CN103436111B - A kind of preparation method of the water-based ultraviolet shielded coating based on ZnO quantum dot - Google Patents
A kind of preparation method of the water-based ultraviolet shielded coating based on ZnO quantum dot Download PDFInfo
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Abstract
The invention belongs to Field of Fine Chemicals, is related to a kind of method that water-based ultraviolet shielded coating is prepared using ZnO quantum dot.I.e., zinc salt and lithium hydroxide ethanol solution are first subjected to solgel reaction and prepare ZnO quantum dot, again using tetraethyl orthosilicate as raw material, layer of silicon dioxide is coated in the surface in situ of ZnO quantum dot, obtains the ZnO quantum dot@SiO that photocatalytic activity is effectively suppressed2Nuclear shell type nano meter particle.Then by ZnO quantum dot@SiO2Nano-particle is transferred in water, then compound with aqueous film-forming resin and wetting agent, and water-based ultraviolet shielded coating is made.ZnO quantum dot@SiO2Content in dry coating is 1 50%, by adjusting coating thickness and ZnO quantum dot@SiO2Content realize the full-shield of the following ultraviolet of 340nm wavelength.The ultraviolet shielded coating aqueous, environmental protective, nontoxic of the present invention, available for outdoor bamboo and wood, plastics etc., can also prepare transparent ultraviolet shielded glass.
Description
Technical field
The invention belongs to technology of fine chemicals, and in particular to a kind of water-based ultraviolet shielded based on ZnO quantum dot
The preparation method of coating.
Background technology
Transparent ultraviolet shielded coating degradable material out of doors（Polymer, wood, bamboo etc.）Protection, ultraviolet shielded glass system
Standby, indoor light source ultraviolet isolation etc. has extensive use, is typically made by adding ultra-violet absorber in varnish
It is standby.Ultra-violet absorber can be generally divided into two major classes, and one kind is organic uv absorbers, mainly include Benzophenone class, benzo
Triazole type, salicylic acid esters, oxanilide class etc.；Another kind of is inorganic nano ultraviolet absorber, mainly there is nano titania
Particle, cerium oxide nanoparicles, zinc oxide nano-particle etc..The extinction coefficient of organic uv absorbers is big, shielding effect
Rate is high, shielding wide waveband, the advantages that transparency is good, but the shortcomings of light, heat endurance are poor, volatile, long-time stability be present
It is bad, moreover, organic uv absorbers catabolite has certain toxicity.Although inorganic nano ultraviolet absorber is with prominent
Light, heat endurance, but easily reunite, while realizing ultraviolet shielded, the transparency for easily causing coating declines；Meanwhile nothing
Machine nano-particle has very strong photocatalytic activity, in the presence of ultraviolet, can accelerate the aging and degraded of polymer coating,
Greatly reduce the service life of coating.Chinese patent CN1412258A reports to be ground by titanium dioxide or zinc oxide nano-powder
Mill is scattered, adds and ultraviolet resistant is prepared in polyacrylic resin.Because nano-powder can not possibly be reached completely by grinding
To primary particle diameter dispersion level, cause the transparent bad of coating.Chinese patent CN101629033A is surpassed with carboxymethyl cellulose
Sound auxiliary law is prepared for adulterating the cerium oxide nanoparicles of calcium, and coats reduction cerium oxide nanoparicles with inertia shell
Photocatalytic activity, then silane coupler modify, then with pure-acrylic emulsion is compound prepares ultraviolet shielded coating.But in this method, two
Cerium oxide nano particle is sintered, in the coating dispersed bad, and the transparency of coating is low.As can be seen here, high durable
Property, the preparation method of the ultraviolet shielded coating of the environment-friendly type of high transparency still urgently develop.
Zinc oxide quantum dot (ZnO QDs) ultraviolet absorption ability is strong, and fluorescent emission intensity is high, and with nontoxic excellent
Point, is usually used in biological fluorescent labelling material, is also the reason of high transparency ultraviolet screener coating inorganic nano ultraviolet absorber
Want to select.Such as, Li etc. is compound with fluoropolymer resin by ZnO QDs, be prepared for transparent ultraviolet shielded coating (S. Li, et al,Adv. Mater., 2007, 19, 4347).But ZnO QDs photocatalytic activity is not accounted in the research, and coating
System is solvent-borne type.By amphipathic nature polyalcohol and surfactant to ZnO QDs cladding (N. R. Jana, et al,Chem. Commun., 2007, 1406; H. M. Xiong, et al, J. Am. Chem. Soc., 2008, 130,
7522; X. Tang, et al, Langmuir, 2009,25,5271.), it can improve ZnO QDs water solubility, but by
In ZnO QDs photocatalytic activity, under the irradiation of ultraviolet light, these amphipathic nature polyalcohols and surfactant are easy to point
Solution, causes ZnO QDs unstabilitys, is not used to the preparation of the water-based ultraviolet shielded coating of high-weatherability, high transparency.
