CN110240192A - A kind of preparation method of the zinc oxide nanosphere of Superhydrophilic - Google Patents
A kind of preparation method of the zinc oxide nanosphere of Superhydrophilic Download PDFInfo
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- CN110240192A CN110240192A CN201910614628.3A CN201910614628A CN110240192A CN 110240192 A CN110240192 A CN 110240192A CN 201910614628 A CN201910614628 A CN 201910614628A CN 110240192 A CN110240192 A CN 110240192A
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- superhydrophilic
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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Abstract
The invention discloses a kind of preparation method of the zinc oxide nanosphere of Superhydrophilic, comprising steps of 1, Zinc diacetate dihydrate is dissolved in dehydrated alcohol, sealing stirring forms clear solution A；2, sodium hydroxide is dissolved in dehydrated alcohol, sealing stirring, forms clear solution B, and the solution A and the solution B are mixed to form solution C；3, trisodium citrate dihydrate is dissolved in distilled water or deionized water, is added in the solution C, form almost clear colloidal solution D；4, the solution D is placed in reaction kettle, then reaction kettle is heated, obtained product is centrifuged, is washed, alcohol is washed and is dried.Zinc oxide material produced by the present invention does not need just have Superhydrophilic under ultraviolet lighting, even if being protected from light after storage for a long time still has excellent wetability.
Description
Technical field
The present invention relates to a kind of preparation methods of zinc oxide nanosphere, more particularly to a kind of zinc oxide nano of Superhydrophilic
The preparation method of rice ball.
Background technique
Hydrophilic antifogging material, it is usually desirable to be in indoor, interior side for glass.Currently, for interior glass
Anti-fog method generallys use the modes such as blowing, electric heating, these modes may such as keep warm with other riding functions of automobile, make
Cold equal mutually conflict；And it combines electric heating wire and obviously increases the manufacture difficulty of vehicle glass.Although high molecular material compares appearance
The characteristics of being easy to do to Superhydrophilic, but being easy aging, limits its application as long-time durable goods.In contrast, metal
Oxide material, such as nontoxic zinc oxide (ZnO) material without the worry in terms of aging, thus are contemplated that it as antifog
Materials'use.
However, it is generally the case that hydrophily is presented under ultraviolet light in nano zinc oxide material, is being detached from ultraviolet lighting
After penetrating a period of time, surface can restore hydrophobicity.This is because zinc salts precipitate calcining is come under the alkaline case generallyd use
During preparing ZnO, it is nonpolar to will form exposureCrystal face, it is microcosmic be rodlike ZnO material, surface is hydrophobic
Property.Under ultraviolet light, these surfaces are likely to form hydroxyl, and then have temporary hydrophily.But it is indoors, interior
Occasion under, the ultraviolet band part of sunlight can be by glass barrier, thus cannot be used；If it is considered that additional ultraviolet lighting
Device, then certainly will increase the complexity of application.
Summary of the invention
For above-mentioned prior art defect, task of the invention lies in the zinc oxide nanospheres for providing a kind of Superhydrophilic
Preparation method makes zinc oxide material not need just have Superhydrophilic under ultraviolet lighting, it is super hydrophilic to solve zinc oxide material
The problem of property is influenced by ultraviolet lighting and influences the scope of application.
The technical scheme is that such: a kind of preparation method of the zinc oxide nanosphere of Superhydrophilic, comprising steps of
1, Zinc diacetate dihydrate is dissolved in dehydrated alcohol, sealing stirring forms clear solution A；2, sodium hydroxide is dissolved in anhydrous second
In alcohol, sealing stirring forms clear solution B, and the solution A and the solution B is mixed to form solution C；3, by two hydrations
Sodium citrate is dissolved in distilled water or deionized water, is added in the solution C, and almost clear colloidal solution D is formed；4, by institute
It states solution D to be placed in reaction kettle, then reaction kettle is heated, obtained product is centrifuged, is washed, alcohol is washed and is dried.
