CN106633140A - Silicon-carrying microsphere, copper net for separating oil from water and preparation method thereof - Google Patents
Silicon-carrying microsphere, copper net for separating oil from water and preparation method thereof Download PDFInfo
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- CN106633140A CN106633140A CN201611234292.0A CN201611234292A CN106633140A CN 106633140 A CN106633140 A CN 106633140A CN 201611234292 A CN201611234292 A CN 201611234292A CN 106633140 A CN106633140 A CN 106633140A
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- microballoon
- preparation
- polymer
- water
- silicon
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- 239000010949 copper Substances 0.000 title claims abstract description 91
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 86
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 86
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 76
- 238000002360 preparation method Methods 0.000 title claims abstract description 75
- 239000004005 microsphere Substances 0.000 title abstract description 11
- 239000006185 dispersion Substances 0.000 claims abstract description 20
- 239000000853 adhesive Substances 0.000 claims abstract description 18
- 230000001070 adhesive effect Effects 0.000 claims abstract description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 214
- 229920000642 polymer Polymers 0.000 claims description 96
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 78
- 229910052710 silicon Inorganic materials 0.000 claims description 78
- 239000010703 silicon Substances 0.000 claims description 78
- 235000019441 ethanol Nutrition 0.000 claims description 69
- 239000000178 monomer Substances 0.000 claims description 51
- 239000003921 oil Substances 0.000 claims description 51
- 238000006243 chemical reaction Methods 0.000 claims description 45
- -1 isodecyl ester Chemical class 0.000 claims description 34
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 33
- 239000011259 mixed solution Substances 0.000 claims description 31
- 238000003756 stirring Methods 0.000 claims description 30
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 27
- 229910000077 silane Inorganic materials 0.000 claims description 27
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 24
- 239000003999 initiator Substances 0.000 claims description 23
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- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 8
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- RUMACXVDVNRZJZ-UHFFFAOYSA-N 2-methylpropyl 2-methylprop-2-enoate Chemical compound CC(C)COC(=O)C(C)=C RUMACXVDVNRZJZ-UHFFFAOYSA-N 0.000 claims description 5
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- LJRSZGKUUZPHEB-UHFFFAOYSA-N 2-[2-(2-prop-2-enoyloxypropoxy)propoxy]propyl prop-2-enoate Chemical compound C=CC(=O)OC(C)COC(C)COC(C)COC(=O)C=C LJRSZGKUUZPHEB-UHFFFAOYSA-N 0.000 claims description 4
- GHUXAYLZEGLXDA-UHFFFAOYSA-N 8-azido-5-ethyl-6-phenylphenanthridin-5-ium-3-amine;bromide Chemical compound [Br-].C12=CC(N=[N+]=[N-])=CC=C2C2=CC=C(N)C=C2[N+](CC)=C1C1=CC=CC=C1 GHUXAYLZEGLXDA-UHFFFAOYSA-N 0.000 claims description 4
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- IAXXETNIOYFMLW-COPLHBTASA-N [(1s,3s,4s)-4,7,7-trimethyl-3-bicyclo[2.2.1]heptanyl] 2-methylprop-2-enoate Chemical compound C1C[C@]2(C)[C@@H](OC(=O)C(=C)C)C[C@H]1C2(C)C IAXXETNIOYFMLW-COPLHBTASA-N 0.000 claims description 4
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- 229940117969 neopentyl glycol Drugs 0.000 claims description 4
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 claims description 4
- CIHOLLKRGTVIJN-UHFFFAOYSA-N tert‐butyl hydroperoxide Chemical compound CC(C)(C)OO CIHOLLKRGTVIJN-UHFFFAOYSA-N 0.000 claims description 4
- PSGCQDPCAWOCSH-UHFFFAOYSA-N (4,7,7-trimethyl-3-bicyclo[2.2.1]heptanyl) prop-2-enoate Chemical compound C1CC2(C)C(OC(=O)C=C)CC1C2(C)C PSGCQDPCAWOCSH-UHFFFAOYSA-N 0.000 claims description 3
- VFZKVQVQOMDJEG-UHFFFAOYSA-N 2-prop-2-enoyloxypropyl prop-2-enoate Chemical compound C=CC(=O)OC(C)COC(=O)C=C VFZKVQVQOMDJEG-UHFFFAOYSA-N 0.000 claims description 3
- DXPPIEDUBFUSEZ-UHFFFAOYSA-N 6-methylheptyl prop-2-enoate Chemical group CC(C)CCCCCOC(=O)C=C DXPPIEDUBFUSEZ-UHFFFAOYSA-N 0.000 claims description 3
- GMSCBRSQMRDRCD-UHFFFAOYSA-N dodecyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCCOC(=O)C(C)=C GMSCBRSQMRDRCD-UHFFFAOYSA-N 0.000 claims description 3
- YDKNBNOOCSNPNS-UHFFFAOYSA-N methyl 1,3-benzoxazole-2-carboxylate Chemical compound C1=CC=C2OC(C(=O)OC)=NC2=C1 YDKNBNOOCSNPNS-UHFFFAOYSA-N 0.000 claims description 3
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- 239000011734 sodium Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 229940005605 valeric acid Drugs 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F212/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F212/02—Monomers containing only one unsaturated aliphatic radical
- C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F212/06—Hydrocarbons
- C08F212/08—Styrene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/14—Methyl esters, e.g. methyl (meth)acrylate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/06—Coating with compositions not containing macromolecular substances
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
- C09D133/04—Homopolymers or copolymers of esters
- C09D133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09D133/10—Homopolymers or copolymers of methacrylic acid esters
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- C08J2333/06—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters of esters containing only carbon, hydrogen, and oxygen, the oxygen atom being present only as part of the carboxyl radical
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Abstract
The invention relates to a silicon-carrying microsphere, a copper net for separating oil from water and a preparation method thereof and belongs to the technical field of a new material for modifying/absorbing a material surface. The preparation method for the silicon-carrying microsphere comprises the following steps: preparing a polymeric microsphere, enveloping the polymeric microsphere and modifying the silicon-carrying microsphere. The preparation method for the silicon-carrying microsphere is simple in process and the prepared silicon-carrying microsphere has uniform granularity and excellent lyophobic property and is beneficial to dispersion. The preparation method for the copper net for separating oil from water comprises the following steps: spraying a double-component adhesive onto the copper net, thereby acquiring a first copper net, and then spraying the prepared silicon-carrying microsphere onto the first copper net, thereby acquiring the copper net for separating oil from water. The copper net prepared according to the method has a better oil-water separating effect and can be conveniently recycled and reused.