The content of the invention
It is an object of the invention to provide a kind of water-based ultraviolet screen that high-weatherability, high transparency are prepared based on ZnO QDs
Cover the method for coating.Specifically include following steps：
Zinc salt and lithium hydroxide are weighed respectively, and ultrasonication is completely dissolved in absolute ethyl alcohol, then by the second of the two
Alcoholic solution mixes, 60-78 DEG C of stirring reaction 3-10 h., obtain the dispersion liquids of ZnO QDs in ethanol.To ZnO QDs ethanol point
Tetraethyl orthosilicate and deionized water are added in dispersion liquid, ultrasound fully mixes, and 6 h of reaction is stirred at room temperature, you can obtain SiO2Cladding
ZnO QDs（ZnO QDs@SiO2）Dispersion liquid, by centrifuging, washing, by ZnO QDs@SiO2Transfer is dispersed in water,
Obtain ZnO QDs@SiO2Aqueous dispersions, then mixed by a certain percentage with aqueous film-forming resin, wetting agent, after being sufficiently stirred,
Produce water-based ultraviolet shielded coating.The coating can be coated on the substrate surfaces such as bamboo and wood, plastics, glass, and low temperature drying is handled, i.e.,
It can obtain transparent ultraviolet shielded coating.
Water-based ultraviolet shielded coating of the present invention based on ZnO QDs, it is characterised in that ZnO QDs particle diameter is 1-
10 nm.Particle diameter is too small, is not easy to prepare, crystallinity deterioration, and ultraviolet absorption ability weakens；Particle diameter is too big, light scattering effect enhancing,
It is unfavorable for preparing transparent ultraviolet shielded coating.
Water-based ultraviolet shielded coating of the present invention based on ZnO QDs, it is characterised in that zinc salt and lithium hydroxide
Mol ratio is 1:4-2:3, reaction temperature is 60-78 DEG C.Wherein zinc salt is in zinc nitrate, zinc sulfate, zinc chloride and zinc acetate
One kind, there is the advantages of cost is low, nontoxic.
Water-based ultraviolet shielded coating of the present invention based on ZnO QDs, it is characterised in that using SiO2Coat ZnO
QDs, can effectively suppress ZnO QDs photocatalytic activity, while can improve its dispersiveness in water, be advantageous to it in water-based painting
Application in material.SiO2Clad is prepared by tetraethyl orthosilicate in ZnO QDs dispersion liquid situs sol-gel process, wherein just
Silester presses Si after ZnO QDs preparations in 24 h:Zn mol ratios 1-3 is added.Tetraethyl orthosilicate addition is very few, is easily caused
ZnO QDs claddings are incomplete, and photocatalytic activity can not effectively be completely cut off, and addition is excessive, be easily caused ZnO QDs@SiO2Receive
Reunion between rice corpuscles, or even dispersion liquid system gel.The addition opportunity of tetraethyl orthosilicate, ZnO QDs were by Yin Aosi too late
Special Grindelwald is aged and particle diameter becomes big, is unfavorable for the preparation of transparent ultraviolet shielded coating.
Water-based ultraviolet shielded coating of the present invention based on ZnO QDs, it is characterised in that used waterborne film-forming
Resin is one kind in styrene-acrylic emulsion, pure-acrylic emulsion, silicone acrylic emulsion, waterborne polyurethane resin, water-based organic-inorganic hybrid resin
Or several mixture.
Water-based ultraviolet shielded coating of the present invention based on ZnO QDs, it is characterised in that used wetting agent is
DISPERBYK-2010、DISPERBYK-2015、Hydropalat 875、WET265、WET500、DISPERBYK-346、
The aqueous wetting agents such as DISPERBYK-349, BYK380N, BYK-381, EFKA3030, EFKA3034, EFKA3500, EFKA3570
In one or more of mixtures.
Water-based ultraviolet shielded coating of the present invention based on ZnO QDs, it is characterised in that ZnO QDs are in dry coating
In content range be 1-50%, preferably 2-30%, most preferably 5-20%.If ZnO QDs dosages are very few, ultraviolet shielded effect
Unobvious；If dosage is excessive, the transparency of coating starts to reduce.