Further, the weight fraction ratio of Zinc diacetate dihydrate and dehydrated alcohol is 5 ︰, 1000~6 ︰ in the step 1
1000。
Further, the weight fraction ratio of sodium hydroxide and dehydrated alcohol is 9 ︰, 40000~11 ︰ in the step 2
40000。
Further, trisodium citrate dihydrate is dissolved in distilled water in the step 3 or the weight fraction ratio of deionized water is
9 ︰, 375~11 ︰ 375.
Further, by the solution A and the solution B when solution A described in the step 2 is mixed with the solution B
In respective dehydrated alcohol 1 ︰ 1 of parts by weight mixing, when obtaining solution D in the step 3 by step 2 sodium hydroxide with
2 ︰ 1 of trisodium citrate dihydrate weight fraction ratio preparation in step 3.
Further, reaction kettle heating temperature is 120~150 DEG C in the step 4, and the reaction time is 3~24 hours.
Further, zinc oxide nanosphere obtained by above-mentioned preparation method has super hydrophilic without ultraviolet light
Property, the diameter of the zinc oxide nanosphere is 150~800nm.
The advantages of the present invention over the prior art are that:
This method, which is formed, has Superhydrophilic zinc oxide nanosphere, has Superhydrophilic without ultraviolet light, makes
Standby host system is as follows: (1) replacing water as solvent using lower polar ethyl alcohol, be conducive to ZnO nonpolarityThe growth of crystal face, from
And polarity { 0002 } face of vertical direction is made to have more ratio to be exposed to surface, thus have the hydroxyl for being more exposed to surface,
It is set to have Superhydrophilic；(2) with the citrate of polyhydroxy, it is intended to be adsorbed on polar { 0002 } surface ZnO, inhibit
Its continued growth, and make the direction of growth of crystal grain along verticalSurface, so that the exposed area on { 0002 } surface
Increase；(3) product obtained by is the large particulate matter (150~800nm) that little particle assembles, and sample has in particle
Outer hole, because of its hydrophily, easily formation concave meniscus, to be easier to condense vapor on surface.
Detailed description of the invention
Fig. 1 is the nitrogen adsorption-desorption isothermal curve and graph of pore diameter distribution for the zinc oxide nanosphere that embodiment 1 obtains.
Fig. 2 is the X ray diffracting spectrum for the zinc oxide nanosphere that embodiment 1 obtains.
Fig. 3 is the transmission electron microscope photo for the zinc oxide nanosphere that embodiment 1 obtains.
Fig. 4 is that the zinc oxide nanosphere that embodiment 1 obtains scatters sealed storage half a year rear surface hydrophily under light indoors
Test result figure.
Specific embodiment
Below with reference to embodiment, the invention will be further described, but not as a limitation of the invention.
Embodiment 1:
The zinc oxide nanosphere of Superhydrophilic the preparation method is as follows:
1) it by weight, by 43.92 parts of Zinc diacetate dihydrates, is dissolved in 8000 parts of dehydrated alcohols, sealing stirring is formed
Clear solution A.
2) it by 2 parts of sodium hydroxides, is dissolved in 8000 parts of dehydrated alcohols, sealing stirring forms clear solution B.By A, B solution
After mixing, solution C is formed.
3) 1 part of trisodium citrate dihydrate is dissolved in 37.5 parts of distilled water, is added in above-mentioned solution C, form almost clarification
Colloidal solution D.
4) solution D is placed in reaction kettle, then reaction kettle is heated, heating temperature is 120 DEG C, and the reaction time is 24 small
When, obtained product is centrifuged, is washed, alcohol is washed and dries obtained product, drying temperature is 85 DEG C, drying temperature
Degree is 8 hours, and the average diameter of obtained zinc oxide nanosphere aggregate is 150nm.
Embodiment 2:
The zinc oxide nanosphere of Superhydrophilic the preparation method is as follows:
1) it by weight, by 40 parts of Zinc diacetate dihydrates, is dissolved in 8000 parts of dehydrated alcohols, sealing stirring is formed clear
Clear solution A.
