the rotating speed of the shaking table in the step 3) is 90-120 rpm, and the shaking time is 6-12 h; the single-side super-hydrophilic modification time in the step 5) is 10-60 min.
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