The coating of gained of the invention can be coated on the substrate surfaces such as bamboo and wood, plastics, glass, and film is in wavelength 340 after drying
Below nm has efficient uv-shielding capacity, meanwhile, visible region have with pure resin coating similar in high transparency.Due to
ZnO QDs photocatalytic activity is effectively completely cut off, in film no longer to organic principle produce photocatalysis, film it is resistance to
Hou Xingjia, uv-shielding capacity are steady in a long-term.
Water-based ultraviolet shielded coating of the present invention based on ZnO QDs, advantage are：
（1）Water-based, environmentally friendly, ZnO QDs quantum dots ultraviolet absorbers itself are nontoxic, stably；（2）The raw material economics of use,
The equipment used is simple, and preparation method is easily operated；（3）Can full-shield wavelength 340 below nm ultraviolet, meanwhile, apply
Film can keep the high transparency similar to pure resin film；（4）ZnO QDs@SiO obtained by the present invention2Can greatly it weaken
ZnO QDs photocatalytic activity, the long-time stability of the uv-shielding capacity of film are good.
Method of testing：
(1) photocatalytic activity method of testing：By ZnO QDs and ZnO QDs@SiO2The rhodamine B aqueous solution is distributed to respectively
In (10 mg/L), in the case of stirring, after 150 W high voltage mercury lamp radiation different time, sample, centrifuge, test
The uv-visible absorption spectra of solution.
(2) uv-shielding capacity method of testing：Straight polymer coating and ultraviolet shielded coating are respectively overlay in containing Luo Dan
Bright B resin coated surface, it is placed in accelerated ageing instrument, after the aging different time, tests the resinous coat containing rhodamine B
Ultraviolet-visible transmitted spectrum.
(3) weatherability method of testing：Ultraviolet shielded painting is placed in accelerated ageing instrument, after the aging different time, surveyed
Try its ultraviolet-visible transmitted spectrum；Tester：The QUV/Se artificial accelerated aging instrument of Q-Panel companies of the U.S.；Test-strips
Part：The nm of wavelength 310, the W/m of radiant power 0.712；Cyclic program：Ultraviolet irradiation 4 h, 60 DEG C, condense 4 h, 50 DEG C.
Brief description of the drawings
Fig. 1 is embodiment 1（a）With comparative example 1（b）Middle nano-particle aqueous dispersions are outer under 365 nm ultra violet lamps
See.
Photocatalytic degradation curves of the Fig. 2 for nano-particle in embodiment 1 and comparative example 1 to rhodamine B（Absorbance（0）, inhale
Luminosity（t）When representing beginning respectively and after the t min that degrade, absorbance of the rhodamine B aqueous solution at 552 nm）.
Fig. 3 is pure third resinous coat（Neat PA）With the floating coat of embodiment 1（Thickness：350 μm）Ultraviolet-visible transmission
Spectrum.
Fig. 4 is embodiment 1（a）With comparative example 1（b）Floating coat（Thickness：65 μm）The forward and backward ultraviolet-visible of accelerated ageing
Transmitted spectrum.
Fig. 5 is the ultraviolet shielded coating in straight polymer coating and embodiment 1 respectively（Thickness：350 μm）Protection under,
The accelerated ageing degradation curve of rhodamine B in resinous coat（Absorbance（0）, absorbance（t）When representing starting respectively and accelerate old
After changing t min, absorbance of the coating containing rhodamine B at 552 nm）.
Embodiment
Embodiment 1：
（1）By 1 mmol LiOH.H2O is added in 50 mL ethanol, 30 min of ultrasound, it is fully dissolved.Add
0.25 mmol Zn(Ac)2.2H2O, 5 min of ultrasound, obtains clear transparent solutions.Then, the clear solution is heated to 70
DEG C, the h of stirring reaction 3, you can obtain ZnO QDs dispersion liquids.Added successively into the dispersion liquid 120 μ L tetraethyl orthosilicates and
400 μ L distilled water, the min of sonic oscillation 20, is then stirred at room temperature 6 h of reaction, obtains ZnO QDs@SiO immediately2Nano-particle
Dispersion liquid.200 mL n-hexanes are added into the dispersion liquid, centrifuges, is washed twice with 15 mL ethanol, and be dispersed in water.
The aqueous dispersions of the nano-particle can keep long-term transparent, stably（See Fig. 1 a）；And ZnO QDs are dispersed in water in comparative example 1
It is that appearance is reunited and deposited phenomenon after 10 min（See Fig. 1 b）, show ZnO QDs@SiO2Nano-particle has excellent moisture
Dissipate property.Meanwhile by ZnO QDs@SiO2Nano-particle is distributed in the rhodamine B aqueous solution, after lucifuge stirs 2 h, uses ultraviolet light
After irradiating 80 min, rhodamine degrades 20%（See Fig. 2）；And use in ZnO QDs comparative example 1, by ultraviolet light
After 80 min, 93% rhodamine B is degraded, and illustrates SiO2Shell can effectively completely cut off ZnO QDs photocatalytic activity.