2) it by 1.8 parts of sodium hydroxides, is dissolved in 8000 parts of dehydrated alcohols, sealing stirring forms clear solution B.A, B is molten
After liquid mixing, solution C is formed.
3) 0.9 part of trisodium citrate dihydrate is dissolved in 37.5 parts of distilled water, is added in above-mentioned solution C, formed almost clear
Clear colloidal solution D.
4) solution D is placed in reaction kettle, then reaction kettle is heated, heating temperature is 130 DEG C, and the reaction time is 12 small
When, obtained product is centrifuged, is washed, alcohol is washed and dries obtained product, drying temperature is 80 DEG C, drying temperature
Degree is 8 hours, and the average diameter of obtained zinc oxide nanosphere aggregate is 800nm.
Embodiment 3:
The zinc oxide nanosphere of Superhydrophilic the preparation method is as follows:
1) it by weight, by 48 parts of Zinc diacetate dihydrates, is dissolved in 8000 parts of dehydrated alcohols, sealing stirring is formed clear
Clear solution A.
2) it by 2.2 parts of sodium hydroxides, is dissolved in 8000 parts of dehydrated alcohols, sealing stirring forms clear solution B.A, B is molten
After liquid mixing, solution C is formed.
3) 1.1 parts of trisodium citrate dihydrates are dissolved in 37.5 parts of distilled water, are added in above-mentioned solution C, formed almost clear
Clear colloidal solution D.
4) solution D being placed in reaction kettle, then reaction kettle is heated, heating temperature is 150 DEG C, and the reaction time is 3 hours,
Obtained product is centrifuged, is washed, alcohol is washed and dries obtained product, drying temperature be 90 DEG C, drying temperature
It is 8 hours, the average diameter of obtained zinc oxide nanosphere aggregate is 500nm.
In order to verify the structure feature and performance of method products obtained therefrom of the invention, 1 resulting materials of embodiment are carried out
Structural characterization and performance test, it can be seen from figure 1 that zinc-oxide nano ball material prepared by the present invention has 3.0,11.9 and 50nm etc.
The aperture of a variety of scales, this makes material have extraordinary capillary condensation effect, is conducive to the condensation of steam.Separately from BET
The specific surface area that can be calculated material is 49.4m2/g。
As it is clear from fig. 2 that the X-ray diffraction peak of zinc-oxide nano ball material prepared by the present invention and wurtzite-type zinc oxide are brilliant
The diffraction maximum position of body is consistent completely；The broadening of diffraction maximum shows that the primary particle partial size of material is smaller, granularmetric analysis result
As shown in the table
XRD half-peak breadth analyzes average grain diameter
It can be seen from figure 3 that zinc-oxide nano ball material prepared by the present invention is the zinc oxide compared with small particle (20nm or so)
The zinc oxide spherical aggregate for the greater particle size (average about 150nm) that grain assembling is formed.
The hydrophilic test result of sealed storage half a year rear surface, test result are shown under Fig. 4 room scattering light, distilled water
It can be sprawled rapidly on sample powder surface and infiltrate absorption.This means that sample in the case where no ultraviolet lighting, can be kept
Its hydrophily is at least more than half a year.
The sheet glass for loading zinc-oxide nano ball material produced by the present invention and common glass sheet are compared, two sheet glass
It is placed in above the water surface that constant temperature is 40 DEG C at 10cm, in 2min, common glass sheet surface has hazed, but the glass of support materials
Piece surface has no droplet.After 2min, there is the moisture film of drawout in the glass sheet surface of support materials, does not block sight.Susceptible of proof
The material has the potentiality applied to hydrophilic antifogging field.
