CN103101963A - Method of preparing and purifying transparent nano-zinc oxide sol - Google Patents
Method of preparing and purifying transparent nano-zinc oxide sol Download PDFInfo
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- CN103101963A CN103101963A CN201110357752XA CN201110357752A CN103101963A CN 103101963 A CN103101963 A CN 103101963A CN 201110357752X A CN201110357752X A CN 201110357752XA CN 201110357752 A CN201110357752 A CN 201110357752A CN 103101963 A CN103101963 A CN 103101963A
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Abstract
The invention relates to a method of preparing and purifying transparent nano-zinc oxide sol. The method comprises the steps: according to the mole ratio of zinc and base of 1:1-1:2, directly mixing zinc salt dissolved in polyhydric alcohols with inorganic base dissolved in polyhydric alcohols for reaction to produce a white zinc hydroxide flocculent precipitate mixed solution, then directly aging the zinc hydroxide filtration at room temperature or under heating condition to obtain transparent sol, or, aging at room temperature or under the heating condition after filtration or centrifugal concentration to obtain transparent sol; then adding monohydric alcohol with less than 3% of moisture content into the sol, so as to flocculate the sol, separating and purifying to obtain the precipitate, then dissipating the precipitate into the polyhydric alcohols to form high-purity transparent nano-zinc oxide sol, wherein the nano-zinc oxide is crystallized nano-zinc oxide. The method is simple, low in energy consumption, and convenient to operate, the obtained crystallized nano-zinc oxide sol has the characteristics of being high in transparency and purity, small in particle size and good in uniformity, and can be produced industrially in large scale.
Description
Technical field
The present invention relates to a kind of preparation and method of purification of transparent nano zinc oxide colloidal sol, the crystallization nano zine oxide colloidal sol that especially utilizes the chemical synthesis preparation to have high-clarity.
Background technology
Nano zine oxide refers to the zinc oxide fine particles of grain-size below 100nm.Because size of particles is little, specific surface area is large, have surface effects, small-size effect and macroscopic quantum channel effect etc., thereby show many special physics, chemistry, surface and interface character, show wide application prospect in rubber, coating, printing ink, color stuffing, catalyzer, the cosmetics of super quality, solar cell and medicine and other fields.But, due to polarity and the particle granular of nano zine oxide itself, therefore, have great specific surface area and higher specific surface energy, they are more easily reunited, be difficult to well disperse in the organic or inorganic medium, directly affected the actual effect of nano zine oxide.In order to reduce the surface polarity of nano material, improve dispersive ability and the avidity of nanoparticle in medium, enlarge the range of application of nano material, main method is that nano-ZnO is carried out surface modification or makes dispersion liquid and the colloidal sol of high dispersive at present.
The method that the most often prepares zinc carbonate colloidal sol be the people such as Spanhel (J.Am.Chem.Soc., 1991, the sol-gel method that 113:2826-2833) proposes, they first are dissolved in zinc acetate in ethanol, are made into Zn
2+Concentration is the ethanolic soln 0.5L of 0.1mol/L, under magnetic stirs in 80 ℃ of heating 180 minutes, and with the alcohol vapour condensation in a receiving flask, to 0.5L, add with the zinc acetate mol ratio is the lithium hydroxide of 1.4: 1 to the gained mixture with the ethanol redilution.Then 0 ℃ of lower ultrasonic oscillation 10 minutes, obtain transparent zinc oxide colloidal sol, this moment, pH approximately 8.2, the surface potential of particle is about neutrality, the zinc oxide content of gained colloidal sol is 0.2～1wt%, can produce precipitation when higher, and the price of lithium hydroxide used is more expensive, so industrial value is not high.
document (J.Phys.Chem. is separately arranged, 1987, 91:3789-3798) report, with the zinc acetate of 1mmol after 50 ℃ of lower vigorous stirring are dissolved in the Virahol of 80-90ml, cumulative volume is diluted to 920ml, again in adding rapidly sodium hydroxide/aqueous isopropanol of the 80ml of dissolving under 50 ℃ equally while continuing to stir under 0 ℃, again with 65 ℃ of heating in water bath 2 hours, again after under room temperature aging 3 days at 30 ℃, the vacuum under pressure drying of 133Pa can be prepared the ZnO transparent dispersion liquid that can disperse in Virahol or water, the 0.01wt% but this preparation method's zinc oxide concentration is only had an appointment, unactual on industrial application.
The people's such as Womelsdorf invention (US 6710091 and Taiwan patent I225470) has disclosed a kind of redispersible nano oxidized gel of zinc preparation, zinc acetate is dissolved in methyl alcohol, or zinc oxide is dissolved in the mixing solutions of acetic acid, methyl alcohol and deionized water, heating for dissolving, add alkali reaction and form dirty solution, then sedimentation, remove supernatant liquor, add again fresh methanol, stir about 50 minutes, supernatant liquor is removed in sedimentation, add again fresh methanol, stir about 50 minutes, the centrifugal supernatant liquor of removing gets the zinc oxide gel.The gained gel be particle diameter less than the nano zine oxide of 15nm, can be scattered in methylene dichloride or chloroform and form translucent colloidal sol, and the mixing solutions that can be scattered in ethylene glycol, water and trolamine gets yellow translucent colloidal sol.This invention can obtain the higher nano zine oxide colloidal sol (～38.6%) of concentration, but in embodiment, alcoholic solvent used is methyl alcohol, and methyl alcohol not only has toxicity and volatile, and is harmful.