（2）By step（1）The nano-particle aqueous dispersions of gained mix with 2 g pure-acrylic emulsions and 5 mg Hydropalat875
Close, 20 min of ultrasound, obtain water-based ultraviolet shielded coating.Quartz glass surfaces are then applied to, 30 DEG C of 48 h of drying, are prepared into
Thickness is respectively 350 μm and 65 μm of two kinds of ultraviolet shielded coatings（Ultraviolet-visible spectrum is shown in Fig. 3 and Fig. 4 respectively）.Thickness is 65
μm coating after the h of artificial accelerated aging 200, transparency has no any change（See Fig. 4 a）, show ultraviolet shielded coating
With good weatherability；And after the h of artificial accelerated aging 200, transparency has very big ultraviolet shielded coating in comparative example 1
Decline（See Fig. 4 b）, declaratives polymer coating degraded.
Embodiment 2：
By 0.4 mmol LiOH.H2O is added in 50 mL ethanol, 30 min of ultrasound, it is fully dissolved.Add 0.25
mmol Zn(Ac)2.2H2O, 5 min of ultrasound, obtains clear transparent solutions.Then, the clear solution is heated to 60 DEG C, stirring
React 10 h, you can obtain ZnO QDs dispersion liquids.120 μ L tetraethyl orthosilicates are added into the dispersion liquid successively and 300 μ L steam
Distilled water, the min of sonic oscillation 20, is then stirred at room temperature 6 h of reaction, obtains ZnO QDs@SiO immediately2The dispersion liquid of nano-particle.
200 mL n-hexanes are added into the dispersion liquid, centrifuges, is washed twice with 15 mL ethanol, and be dispersed in water.By receiving for gained
Rice corpuscles aqueous dispersions mix with 2 g pure-acrylic emulsions and 5 mg DISPERBYK-346,20 min of ultrasound, obtain water-based ultraviolet screen
Cover coating.Quartz glass surfaces are then applied to, 30 DEG C of 48 h of drying, obtain ultraviolet shielded coating.The thickness of the coating is 350
μm, the light transmittance at 300 nm is 4%, and the light transmittance at 550 nm is 88%, close to the transparent of pure acrylic resin coating
Degree（91%）, show that the coating has high transparency and ultraviolet shielded effect.
Embodiment 3：
By 1 mmol LiOH.H2O is added in 50 mL ethanol, 30 min of ultrasound, it is fully dissolved.Add 0.25
mmol Zn(Ac)2.2H2O, 5 min of ultrasound, obtains clear transparent solutions.Then, the clear solution is heated to 70 DEG C, stirring
3 h are reacted, obtain ZnO QDs dispersion liquids.120 μ L tetraethyl orthosilicates and 300 μ L distilled water are added into the dispersion liquid successively,
The min of sonic oscillation 20 immediately, 6 h of reaction are then stirred at room temperature, obtain ZnO QDs@SiO2The dispersion liquid of nano-particle.To this
200 mL n-hexanes are added in dispersion liquid, centrifuges, is washed twice with 15 mL ethanol, and be dispersed in water.By the nanoparticle of gained
Sub- aqueous dispersions mix with 2 g aqueous polyurethanes and 5 mg DISPERBYK-346,20 min of ultrasound, obtain water-based ultraviolet shielded
Coating.Quartz glass surfaces are then applied to, 30 DEG C of 48 h of drying, obtain ultraviolet shielded coating.The thickness of the coating is 300 μ
M, the light transmittance at 300 nm are 5%, and transmitance is 89% at 500 nm.
Comparative example 1：
By 1 mmol LiOH.H2O is added in 50 mL ethanol, 30 min of ultrasound, it is fully dissolved.Add 0.25
mmol Zn(Ac)2.2H2O, 5 min of ultrasound, obtains clear transparent solutions.Then, the clear solution is heated to 70 DEG C, stirring
3 h are reacted, obtain ZnO QDs dispersion liquids.200 mL n-hexanes are added into the dispersion liquid, centrifuges, two is washed with 15 mL ethanol
It is secondary, and be dispersed in water.By the dispersion liquid and 2 g pure-acrylic emulsions and 5 mg Hydropalat875 mixing, 20 min of ultrasound,
Quartz glass surfaces are coated to, 30 DEG C of 48 h of drying, obtain ultraviolet shielded coating, the thickness of coating is 65 μm.Ultraviolet-visible
Spectrum and artificial accelerated aging result are shown in Fig. 4 b.