Description
Technical field
The present invention relates to material surface modifying/absorption new material technology field, and more particularly to a kind of load silicon microballoon, profit
Separation copper mesh and preparation method thereof.
Background technology
The generation of event and the raising of people's environmental consciousness are revealed with offshore oil, how petroleum pollution in ocean is solved
Become the focus and difficult point of recent scientific research.Earliest oily water separating equipment is based on physical diffusion method, freezing method, biology drop
Solution, situ combustion method and skimming method etc..And these methods exist and can not effectively reclaim oil spilling or can cause secondary pollution
The problems such as.Since the super compatibility materials of reported first such as Jiang Lei in 2004 are used for after water-oil separating, super hydrophobic material causes all
The concern of many scholars.Research finds that super-hydrophobic/super-oleophilic material has preferable Selective adsorption to oil water mixture, can be with
Water-oil separating is realized, this has great meaning for process petroleum pollution in ocean.
High, the pressure fabric of compactness, the strong sponge of loose, oil absorption and rigid backbone, the metal being easily assembled
Net etc. is to use more water-oil separating material.And the structure of super-hydrophobic coat to be then this kind of material really be able in practice should
Key.The structure of super-hydrophobic coat mainly includes two aspects：One is to modify low-surface energy substance in coarse substrate；
Two is to build the surface fine structure with certain roughness in hydrophobic surface.And the structure of rough interfaces be then realize it is super-hydrophobic
A most important step.
There is plasma method using the method at the more super-hydrophobic interface of structure at present, chemical vapor infiltration, Electrospinning Method is changed
Learn etching method etc..But the material of costliness, special equipment or strict reaction condition significantly limit super-hydrophobic coat
Promotion and application in practice.Lu et al. is by by the TiO of～200nm and～20nm2Mix to provide surface roughness, lead to
Cross tridecafluoro-n-octyltriethoxysilane to provide low-surface energy substance structure super-hydrophobic coat.Chen et al. is by by ten trifluoros
Calcium carbonate after octyltri-ethoxysilane modification is sprayed on adhesive, and constructing automatically cleaning interface and this coating can be with
Undergo repeated multiple times scraping and still keep superhydrophobic characteristic.But these methods have used price, and surface energy costly is extremely low
Fluorine containing silane coupling agent low-surface-energy modification is carried out to substrate surface, also limit to a certain extent super hydrophobic material should
With.
At present micro-nano compound structure microballoon prepares the research of super-hydrophobic coat, is concentrated mainly on and is received by hundreds of nanometer and tens
The SiO of rice2Or TiO2Micro-/ nano particle provides surface roughness, and to other multiple dimensioned micro-/ nano particles super-hydrophobic coat is built
Research it is relatively fewer.Therefore, the special wellability based on material, is easy to get using raw material economics, and preparation process is simply efficient, system
Standby mild condition, the technological means being produced on a large scale, the material of design and preparation with high efficiency oil-water stalling characteristic has weight
The using value wanted and meaning.
The content of the invention
It is an object of the invention to provide a kind of preparation method for carrying silicon microballoon, the method is easy to operate, and reaction condition is easy
Control, raw material is easy to get, and obtained microballoon hydrophobicity is strong, and application is wider, and suitable for large-scale production application, using scale
Change application.
Another object of the present invention is to provide a kind of preparation method of water-oil separating copper mesh, this kind of copper mesh can be used extensively
In greasy dirt is processed, also facilitate and reclaim copper mesh, can reuse, and be not result in the passivation of copper mesh.
The present invention solves its technical problem and employs the following technical solutions to realize.
A kind of preparation method for carrying silicon microballoon, it comprises the steps：
Polymer microballoon preparation process：Polymer monomer, initiator, dispersant and crosslinking agent are added to into ethanol/water to mix
In closing solution, polymer microballoon is obtained, is passed through nitrogen 25-35min, then 70-75 DEG C of oil bath reaction, reaction uses respectively water after terminating
With ethanol dispersion centrifugation 2-5 time；
Polymer microballoon is coated with step：Obtained polymer microballoon is scattered in ethanol/water mixed solution, polymer is micro-
Ball is 1 with ethanol/water mixed solution solid-liquid ratio:1-1.2, adds ammoniacal liquor, is stirring evenly and then adding into tetraethyl orthosilicate, 18-24 DEG C
Reaction 22-26h, reaction is centrifuged 2-5 time respectively after terminating with water and ethanol dispersion, obtains carrying silicon microballoon；
Carry silicon microballoon modification step：Silane coupler is added in absolute ethyl alcohol, load silicon microballoon is stirring evenly and then adding into,
1-4h is stirred under 18-24 DEG C of temperature conditionss, hydrophobic silane is obtained and is coupled load silicon microballoon.
A kind of preparation method of water-oil separating copper mesh, by amion-terminated polyurethane/epoxy resin two-component adhesive spraying
On copper mesh, the first copper mesh is obtained；Again first will be sprayed at using load silicon microballoon obtained in the preparation method of above-mentioned load silicon microballoon
Copper mesh, obtains water-oil separating copper mesh.
The beneficial effect of a kind of load silicon microballoon, the water-oil separating copper mesh of the embodiment of the present invention and preparation method thereof is：Should
Method is simple, and raw material is easy to get, and obtained microballoon hydrophobicity is strong, and application is wider, stable performance, uniform particle sizes, is suitable for
In large-scale production application, using scale application；Process greasy dirt can be widely used in by copper mesh obtained in the method, also side
Just copper mesh is reclaimed, can be reused, and be not result in the passivation of copper mesh.
Description of the drawings
In order to be illustrated more clearly that the technical scheme of the embodiment of the present invention, below will be attached to what is used needed for embodiment
Figure is briefly described, it will be appreciated that the following drawings illustrate only certain embodiments of the present invention, thus be not construed as it is right
The restriction of scope, for those of ordinary skill in the art, on the premise of not paying creative work, can be with according to this
A little accompanying drawings obtain other related accompanying drawings.
