CN105778642A - Rare-earth super-hydrophobic coating capable of keeping fluorescence stability in aqueous solution and preparation method of rare-earth super-hydrophobic coating - Google Patents
Rare-earth super-hydrophobic coating capable of keeping fluorescence stability in aqueous solution and preparation method of rare-earth super-hydrophobic coating Download PDFInfo
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- C09D127/12—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 a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
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Abstract
The invention discloses rare-earth super-hydrophobic coating capable of keeping fluorescence stability in an aqueous solution and a preparation method of the rare-earth super-hydrophobic coating. The preparation method includes the steps of firstly, using a seeded emulsion polymerization method to prepare core-shell nanoparticles with carboxylic on the surface; secondly, dispersing the core-shell nanoparticles in an organic solvent, and then allowing the dispersed core-shell nanoparticles to have complexing reaction with small-molecule ligands and a rare-earth compound to obtain complexing composite nanoparticles; thirdly, evenly dispersing the obtained complexing composite nanoparticles and low-surface-energy polymer particles, then coating on a certain matrix to obtain the super-hydrophobic coating with the micro-nano structure after the solvent volatilizes. The preparation method has the advantages that the rare-earth super-hydrophobic coating prepared by the method can solve the problem that rare-earth materials are prone to quenching when meeting water, the fluorescence strength of the rare-earth super-hydrophobic coating in purified water or the aqueous solution can be kept unchanged, the method is simple, economical and environmentally friendly, and the rare-earth super-hydrophobic coating is promising in application prospect in fields such as fluorescent display equipment and solar cells.
Description
Technical field
The invention belongs to rare-earth fluorescent, super hydrophobic coating field, rare earth super-hydrophobic coat being specifically related to fluorescent stabilization in a kind of aqueous solution and preparation method thereof.
Background technology
By the Folium Nelumbinis to nature, rice research finds, micron and the consequent super hydrophobic surface that organically combines of nanostructured that its surface exists have the contact angle of more than 150 ° and the roll angle less than 10 °, thus giving super hydrophobic surface self-cleaning performance, simultaneously super hydrophobic surface makes it have a extensive future in microfluid system and bio-compatible due to the wettability that surface is special.
Rare earth material is due to its special 4f electron transition, at optics, electricity, magnetic property.But owing to rare earth material is generally inorganic salt, meeting water unstable, biocompatibility is bad and makes application be limited.Therefore, in conjunction with super-hydrophobic and rare earth material excellent properties, there is very big researching value.
In the preparation method that presently, there are, needing post processing to modify low-surface energy substance, or be polymerized in substrate, process is loaded down with trivial details, and the scope of application is little.And have not yet to see the rare earth super-hydrophobic coat that the present invention relates to and soak the report that fluorescence is affected aspect in aqueous.
Summary of the invention
The present invention provides a kind of rare earth super-hydrophobic coat and preparation method thereof.The super-hydrophobic coat prepared by the design of nano-micro structure can be soaked in aqueous and still keep fluorescence and superhydrophobic property, and super-hydrophobic coat preparation method is simple, without complicated technology, economic and environment-friendly, can be mass-produced, it is adaptable to moist, the multiple occasion of display etc. under water.
Technical scheme:
The preparation method of the rare earth super-hydrophobic coat of fluorescent stabilization in a kind of aqueous solution, step is as follows:
Step 1: it is the 50 carboxylic core-shell nanos in 300nm surface that seed emulsion polymerization prepares particle diameter；
Step 2: core-shell nano step 1 obtained disperses in organic solvent, adds smaller ligand and rare earth compound complexation reaction obtains the coordination composite nanoparticle suspension that solid content is 1 20%；Core-shell nano: smaller ligand: the mass ratio 1:0.5 5:0.1 5 of rare earth compound；
Step 3: be coat in substrate after 1-45% is scattered in organic solvent according to solid content by the coordination composite nanoparticle obtained and low-surface-energy polymer particles, after solvent volatilization, the super-hydrophobic coat of the micro-nano structure obtained；Coordination composite nanoparticle and micron order low-surface energy substance microspheres quality are than for 1:1-10.