Claims (4)
1. a kind of water-based ultraviolet shielded preparation method for coating based on ZnO quantum dot, it is characterised in that comprise the following steps：First
Sol gel reaction occurs in ethanol solution using zinc salt and lithium hydroxide and prepares ZnO quantum dot, then adds positive silicic acid second
Ester and water, layer of silicon dioxide is coated in ZnO quantum dot surface in situ using the hydrolysis-condensation reaction of tetraethyl orthosilicate, is made
ZnO QDs@SiO2Nano-particle；By ZnO QDs@SiO2Nano-particle transfer be dispersed in water, then with aqueous film-forming resin,
Wetting agent is sufficiently stirred mixing, that is, the water-based ultraviolet shielded coating based on ZnO quantum dot is made；
Wherein,
The particle diameter of ZnO quantum dot is 1-10 nm；
The SiO on ZnO QDs surfaces2It is coated in 24 h after prepared by ZnO QDs and carries out；
By Si:Zn mol ratios are that-polycondensation reaction is hydrolyzed in the metered tetraethyl orthosilicates of 1-3；
Aqueous film-forming resin is that styrene-acrylic emulsion, pure-acrylic emulsion, silicone acrylic emulsion, waterborne polyurethane resin and water-based organic and inorganic are miscellaneous
Change one or more of mixtures in resin；
Wetting agent be DISPERBYK-2010, DISPERBYK-2015, Hydropalat875, WET265, WET500,
DISPERBYK-346、DISPERBYK-349、BYK380N、BYK-381、EFKA3030、EFKA3034、EFKA3500、
One or more of mixtures in EFKA3570 aqueous wetting agents.
2. the water-based ultraviolet shielded preparation method for coating based on ZnO quantum dot as described in claim 1, it is characterised in that zinc salt
Amount ratio with the material of lithium hydroxide is 1:4-2:3, reaction temperature is 60-78 DEG C, and the reaction time is 3-10 h.
3. the water-based ultraviolet shielded preparation method for coating based on ZnO quantum dot as described in claim 1, it is characterised in that zinc salt
For one kind in zinc nitrate, zinc sulfate, zinc chloride or zinc acetate.
4. the water-based ultraviolet shielded preparation method for coating based on ZnO quantum dot as described in claim 1, it is characterised in that ZnO
Percentage compositions of the QDs in film is 1-50%, and wavelength is realized by the content for adjusting coating thickness or ZnO QDs nano-particles<
340 nm ultraviolet full-shield.
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| CN105694362B (en) * | 2014-11-27 | 2018-01-02 | 中国科学院化学研究所 | Light-shielding polymer nano composite material |
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| SG11201805448YA (en) * | 2015-12-24 | 2018-07-30 | Agency Science Tech & Res | A film coating |
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| CN107858828A (en) * | 2017-11-16 | 2018-03-30 | 查治刚 | Quantum material coating, its preparation method, quantum material coated cloth |
| CN111205578B (en) * | 2018-11-22 | 2022-11-08 | 深圳光启超材料技术有限公司 | Ultraviolet absorbing film and method for producing the same |
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| CN110563023A (en) * | 2019-09-23 | 2019-12-13 | 陕西科技大学 | high-fluorescence-brightness ZnO quantum dot and preparation method thereof |
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| CN114276699B (en) * | 2022-01-10 | 2022-08-12 | 广州柏为科技有限公司 | Surface modification method of nano ZnO and application of nano ZnO in sunscreen cosmetics |
| CN114736669B (en) * | 2022-05-10 | 2023-06-13 | 江南大学 | CMC-Na/CdS@ZnS flexible quantum dot film and preparation method thereof |
| CN114921168B (en) * | 2022-06-24 | 2023-04-28 | 中国铁道科学研究院集团有限公司金属及化学研究所 | Carbon-silicon nano material modified aqueous polyurethane emulsion, synthesis method and application thereof |
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| JP2009193991A (en) * | 2008-02-12 | 2009-08-27 | Murata Mfg Co Ltd | Zinc oxide quantum dot and its manufacturing method |
| CN102559171A (en) * | 2011-09-26 | 2012-07-11 | 吉首大学 | Method for preparing zinc oxide quantum dots capable of being dispersed in aqueous solution stably |
| CN102690520B (en) * | 2012-06-01 | 2014-05-14 | 苏州大学 | Transparent ZnO quantum dot/organic silicon nanocomposite material, and preparation method and application thereof |
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