Fig. 1 a are the contact angle experiments figure of the unmodified copper mesh that the embodiment of the present invention 8 is provided；
Fig. 1 b are the contact angle experiments figure of the copper mesh of the modified that the embodiment of the present invention 8 is provided；
Fig. 2 a are that the embodiment of the present invention 8 carries silicon microballoon SEM scanning figures；
Fig. 2 b are that the embodiment of the present invention 8 carries silicon microballoon AFM scan figure.
Specific embodiment
To make purpose, technical scheme and the advantage of the embodiment of the present invention clearer, below will be in the embodiment of the present invention
Technical scheme be clearly and completely described.Unreceipted actual conditions person, builds according to normal condition or manufacturer in embodiment
The condition of view is carried out.Agents useful for same or the unreceipted production firm person of instrument, being can pass through the conventional product that commercially available purchase is obtained
Product.
A kind of water-oil separating copper mesh of the embodiment of the present invention and preparation method thereof is specifically described below.
A kind of preparation method for carrying silicon microballoon, it comprises the steps：
Polymer microballoon preparation process：Polymer monomer, initiator, dispersant and crosslinking agent are added to into ethanol/water to mix
In closing solution, polymer microballoon is obtained, is passed through nitrogen 25-35min, then 70-75 DEG C of oil bath reaction, reaction uses respectively water after terminating
With ethanol dispersion centrifugation 2-5 time.
Polymer monomer, initiator, dispersant and crosslinking agent are added in ethanol/water mixed solution is conducive to raw material to mix
Close, be passed through nitrogen, form nitrogen protection, the polymerization for being conducive to polymer microballoon is formed, 70-75 DEG C of oil bath reaction accelerates micro-
The formation of ball.
Further, in present pre-ferred embodiments, preparing the polymer monomer of polymer microballoon includes styrene, first
Base methyl acrylate, EMA, isobornyl methacrylate, butyl methacrylate, lauryl
Ester, Isobutyl methacrylate, isodecyl methacrylate, EHMA, methyl acrylate, ethyl acrylate,
Isobornyl acrylate, butyl acrylate, lauryl acrylate, isobutyl acrylate, isodecyl acrylate or acrylic acid are different pungent
At least one of ester.
Further, in present pre-ferred embodiments, the polymer microballoon that polymer microballoon preparation process is prepared
Including first polymer microballoon and second polymer microballoon, the particle diameter of first polymer microballoon is 0.2～1.0 μm, the second polymerization
The particle diameter of thing microballoon is 20-200nm；Preparing the initiator of first polymer microballoon includes azodiisobutyronitrile, azo two different heptan
At least one of nitrile, benzoyl peroxide, TBHP, peroxidized t-butyl perbenzoate.
Further, in present pre-ferred embodiments, preparing the initiator of second polymer microballoon includes azo dicyan
Base valeric acid, the isobutyl imidazoline hydrochloride of azo two, azo diisobutyl amidine hydrochloride, the hydration of the N- hydroxyisobutyls amidine of azo two
Thing, the N of azo two, N cyclobutyl isobutyl amidine hydrate, azo dimethyl N-2- hydroxyl butylacrylamides, ammonium persulfate, persulfuric acid
At least one of potassium.
Further, in present pre-ferred embodiments, the crosslinking agent in polymer microballoon preparation process includes divinyl
Base benzene, diethylene glycol diacrylate, triethylene glycol diacrylate, polyethyleneglycol diacrylate, the propylene of DPG two
Acid esters, tri (propylene glycol) diacrylate, BDO diacrylate, 1,6 hexanediyl ester, neopentyl glycol
Diacrylate, 2 (the third oxidation) neopentylglycol diacrylates, ethoxylated bisphenol A diacrylates, (ethyoxyl) bisphenol fluorene two
At least one of acrylate, 6 (ethyoxyl) bisphenol fluorene diacrylates, tricyclic decane Dimethanol Diacrylate.
Further, in present pre-ferred embodiments, the dispersant in polymer microballoon preparation process is polyethylene pyrrole
Pyrrolidone.
Polymer microballoon is coated with step：Obtained polymer microballoon is scattered in ethanol/water mixed solution, polymer is micro-
Ball is 1 with ethanol/water mixed solution solid-liquid ratio:0.9-1.2, adds ammoniacal liquor, is stirring evenly and then adding into tetraethyl orthosilicate, 18-24
DEG C reaction 22-26h, reaction terminate after respectively with water and ethanol dispersion centrifugation 2-5 time, obtain load silicon microballoon.
Further, in present pre-ferred embodiments, the load silicon microballoon added in silicon microballoon modification step is carried by first
Polymer microballoon and second polymer microballoon are constituted, and first polymer microballoon and second polymer microballoon are 0.4/ according to mass ratio
0.6～0.6/0.4 is constituted.
Carry silicon microballoon modification step：Silane coupler is added in absolute ethyl alcohol, load silicon microballoon is stirring evenly and then adding into,
1-4h is stirred under 18-24 DEG C of temperature conditionss, hydrophobic silane is obtained and is coupled load silicon microballoon；
Further, in present pre-ferred embodiments, it is carbon atom to carry the silane coupler in silicon microballoon modification step
Long carbon chain silane coupler of the number more than ten, silane coupler is 0.5/100～1/100 with the volume ratio of ethanol.
A kind of preparation method of water-oil separating copper mesh, by amion-terminated polyurethane/epoxy resin two-component adhesive spraying
On copper mesh, the first copper mesh is obtained；The first copper mesh will be sprayed at using the obtained silicon microballoon that carries of said method again, obtain profit point
From with copper mesh.
Further, in present pre-ferred embodiments, by amion-terminated polyurethane and epoxy resin according to 0.8-1.2：
The ratio mixing of 0.9-1.1, is then blended with acetone, obtains amion-terminated polyurethane/asphalt mixtures modified by epoxy resin that concentration is 0.005-0.1g/mL
Fat two-component adhesive.
The feature and performance of the present invention are described in further detail with reference to embodiments.