Claims (7)
1. a kind of preparation method of the zinc oxide nanosphere of Superhydrophilic, which is characterized in that comprising steps of 1, by two be hydrated acetic acid
Zinc is dissolved in dehydrated alcohol, and sealing stirring forms clear solution A；2, sodium hydroxide is dissolved in dehydrated alcohol, sealing stirring,
Clear solution B is formed, and the solution A and the solution B are mixed to form solution C；3, trisodium citrate dihydrate is dissolved in steaming
It in distilled water or deionized water, is added in the solution C, forms almost clear colloidal solution D；4, the solution D is placed in instead
It answers in kettle, then reaction kettle is heated, obtained product is centrifuged, is washed, alcohol is washed and is dried.
2. the preparation method of the zinc oxide nanosphere of Superhydrophilic according to claim 1, which is characterized in that the step
The weight fraction ratio of Zinc diacetate dihydrate and dehydrated alcohol is 5 ︰, 1000~6 ︰ 1000 in 1.
3. the preparation method of the zinc oxide nanosphere of Superhydrophilic according to claim 1, which is characterized in that the step
The weight fraction ratio of sodium hydroxide and dehydrated alcohol is 9 ︰, 40000~11 ︰ 40000 in 2.
4. the preparation method of the zinc oxide nanosphere of Superhydrophilic according to claim 1, which is characterized in that the step
It is 9 ︰, 375~11 ︰ 375 that trisodium citrate dihydrate, which is dissolved in distilled water or the weight fraction ratio of deionized water, in 3.
5. the preparation method of the zinc oxide nanosphere of Superhydrophilic according to claim 1, which is characterized in that the step
By the parts by weight of respective dehydrated alcohol in the solution A and the solution B when solution A described in 2 is mixed with the solution B
1 ︰ 1 mixing, by the sodium hydroxide in step 2 and the trisodium citrate dihydrate weight in step 3 when obtaining solution D in the step 3
Measure 2 ︰ 1 of portion rate preparation.
6. the preparation method of the zinc oxide nanosphere of Superhydrophilic according to claim 1, which is characterized in that the step
Reaction kettle heating temperature is 120~150 DEG C in 4, and the reaction time is 3~24 hours.
7. the preparation method of the zinc oxide nanosphere of Superhydrophilic according to claim 1, which is characterized in that obtained
Zinc oxide nanosphere has Superhydrophilic without ultraviolet light, and the diameter of the zinc oxide nanosphere is 150~800nm.
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| CN101880054A (en) * | 2009-05-08 | 2010-11-10 | 中国科学院兰州化学物理研究所 | Method for preparing hollow zinc oxide microspheres |
| CN101979324A (en) * | 2010-11-02 | 2011-02-23 | 上海大学 | Method for preparing monodisperse zinc oxide microspheres |
| CN102701267A (en) * | 2012-06-04 | 2012-10-03 | 兰州大学 | Preparation method for ZnO nanosphere with yolk-eggshell structure |
| CN102730747A (en) * | 2012-07-16 | 2012-10-17 | 河南师范大学 | Method for preparing zinc oxide with different microstructures by sol-gel assisted hydrothermal process |
| CN103991896A (en) * | 2014-04-08 | 2014-08-20 | 西北大学 | Spherical zinc oxide nanometer material preparation method |
| US20160104616A1 (en) * | 2014-10-14 | 2016-04-14 | Gwangju Institute Of Science And Technology | Method of fabricating zinc oxide nanostructures using liquid masking layer |
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| CN101880054A (en) * | 2009-05-08 | 2010-11-10 | 中国科学院兰州化学物理研究所 | Method for preparing hollow zinc oxide microspheres |
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| CN102701267A (en) * | 2012-06-04 | 2012-10-03 | 兰州大学 | Preparation method for ZnO nanosphere with yolk-eggshell structure |
| CN102730747A (en) * | 2012-07-16 | 2012-10-17 | 河南师范大学 | Method for preparing zinc oxide with different microstructures by sol-gel assisted hydrothermal process |
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| US20160104616A1 (en) * | 2014-10-14 | 2016-04-14 | Gwangju Institute Of Science And Technology | Method of fabricating zinc oxide nanostructures using liquid masking layer |
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