Described smaller ligand be organic acid R-COOH, Phen, oxine, acetylacetone,2,4-pentanedione, benzoyl acetone, α-thenoyltrifluoroacetone, benzoyltrifluoroacetone, 2,2 '-bipyridyl, 2,2 ': 6 '; 2 " one or more mixing in-terpyridyl, TOPO, tributyl phosphate, hexaoxacyclooctadecane-6-6,15-crown ether-5, wherein R is C1To C18Halo or the fat group of non-halo or aromatic group.
Described rare earth compound is containing europium, terbium, lanthanum, samarium, gadolinium, dysprosium, holmium, erbium, thulium, one or more mixing in the nitrate of cerium, ytterbium or lutecium, chlorate.
Described organic solvent is one or more mixing in aliphatic hydrocarbon, aromatic hydrocarbon, chlorohydrocarbon, alkylol, alkyl ketone, oxolane dimethyl sulfoxide, N,N-dimethylformamide, DMAC N,N' dimethyl acetamide, N-Methyl pyrrolidone.
Described low-surface-energy polymer particles is one or more mixing in Kynoar, politef, polysiloxanes, polytrifluorochloroethylene, and its particle diameter is 0.05 100 μm.
The mode of described coating is casting, brushes or spin coating.
Described base material is glass, quartz, marble, pottery or timber.
Beneficial effects of the present invention: the present invention prepares rare-earth fluorescent super-hydrophobic coat and can apply under relatively harsh conditions, namely coating remains to keep its fluorescent emission and super hydrophilic-super hydrophobic performance in humidity, pure water or aqueous solution such as sodium-chloride water solution, sodium nitrate aqueous solution etc..Rare-earth fluorescent super-hydrophobic coat preparation method of the present invention is simple, it is possible to convenient and different rare earth ions coordination, and technique is simple, is suitable for large-scale production.
Detailed description of the invention
Below in conjunction with embodiment, the present invention will be described in more detail.
Embodiment 1
Taking particle diameter is 100nm, shell is dispersed in alcoholic solution containing polyacrylic core-shell nano and obtains the solution that solid content is 1%, then taking this solution a certain amount of makes its quality comprising emulsion particle be 0.02g, by itself and 0.005g acetylacetone,2,4-pentanedione, 0.005g Phen, 0.01g europium chloride magnetic agitation obtained mixture after 3 hours.Take a certain amount of mixture, and mixture and polytetrafluoroethylene powder that particle diameter is 8 μm are cast than after disperseing for 1:5 film on the glass sheet according to solid masses.After solvent volatilizees, measure contact angle, and coating is put into immersion in sodium-chloride water solution, measure the contact angle change of 12 hours, observe fluorescence with ultraviolet photometer simultaneously.
Coating contact angle is all higher than 150 °, soaks through water and inorganic salt solution and still has fluorescence and super-hydrophobicity.
Embodiment 2
Taking particle diameter is 100nm, shell is dispersed in methanol solution containing polyacrylic core-shell nano and obtains the solution that solid content is 3%, then taking this solution a certain amount of makes its quality comprising emulsion particle be 0.01g, by itself and 0.005g acetylacetone,2,4-pentanedione, 0.02g M-phthalic acid, 0.01g Terbium nitrate (Tb(NO3)3) magnetic agitation obtained mixture after 3 hours.Take a certain amount of mixture, and mixture and politef microsphere that particle diameter is 5 μm are cast than after disperseing for 1:10 film on the glass sheet according to solid masses.After solvent volatilizees, measure contact angle, and coating is put into immersion in sodium nitrate aqueous solution, measure the contact angle change of 24 hours, observe fluorescence with ultraviolet photometer simultaneously.
Coating contact angle is all higher than 150 °, soaks through water and inorganic salt solution and still has fluorescence and super-hydrophobicity.