Embodiment 1
A kind of preparation method for carrying silicon microballoon, it comprises the steps：
Polymer microballoon preparation process：(1) preparation of first polymer microballoon, will account for the monomer of overall reaction system quality 5%
Styrene, methyl methacrylate, EMA；It is even relative to the initiator azodiisobutyronitrile of monomer mass 1%
The different heptonitrile of nitrogen two；Relative to the cross-linker divinylbenzene of monomer mass 1%, diethylene glycol diacrylate, triethylene glycol two
Acrylate；And relative to the polyethylene of dispersing agent pyrrolidones of monomer mass 10%；It is added to the second of volume fraction 20%
In alcohol/water mixed solution, stir, be passed through nitrogen 25min, then react 10h in 70 DEG C of oil bath pan；After reaction terminates
It is centrifuged 2 times with water and ethanol dispersion respectively, micron order first polymer microballoon is obtained；
(2) preparation of second polymer microballoon, will account for the monomer methacrylic acid isobornyl thiocyanoacetate of overall reaction system quality 5%；
Relative to the initiator azo diisobutyl amidine hydrochloride of monomer mass 2%；Relative to the crosslinking agent 1,4- fourths of monomer mass 3%
Omega-diol diacrylate；And relative to the polyethylene of dispersing agent pyrrolidones of monomer mass 10%；It is added to volume fraction
In 20% ethanol/water mixed solution, stir, be passed through nitrogen 28min, then react 6h in 71 DEG C of oil bath pan；Instead
Respectively with water and ethanol dispersion 2 prepared submicron order second polymer microballoons of centrifugation after should terminating.
Polymer microballoon is coated with step：By obtained first polymer microballoon and second polymer microballoon according to 0.4:0.6
Mass ratio mixing, in being scattered in ethanol/water mixed solution, polymer microballoon and ethanol/water mixed solution solid-liquid ratio are 1:1,
The ammoniacal liquor of the volume of ethanol/water mixed solution 1/200 is added, is stirring evenly and then adding into and the isopyknic tetraethyl orthosilicate of ammoniacal liquor, 21
DEG C reaction 23h, reaction terminate after respectively with water and ethanol dispersion centrifugation 3 times, obtain carry silicon microballoon.
Carry silicon microballoon modification step：Silane coupler is added in absolute ethyl alcohol, the volume of silane coupler and ethanol
Than 0.5:100；Load silicon microballoon is stirring evenly and then adding into, it is 0.9 to carry silicon microballoon with the solid-liquid ratio of absolute ethyl alcohol:10；18 DEG C of temperature
4h is stirred under the conditions of degree, hydrophobic silane is obtained and is coupled load silicon microballoon.
Embodiment 2
A kind of preparation method for carrying silicon microballoon, it comprises the steps：
Polymer microballoon preparation process：(1) preparation of first polymer microballoon, will account for the monomer of overall reaction system quality 7%
Styrene；Relative to the initiator ABVN of monomer mass 1.5%；Relative to the crosslinking agent bag of monomer mass 1.5%
Include divinylbenzene, diethylene glycol diacrylate, triethylene glycol diacrylate, polyethyleneglycol diacrylate, dipropyl two
Alcohol diacrylate, tri (propylene glycol) diacrylate, BDO diacrylate, 1,6 hexanediyl ester,
Neopentylglycol diacrylate, 2 (the third oxidation) neopentylglycol diacrylates, ethoxylated bisphenol A diacrylates, (ethyoxyl)
Bisphenol fluorene diacrylate, 6 (ethyoxyl) bisphenol fluorene diacrylates, tricyclic decane Dimethanol Diacrylate；And it is relative
In the polyethylene of dispersing agent pyrrolidones of monomer mass 12%；In being added to the ethanol/water mixed solution of volume fraction 18%, stir
Mix uniform, be passed through nitrogen 27min, then react 6h in 75 DEG C of oil bath pan；Reaction is disperseed respectively after terminating with water and ethanol
3 prepared micron order first polymer microballoons of centrifugation；
(2) preparation of second polymer microballoon, will account for the monomer methacrylic acid lauryl of overall reaction system quality 6%, first
Base isobutyl acrylate；Relative to the initiator azo diisobutyl amidine hydrochloride of monomer mass 1.5%, the N- hydroxyls of azo two are different
Butyl amidine hydrate；Relative to the crosslinking agent polyethyleneglycol diacrylate of monomer mass 1%, propylene glycol diacrylate；
And relative to the polyethylene of dispersing agent pyrrolidones of monomer mass 13%；It is added to the ethanol/water mixing of volume fraction 22%
In solution, stir, be passed through nitrogen 30min, then react 8h in 73 DEG C of oil bath pan；Reaction terminate after respectively with water and
Ethanol dispersion centrifugation 2 times, is obtained submicron order second polymer microballoon.
Polymer microballoon is coated with step：By obtained first polymer microballoon and second polymer microballoon according to 0.5:0.5
Mass ratio mixing, in being scattered in ethanol/water mixed solution, polymer microballoon and ethanol/water mixed solution solid-liquid ratio are 1:
1.1, the ammoniacal liquor of the volume of ethanol/water mixed solution 1/210 is added, it is stirring evenly and then adding into positive silicic acid second isopyknic with ammoniacal liquor
Ester, 18 DEG C of reaction 24h, reaction is centrifuged 5 times respectively after terminating with water and ethanol dispersion, obtains carrying silicon microballoon.
Carry silicon microballoon modification step：Silane coupler is added in absolute ethyl alcohol, the volume of silane coupler and ethanol
Than 1:190；Load silicon microballoon is stirring evenly and then adding into, it is 1.1 to carry silicon microballoon with the solid-liquid ratio of absolute ethyl alcohol:10；20 DEG C of temperature
Under the conditions of stir 3h, obtain hydrophobic silane be coupled carry silicon microballoon.
Embodiment 3
A kind of preparation method for carrying silicon microballoon, it comprises the steps：
Polymer microballoon preparation process：(1) preparation of first polymer microballoon, will account for the monomer of overall reaction system quality 9%,
Monomer includes styrene, methyl methacrylate, EMA, isobornyl methacrylate, methacrylic acid fourth
Ester, lauryl methacrylate, Isobutyl methacrylate, isodecyl methacrylate, EHMA, acrylic acid
Methyl esters, ethyl acrylate, isobornyl acrylate, butyl acrylate, lauryl acrylate, isobutyl acrylate, acrylic acid are different
Last of the ten Heavenly stems ester or Isooctyl acrylate monomer；Relative to the initiator azodiisobutyronitrile of monomer mass 2%, ABVN, peroxidating
Benzoyl, TBHP；Relative to the cross-linker divinylbenzene of monomer mass 3%, diethylene glycol diacrylate；
And relative to the polyethylene of dispersing agent pyrrolidones of monomer mass 16%；It is added to the ethanol/water mixing of volume fraction 22%
In solution, stir, be passed through nitrogen 35min, then react 7h in 74 DEG C of oil bath pan；Reaction terminate after respectively with water and
Ethanol dispersion 4 prepared micron order first polymer microballoons of centrifugation；
(2) preparation of second polymer microballoon, will account for the monomer styrene of overall reaction system quality 10%, methyl methacrylate
Ester, EMA, isobornyl methacrylate, butyl methacrylate, lauryl methacrylate, metering system
Sour isobutyl ester, isodecyl methacrylate, EHMA, methyl acrylate, ethyl acrylate, isobomyl acrylate
Ester, butyl acrylate, lauryl acrylate, isobutyl acrylate, isodecyl acrylate or Isooctyl acrylate monomer；Relative to monomer
The initiator azo dicyano valeric acid of quality 3%, the isobutyl imidazoline hydrochloride of azo two, azo diisobutyl amidine hydrochloride；Phase
For the crosslinking agent polyethyleneglycol diacrylate of monomer mass 2%, propylene glycol diacrylate；And relative to monomer matter
The polyethylene of dispersing agent pyrrolidones of amount 18%；In being added to the ethanol/water mixed solution of volume fraction 22%, stir,
Nitrogen 35min is passed through, then 6h is reacted in 75 DEG C of oil bath pan；Reaction is centrifuged 5 times respectively after terminating with water and ethanol dispersion,
Prepared submicron order second polymer microballoon.
Polymer microballoon is coated with step：By obtained first polymer microballoon and second polymer microballoon according to 0.6:0.4
Mass ratio mixing, in being scattered in ethanol/water mixed solution, polymer microballoon and ethanol/water mixed solution solid-liquid ratio are 1:
1.2, the ammoniacal liquor of the volume of ethanol/water mixed solution 1/220 is added, it is stirring evenly and then adding into positive silicic acid second isopyknic with ammoniacal liquor
Ester, 20 DEG C of reaction 26h, reaction is centrifuged 2 times respectively after terminating with water and ethanol dispersion, obtains carrying silicon microballoon.
Carry silicon microballoon modification step：Silane coupler is added in absolute ethyl alcohol, the volume of silane coupler and ethanol
Than 1:180；Load silicon microballoon is stirring evenly and then adding into, it is 1.0 to carry silicon microballoon with the solid-liquid ratio of absolute ethyl alcohol:10；22 DEG C of temperature
Under the conditions of stir 2h, obtain hydrophobic silane be coupled carry silicon microballoon.
Embodiment 4
A kind of preparation method for carrying silicon microballoon, it comprises the steps：
Polymer microballoon preparation process：(1) preparation of first polymer microballoon, will account for overall reaction system quality 10% single
Body, monomer includes styrene, methyl methacrylate；Relative to the initiator azodiisobutyronitrile of monomer mass 3%, azo two
Different heptonitrile, benzoyl peroxide；Relative to the cross-linker divinylbenzene of monomer mass 2%, diethylene glycol diacrylate；With
And relative to the polyethylene of dispersing agent pyrrolidones of monomer mass 18%；The ethanol/water mixing for being added to volume fraction 18% is molten
In liquid, stir, be passed through nitrogen 32min, then react 8h in 73 DEG C of oil bath pan；Reaction uses respectively water and second after terminating
Alcohol dispersion 5 prepared micron order first polymer microballoons of centrifugation；
(2) preparation of second polymer microballoon, will account for the monomer styrene of overall reaction system quality 8%, the methacrylic acid moon
Osmanthus ester, Isobutyl methacrylate；Relative to the N of initiator azo two of monomer mass 1%, the hydration of N ' cyclobutyl isobutyl amidine
Thing, azo dimethyl N-2- hydroxyl butylacrylamides, ammonium persulfate, potassium peroxydisulfate；Relative to the crosslinking agent of monomer mass 1.5%
Divinylbenzene, diethylene glycol diacrylate, triethylene glycol diacrylate, polyethyleneglycol diacrylate, DPG
Diacrylate, tri (propylene glycol) diacrylate, BDO diacrylate, 1,6 hexanediyl ester, newly
Diacrylate, 2 (the third oxidation) neopentylglycol diacrylates, ethoxylated bisphenol A diacrylates, (ethyoxyl) is double
Phenol fluorenes diacrylate, 6 (ethyoxyl) bisphenol fluorene diacrylates, tricyclic decane Dimethanol Diacrylate；And relative to
The polyethylene of dispersing agent pyrrolidones of monomer mass 11%；In being added to the ethanol/water mixed solution of volume fraction 22%, stirring
Uniformly, nitrogen 25min is passed through, then 10h is reacted in 72 DEG C of oil bath pan；Reaction terminate after respectively with water and ethanol disperse from
The heart 3 times, is obtained submicron order second polymer microballoon.
Polymer microballoon is coated with step：By obtained first polymer microballoon and second polymer microballoon according to 0.4:0.6
Mass ratio mixing, in being scattered in ethanol/water mixed solution, polymer microballoon and ethanol/water mixed solution solid-liquid ratio are 1:
0.9, the ammoniacal liquor of the volume of ethanol/water mixed solution 1/230 is added, it is stirring evenly and then adding into positive silicic acid second isopyknic with ammoniacal liquor
Ester, 24 DEG C of reaction 22h, reaction is centrifuged 3 times respectively after terminating with water and ethanol dispersion, obtains carrying silicon microballoon.
Carry silicon microballoon modification step：Silane coupler is added in absolute ethyl alcohol, the volume of silane coupler and ethanol
Than 1:190；Load silicon microballoon is stirring evenly and then adding into, it is 0.9 to carry silicon microballoon with the solid-liquid ratio of absolute ethyl alcohol:10；20 DEG C of temperature
Under the conditions of stir 3h, obtain hydrophobic silane be coupled carry silicon microballoon.