Embodiment 3
Taking particle diameter is 100nm, shell is dispersed in chlorohydrocarbon solution containing polyacrylic core-shell nano and obtains the solution that solid content is 2%, then taking this solution a certain amount of makes its quality comprising emulsion particle be 0.04g, by itself and 0.02g salicylic acid, 0.02g Phen, 0.03g holmium nitrate magnetic agitation obtained mixture after 3 hours.Take a certain amount of mixture, and mixture and Kynoar microsphere that particle diameter is 10 μm are cast than after disperseing for 1:10 film on the glass sheet according to solid masses.After solvent volatilizees, measure contact angle, and coating is put into immersion in pure water solution, measure the contact angle change of 48 hours, observe fluorescence with ultraviolet photometer simultaneously.
Embodiment 4
Taking particle diameter is 150nm, shell is dispersed in alcoholic solution containing polyacrylic core-shell nano and obtains the solution that solid content is 4%, then taking this solution a certain amount of makes its quality comprising emulsion particle be 0.05g, by itself and 0.01g acetylacetone,2,4-pentanedione, 0.03g M-phthalic acid, 0.02g Lanthanum (III) nitrate magnetic agitation obtained mixture after 3 hours.Take a certain amount of mixture, and mixture and polysiloxanes microsphere that particle diameter is 20 μm are cast than after disperseing for 1:5 film on the glass sheet according to solid masses.After solvent volatilizees, measure contact angle, and coating is put into immersion in sodium-chloride water solution, measure the contact angle change of 48 hours, observe fluorescence with ultraviolet photometer simultaneously.
Coating contact angle is all higher than 150 °, soaks through water and inorganic salt solution and still has fluorescence and super-hydrophobicity.
Embodiment 5
Taking particle diameter is 150nm, shell is dispersed in alcoholic solution containing polyacrylic core-shell nano and obtains the solution that solid content is 5%, then taking this solution a certain amount of makes its quality comprising emulsion particle be 0.01g, by itself and 0.02g salicylic acid, 0.015g Phen, 0.03g lutecium nitrate magnetic agitation obtained mixture after 3 hours.Take a certain amount of mixture, and mixture and polytrifluorochloroethylene microsphere that particle diameter is 15 μm are cast than after disperseing for 1:5 film on the glass sheet according to solid masses.After solvent volatilizees, measure contact angle, and coating is put into immersion in sodium nitrate aqueous solution, measure the contact angle change of 48 hours, observe fluorescence with ultraviolet photometer simultaneously.
Coating contact angle is all higher than 150 °, soaks through water and inorganic salt solution and still has fluorescence and super-hydrophobicity.
Above-described embodiment is embodiment of the present invention, but embodiments of the present invention being not restricted by the embodiments, other are any without departing from the change made under principles of the invention and spirit, are included in protection scope of the present invention.
Claims (10)
1. the preparation method of the rare earth super-hydrophobic coat of fluorescent stabilization in an aqueous solution, it is characterised in that step is as follows:
Step 1: it is the 50 carboxylic core-shell nanos in 300nm surface that seed emulsion polymerization prepares particle diameter；
Step 2: core-shell nano step 1 obtained disperses in organic solvent, adds smaller ligand and rare earth compound complexation reaction obtains the coordination composite nanoparticle suspension that solid content is 1-20%；Core-shell nano: smaller ligand: the mass ratio 1:0.1-5:0.1-10 of rare earth compound；
Step 3: be coat in substrate after 1-45% is scattered in organic solvent according to solid content by the coordination composite nanoparticle obtained and low-surface-energy polymer particles, after solvent volatilization, the super-hydrophobic coat of the micro-nano structure obtained；Coordination composite nanoparticle and low-surface energy substance polymer particles mass ratio are 1:1-10.