Embodiment 5
A kind of preparation method for carrying silicon microballoon, it comprises the steps：
Polymer microballoon preparation process：(1) preparation of first polymer microballoon, will account for the monomer of overall reaction system quality 6%,
Monomer includes styrene, methyl methacrylate, butyl methacrylate；Relative to the initiator azo of monomer mass 2.5%
Bis-isobutyronitrile, ABVN, benzoyl peroxide, TBHP, peroxidized t-butyl perbenzoate；Relative to list
The cross-linker divinylbenzene of weight 2%, diethylene glycol diacrylate, triethylene glycol diacrylate, polyethylene glycol two
Acrylate；And relative to the polyethylene of dispersing agent pyrrolidones of monomer mass 14%；It is added to the second of volume fraction 18%
In alcohol/water mixed solution, stir, be passed through nitrogen 29min, then react 9h in 72 DEG C of oil bath pan；After reaction terminates
Respectively with water and ethanol dispersion 3 prepared micron order first polymer microballoons of centrifugation；
(2) preparation of second polymer microballoon, will account for the monomer styrene of overall reaction system quality 7%, the methacrylic acid moon
Osmanthus ester, Isobutyl methacrylate, isobutyl acrylate；Relative to the initiator azo dicyano valeric acid of monomer mass 2.5%,
The isobutyl imidazoline hydrochloride of azo two, azo diisobutyl amidine hydrochloride, the N- hydroxyisobutyl amidine hydrates of azo two, azo two
N, N ' cyclobutyl isobutyl amidine hydrate, azo dimethyl N-2- hydroxyl butylacrylamides, ammonium persulfate, potassium peroxydisulfate；Relatively
In the cross-linker divinylbenzene of monomer mass 2%, diethylene glycol diacrylate, triethylene glycol diacrylate；And phase
For the polyethylene of dispersing agent pyrrolidones of monomer mass 15%；In being added to the ethanol/water mixed solution of volume fraction 22%,
Stir, be passed through nitrogen 32min, then react 8h in 70 DEG C of oil bath pan；Reaction is divided respectively after terminating with water and ethanol
Centrifugation 4 times is dissipated, submicron order second polymer microballoon is obtained.
Polymer microballoon is coated with step：By obtained first polymer microballoon and second polymer microballoon according to 0.5:0.5
Mass ratio mixing, in being scattered in ethanol/water mixed solution, polymer microballoon and ethanol/water mixed solution solid-liquid ratio are 1:
1.1, the ammoniacal liquor of the volume of ethanol/water mixed solution 1/240 is added, it is stirring evenly and then adding into positive silicic acid second isopyknic with ammoniacal liquor
Ester, 22 DEG C of reaction 25h, reaction is centrifuged 4 times respectively after terminating with water and ethanol dispersion, obtains carrying silicon microballoon.
Carry silicon microballoon modification step：Silane coupler is added in absolute ethyl alcohol, the volume of silane coupler and ethanol
Than 1:100；Load silicon microballoon is stirring evenly and then adding into, it is 0.8 to carry silicon microballoon with the solid-liquid ratio of absolute ethyl alcohol:10；20 DEG C of temperature
Under the conditions of stir 3h, obtain hydrophobic silane be coupled carry silicon microballoon.
Embodiment 6
A kind of preparation method of water-oil separating copper mesh, comprises the following steps：
Preparatory stage：Copper mesh is cleaned successively with acetone, ethanol and deionized water, removes the inorganic dust of copper mesh surface attachment
And organic matter, after having cleaned, it is put into dried for standby in 100 DEG C of baking oven.
The preparation of two-component adhesive：By amion-terminated polyurethane and epoxy resin according to 0.8：1.1 ratio mixing, then
With acetone blending, amion-terminated polyurethane/epoxy resin two-component adhesive that concentration is 0.005g/mL is obtained.
Copper mesh is sprayed：Amion-terminated polyurethane/epoxy resin two-component adhesive is sprayed on copper mesh, then by embodiment 1
The load silicon microballoon of preparation to be sprayed to and obtain water-oil separating copper mesh on copper mesh.
Embodiment 7
A kind of preparation method of water-oil separating copper mesh, comprises the following steps：
Preparatory stage：Copper mesh is cleaned successively with acetone, ethanol and deionized water, removes the inorganic dust of copper mesh surface attachment
And organic matter, after having cleaned, it is put into dried for standby in 102 DEG C of baking oven.
The preparation of two-component adhesive：By amion-terminated polyurethane and epoxy resin according to 1.2：0.9 ratio mixing, then
With acetone blending, amion-terminated polyurethane/epoxy resin two-component adhesive that concentration is 0.006g/mL is obtained.
Copper mesh is sprayed：Amion-terminated polyurethane/epoxy resin two-component adhesive is sprayed on copper mesh, then by embodiment 3
The load silicon microballoon of preparation to be sprayed to and obtain water-oil separating copper mesh on copper mesh.
Embodiment 8
A kind of preparation method of water-oil separating copper mesh, comprises the following steps：
Preparatory stage：Copper mesh is cleaned successively with acetone, ethanol and deionized water, removes the inorganic dust of copper mesh surface attachment
And organic matter, after having cleaned, it is put into dried for standby in 104 DEG C of baking oven.
The preparation of two-component adhesive：By amion-terminated polyurethane and epoxy resin according to 0.8：0.9 ratio mixing, then
With acetone blending, amion-terminated polyurethane/epoxy resin two-component adhesive that concentration is 0.01g/mL is obtained.
Copper mesh is sprayed：Amion-terminated polyurethane/epoxy resin two-component adhesive is sprayed on copper mesh, then by embodiment 2
The load silicon microballoon of preparation to be sprayed to and obtain water-oil separating copper mesh on copper mesh.
Embodiment 9
A kind of preparation method of water-oil separating copper mesh, comprises the following steps：
Preparatory stage：Copper mesh is cleaned successively with acetone, ethanol and deionized water, removes the inorganic dust of copper mesh surface attachment
And organic matter, after having cleaned, it is put into dried for standby in 103 DEG C of baking oven.
The preparation of two-component adhesive：By amion-terminated polyurethane and epoxy resin according to 1.2：1.1 ratio mixing, then
With acetone blending, amion-terminated polyurethane/epoxy resin two-component adhesive that concentration is 0.007g/mL is obtained.
Copper mesh is sprayed：Amion-terminated polyurethane/epoxy resin two-component adhesive is sprayed on copper mesh, then by embodiment 4
The load silicon microballoon of preparation to be sprayed to and obtain water-oil separating copper mesh on copper mesh.
Comparative example 1
200 mesh brass screens (size is 3cm × 3cm) are used into respectively 1molL‐1Watery hydrochloric acid, absolute ethyl alcohol and deionized water
It is cleaned by ultrasonic 10min or so, and is dried up with nitrogen standby；Prepare 2molL‐1Copper-bath and 1molL‐1Thiosulfuric acid
Sodium solution, in terms of volume parts, takes respectively 5 parts of copper-baths and the mixing of 10 parts of hypo solutions, and with 85 parts go from
Sub- water dilution is obtained chemical sinking effusion；The 200 mesh brass screens for cleaning are placed in 50 DEG C of deposition liquid；After 30min, by copper mesh
Deionized water cleaning is taken out, is dried, finally dry copper mesh is immersed in into hydroxy-end capped dimethyl silicone polymer and methyl
2h in the mixed solution of the n-hexane of tributanoximo silane curing agent, takes out and obtains final product for profit after heating 4h at 60 DEG C
The copper mesh of detached super-hydrophobic/super-oleophilic.Wherein, hydroxy-end capped dimethyl silicone polymer molecular weight is 3000, molten mixing
Mass fraction in liquid is 1%；The quality of methyl tributanoximo silane curing agent is hydroxy-end capped dimethyl silicone polymer
The 15% of quality.
Comparative example 2
(1) will be cleaned by ultrasonic in the copper mesh immersion absolute ethyl alcohol of 200 mesh, normal temperature dries；
(2) by E-44 type epoxy resin (6101), diluent, (toluene/acetone volume ratio is 2:1), nano-silica powder
Last (40～60 nanometers of particle diameter) presses 1 with curing agent T-31:20:6:0.5 ratio mixing, ultrasound is dispersed；
(3) fabric web is immersed in the mixed liquor that step (2) is obtained, solidification is dried at room temperature in taking-up, that is, had
The super-hydrophobic oil-water separation mesh film with super oleophylic function.
Comparative example 3
Super-hydrophobic mesh structural porous film is prepared in accordance with the following steps：
1st step：Mesh structural porous Cu films are prepared using bubble hydrogen template
The mesh structural porous Cu films of bubble hydrogen template electro-deposition are with platinized platinum (1cm2) make anode, copper mesh is adopted to electrode
(300 μm of aperture, area 3*3cm2) it is negative electrode.The pre-treatment of copper mesh is rinsed including polishing, oil removing, acid etch, water in experiment,
Soaked in absolute ethyl alcohol, acetone cleaning, low temperature air blast drying.Plating solution consists of the CuSO of 0.2mol/L4And 1molL-1H2SO4,
PH is controlled in the range of 4.0 ± 0.5, and the current density of electro-deposition is 3Acm-2, sedimentation time is 10s.It is post-depositional netted
Film should immediately use distilled water flushing, be dried after soaked in absolute ethyl alcohol, obtain mesh structural porous Cu films.
2nd step：The surface of mesh structural porous Cu films is modified
Above-mentioned mesh structural porous Cu films leaching is placed in into 200 DEG C of oxidation 5h in electric furnace.Reticulated film immersion after oxidation
In ethanol solution containing 3mmol/L n- dodecyl mereaptans and 1mmol/L tetradecylic acids, in being placed in 50 DEG C of drying boxes, take out after 1h, use
A large amount of deionized water rinsings dry, and obtain super-hydrophobic mesh structural porous thin-film network.
Experimental example
By the water-oil separating copper mesh obtained by testing example 8 and copper mesh obtained in comparative example 1-3 is in deionized water
With n-hexane as medium static contact angle.Test result such as table 1.
The contact angle test result of table 1
As seen from Table 1, the super-hydrophobic water-oil separating copper mesh for being prepared by embodiment 8, in air, in super-hydrophobic profit point
From with 5 μ L deionized waters are added on copper mesh, the static contact angle of the actually measured super-hydrophobic water-oil separating copper mesh is 163 ° (such as schemes
1), static contact angle of the static contact angle of super-hydrophobic water-oil separating copper mesh prepared by embodiment 8 more than comparative example 1-3.It is right
It is bigger in the static contact angle of water, illustrate that the hydrophobicity of material is better.So may determine that from experimental result, prepared by embodiment 8
Super-hydrophobic water-oil separating copper mesh hydrophobic performance it is more prominent.In general greasy dirt, containing compositions such as n-hexanes, by testing just
The static contact angle of hexane, it is found that super-hydrophobic water-oil separating copper mesh contact angle prepared by embodiment 8 is 0, less than comparative example 1-3
The copper mesh of preparation.The static contact angle of n-hexane is less, illustrates greasy dirt etc. more easily by copper mesh.As can be seen that embodiment 8
More preferably, greasy dirt handling capacity is higher, so super-hydrophobic water-oil separating for super-hydrophobic water-oil separating prepared by method copper mesh hydrophobicity
Greasy dirt separating power with copper mesh is higher.Secondly the load for preparing the super-hydrophobic water-oil separating copper mesh of embodiment 8 is also illustrated
The excellent performance of silicon microballoon, as shown in Fig. 2 the load silicon microsphere particle size prepared in embodiment 8 is uniform, full grains are consistent, favorably
In the super-hydrophobic water-oil separating copper mesh that forming properties are excellent.
In sum, the load silicon microballoon of the embodiment of the present invention and water-oil separating copper mesh manufacture craft；The load silicon microballoon
Preparation process is simple, the load silicon microsphere particle size of preparation is uniform, excellent performance, beneficial to dispersion；The water-oil separating makes work with copper mesh
Skill can reach by simple spraying it is anticipated that and the hydrophobicity of the water-oil separating copper mesh of the method preparation is more good, energy
Meet the needs of production.
Embodiments described above is a part of embodiment of the invention, rather than the embodiment of whole.The reality of the present invention
The detailed description for applying example is not intended to limit the scope of claimed invention, but is merely representative of the selected enforcement of the present invention
Example.Based on the embodiment in the present invention, what those of ordinary skill in the art were obtained under the premise of creative work is not made
Every other embodiment, belongs to the scope of protection of the invention.