2. described preparation method according to claim 1, it is characterized in that, described smaller ligand be organic acid R-COOH, Phen, oxine, acetylacetone,2,4-pentanedione, benzoyl acetone, α-thenoyltrifluoroacetone, benzoyltrifluoroacetone, 2,2 '-bipyridyl, 2,2 ': 6 '; 2 " one or more mixing in-terpyridyl, TOPO, tributyl phosphate, hexaoxacyclooctadecane-6-6,15-crown ether-5, wherein R is C1To C18Halo or the fat group of non-halo or aromatic group.
3. described preparation method according to claim 1 and 2, it is characterised in that described rare earth compound is containing europium, terbium, lanthanum, samarium, gadolinium, dysprosium, holmium, erbium, thulium, one or more mixing in the nitrate of cerium, ytterbium or lutecium, chlorate.
4. described preparation method according to claim 1 and 2, it is characterized in that, described low-surface-energy polymer particles is one or more mixing in Kynoar, politef, polysiloxanes, polytrifluorochloroethylene, and its particle diameter is 0.05 100 μm.
5. described preparation method according to claim 3, it is characterized in that, described low-surface-energy polymer particles is one or more mixing in Kynoar, politef, polysiloxanes, polytrifluorochloroethylene, and its particle diameter is 0.05 100 μm.
6. the preparation method described according to claim 1,2 or 5, it is characterized in that, described organic solvent is aliphatic hydrocarbon, aromatic hydrocarbon, chlorohydrocarbon, alkylol, alkyl ketone, oxolane, dimethyl sulfoxide, N, one or more mixing in dinethylformamide, N,N-dimethylacetamide, N-Methyl pyrrolidone.
7. described preparation method according to claim 3, it is characterized in that, described organic solvent is aliphatic hydrocarbon, aromatic hydrocarbon, chlorohydrocarbon, alkylol, alkyl ketone, oxolane, dimethyl sulfoxide, N, one or more mixing in dinethylformamide, N,N-dimethylacetamide, N-Methyl pyrrolidone.
8. described preparation method according to claim 4, it is characterized in that, described organic solvent is aliphatic hydrocarbon, aromatic hydrocarbon, chlorohydrocarbon, alkylol, alkyl ketone, oxolane, dimethyl sulfoxide, N, one or more mixing in dinethylformamide, N,N-dimethylacetamide, N-Methyl pyrrolidone.
9. the preparation method described according to claim 1,2,5,7 or 8, it is characterised in that the mode of described coating includes casting, brushes or spin coating；Described base material is glass, quartz, marble, pottery or timber.
10. described preparation method according to claim 6, it is characterised in that the mode of described coating includes casting, brushes or spin coating；Described base material is glass, quartz, marble, pottery or timber.
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| CN108359344A (en) * | 2018-01-19 | 2018-08-03 | 大连理工大学 | A kind of preparation method of high hydrophobicity high temperature resistant fluoresent coating |
| CN108409911A (en) * | 2018-01-19 | 2018-08-17 | 大连理工大学 | A kind of preparation method of super-hydrophobicity automatically cleaning fluoresent coating |
| CN110603299A (en) * | 2017-05-20 | 2019-12-20 | 霍尼韦尔国际公司 | MILK LUMILUX Dispersion |
| CN111909385A (en) * | 2020-07-10 | 2020-11-10 | 浙江工业大学 | Rare earth supermolecule gel luminescent material, and preparation method and application thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110603299A (en) * | 2017-05-20 | 2019-12-20 | 霍尼韦尔国际公司 | MILK LUMILUX Dispersion |
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| CN108409911A (en) * | 2018-01-19 | 2018-08-17 | 大连理工大学 | A kind of preparation method of super-hydrophobicity automatically cleaning fluoresent coating |
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| CN111909385A (en) * | 2020-07-10 | 2020-11-10 | 浙江工业大学 | Rare earth supermolecule gel luminescent material, and preparation method and application thereof |
| CN111909385B (en) * | 2020-07-10 | 2022-04-08 | 浙江工业大学 | Rare earth supermolecule gel luminescent material, and preparation method and application thereof |
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