Claims (10)
1. it is a kind of carry silicon microballoon preparation method, it is characterised in that it comprises the steps：Polymer microballoon preparation process：Will
Polymer monomer, initiator, dispersant and crosslinking agent are added in ethanol/water mixed solution, and polymer microballoon is obtained, and are passed through nitrogen
Gas 25-35min, then 70-75 DEG C of oil bath reaction 6-10h, reaction is centrifuged 2-5 time respectively after terminating with water and ethanol dispersion；
Polymer microballoon is coated with step：The obtained polymer microballoon is scattered in ethanol/water mixed solution, the polymerization
Thing microballoon is 1 with the ethanol/water mixed solution solid-liquid ratio:0.9-1.2, adds the ammoniacal liquor of cumulative volume 1/200-1/240, stirring
Uniform rear addition and the isopyknic tetraethyl orthosilicate of ammoniacal liquor, 18-24 DEG C of reaction 22-26h, reaction uses respectively water and ethanol after terminating
Dispersion centrifugation 2-5 time, obtains carrying silicon microballoon；
Carry silicon microballoon modification step：Silane coupler is added in absolute ethyl alcohol, the load silicon microballoon is stirring evenly and then adding into,
Centrifugation after 1-4h is stirred under 18-24 DEG C of temperature conditionss, 50-70 DEG C of condition is dried, obtain hydrophobic silane and be coupled load silicon
Microballoon.
2. it is according to claim 1 carry silicon microballoon preparation method, it is characterised in for preparing the polymer microballoon gather
Monomer adduct includes styrene, methyl methacrylate, EMA, isobornyl methacrylate, metering system
Acid butyl ester, lauryl methacrylate, Isobutyl methacrylate, isodecyl methacrylate, EHMA, third
E pioic acid methyl ester, ethyl acrylate, isobornyl acrylate, butyl acrylate, lauryl acrylate, isobutyl acrylate, propylene
At least one of sour isodecyl ester or Isooctyl acrylate monomer, the quality of the polymer monomer accounts for the 5%-10% of reaction system.
3. it is according to claim 1 carry silicon microballoon preparation method, it is characterised in that the polymer microballoon preparation process
The polymer microballoon of preparation includes first polymer microballoon and second polymer microballoon, and the particle diameter of the first polymer microballoon is
0.2～1.0 μm, the particle diameter of the second polymer microballoon is 20-200nm；The initiator includes the first initiator and second
Initiator；Preparing first initiator of the first polymer microballoon includes azodiisobutyronitrile, ABVN, mistake
At least one of BP, TBHP, peroxidized t-butyl perbenzoate, the quality of first initiator is accounted for
The 1%-3% of the monomer mass.
4. it is according to claim 3 carry silicon microballoon preparation method, it is characterised in that prepare the second polymer microballoon
Second initiator include azo dicyano valeric acid, the isobutyl imidazoline hydrochloride of azo two, azo diisobutyl amidine hydrochloric acid
Salt, the N- hydroxyisobutyl amidine hydrates of azo two, the N of azo two, N ' cyclobutyl isobutyl amidine hydrate, azo dimethyl N-2- hydroxyls
At least one of butylacrylamide, ammonium persulfate, potassium peroxydisulfate, the quality of second initiator accounts for the monomer mass
1%-3%.
5. it is according to claim 1 carry silicon microballoon preparation method, it is characterised in that the polymer microballoon preparation process
In the crosslinking agent include divinylbenzene, diethylene glycol diacrylate, triethylene glycol diacrylate, polyethylene glycol two
Acrylate, propylene glycol diacrylate, tri (propylene glycol) diacrylate, BDO diacrylate, 1,6 oneself
Omega-diol diacrylate, neopentylglycol diacrylate, 2 (the third oxidation) neopentylglycol diacrylates, ethoxylated bisphenol A dipropyls
Olefin(e) acid ester, (ethyoxyl) bisphenol fluorene diacrylate, 6 (ethyoxyl) bisphenol fluorene diacrylates, tricyclic decane dimethanol dipropyl
At least one of olefin(e) acid ester, the quality of the crosslinking agent accounts for the 1%-3% of the monomer mass.
6. it is according to claim 1 carry silicon microballoon preparation method, it is characterised in that the polymer microballoon preparation process
In the dispersant be polyvinylpyrrolidone.
7. it is according to claim 3 carry silicon microballoon preparation method, it is characterised in that polymer microballoon coating step in plus
The load silicon microballoon for entering is made up of the first polymer microballoon and the second polymer microballoon, and the first polymer is micro-
Ball and the second polymer microballoon are 0.4/0.6～0.6/0.4 compositions according to mass ratio.
8. it is according to claim 1 carry silicon microballoon preparation method, it is characterised in that the load silicon microballoon modification step
In, the silane coupler is 0.5/100～1/100 with the volume ratio of the absolute ethyl alcohol, described to carry silicon microballoon and anhydrous second
The solid-liquid ratio of alcohol is 0.8-1.1:10.
9. a kind of preparation method of water-oil separating copper mesh, it is characterised in that by amion-terminated polyurethane/epoxy resin two component
Stick is sprayed on copper mesh, obtains the first copper mesh；Again by using the preparation method that silicon microballoon is carried described in any one of claim 1-8
The obtained load silicon microballoon is sprayed at first copper mesh, obtains the water-oil separating copper mesh.
10. preparation method according to claim 9, it is characterised in that by amion-terminated polyurethane and epoxy resin according to
0.8-1.2：The ratio mixing of 0.9-1.1, is then blended with acetone, obtains the end amido that concentration is 0.005-0.1g/mL
Polyurethane/epoxy resin double-component adhesive.
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| CN109659550A (en) * | 2019-01-21 | 2019-04-19 | 浙江理工大学 | A kind of flower-shaped C SnS of tree peony2The preparation method of lithium cell cathode material |
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| CN114369190A (en) * | 2022-01-24 | 2022-04-19 | 西南石油大学 | Preparation method of high-elasticity super-hydrophobic polystyrene porous material |
| CN114369190B (en) * | 2022-01-24 | 2023-09-22 | 西南石油大学 | Preparation method of high-elasticity super-hydrophobic polystyrene porous material |
| CN115155471A (en) * | 2022-05-20 | 2022-10-11 | 大连理工大学 | Method for immobilizing micro-nano structure microspheres by spraying method |
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