US Patent No. 20060222586 and Taiwan patent I257918 propose a kind of novel method of nano zine oxide crystallization colloidal sol, utilize ethylene glycol to be reaction medium, zinc chloride and mineral alkali are dissolved in respectively ethylene glycol or contain in the ethylene glycol solution of a small amount of water, be made into the zinc solution of 2mol/L and the alkaline solution of 2mol/L, again with certain rate of titration, simultaneously with the ethylene glycol solution of zinc salt with contain the alkali ethylene glycol solution and be added drop-wise in the beaker that the proper amount of glycol damping fluid is housed in advance, by adjusting the rate of addition of zinc salt and alkaline solution, the pH value of controlling neutralizer is 9.0, the white flocks that obtains was directly heated 2 hours under 80 ℃, neutralizer is become transparent by white, can get transparent zinc-oxide nano colloidal sol, content can reach 2.5wt%.In addition, after white neutralizer is filtered, after getting rid of unnecessary ethylene glycol, white soup compound was heated 2 hours under 80 ℃, can get high density zinc carbonate Nano sol, concentration can reach 20wt%.The method institute spent glycol boiling point is high, and high without methyl alcohol toxicity, meets environmental requirement and has larger industrial value, but have poly-more complicated of neutralization reaction step, and rate of addition is slow, the more difficult to govern control of pH value in industrial production.And do not mention how removing by product sodium-chlor in invention, the purity that therefore how to improve nano zine oxide colloidal sol will be industrialized key.
Summary of the invention
The object of the invention is to the problem for the prior art existence, a kind of preparation and method of purification of nano zine oxide colloidal sol is provided.
In order to realize above purpose, the present invention realizes by following steps.
(1) preparation of raw material
Soluble zinc salt is dissolved in polyvalent alcohol, through 70～100 ℃ of heated and stirred dissolvings, is mixed with the clear solution that concentration is 0.1～4mol/L, cool to room temperature is stand-by.In another container, alkali is dissolved in polyvalent alcohol in 70～85 ℃ of heated and stirred situations, to be mixed with concentration be the faint yellow or henna clear solution of 0.1～3mol/L, and cool to room temperature is stand-by.
Select zinc salt for containing low crystal water or anhydrous zinc acetate, zinc chloride, zinc nitrate etc., preferred zinc chloride; Described alkali source is sodium hydroxide, potassium hydroxide, and Ammonia mineral alkali or contain the organic bases of a small amount of water, preferred sodium hydroxide; Described polyvalent alcohol is one or more mixing solutionss without water glycol, propylene glycol, butyleneglycol, glycerol and glycol ether etc., preferred ethylene glycol.
(2) preparation of transparent nano zinc oxide colloidal sol
Mol ratio by zinc and alkali is 1: 1～1: 2, under stirring state, zinc solution is directly poured in the alkali lye that measures, or alkali lye is directly poured into (or splashing into) in the zinc solution that measures, continue again to stir 30 minutes gained neutralizer pH:7～11.5 after adding.Neutralizer removed by filter partial solvent or neutralizer was directly stirred 15～30 hours under room temperature (25 ℃), can get zinc carbonate colloidal sol; Or heated under 60～100 ℃ 0.5～4 hour, also can obtain zinc carbonate colloidal sol.
(3) purification of transparent nano zinc oxide colloidal sol
Add water content to be less than or equal to 3% unary alcohol solvent in vitreosol, make the colloidal sol flocculation, stirred～10 minutes, carry out rapidly centrifugation or filtration, clean with monohydroxy-alcohol and separate, gained gel deposition thing can be scattered in and form the transparent or semitransparent colloidal sol that contains zinc oxide 1%～20% in polyvalent alcohol.Wherein contain water inventory and calculate with saltiness in colloidal sol and the solubleness in alcohol and water thereof, guarantee that byproduct salt can dissolve fully.Described monohydroxy-alcohol is one or more mixed solvents of methyl alcohol, ethanol, Virahol, preferred alcohol.
In gained colloidal sol of the present invention, the particle diameter of nano zine oxide is relevant with heat-up time with pH value, Heating temperature, and the pH value is larger, Heating temperature is higher and heat-up time is longer, and the particle diameter of gained nano zine oxide is larger.The inventive method is simple, and energy consumption is low, and is easy to operate, selects raw material to be easy to get.Gained zinc oxide colloidal sol has that transparency is high, purity is high, the characteristics that particle diameter is little and homogeneity is good, but large-scale industrialized production.
Description of drawings
Fig. 1 zinc oxide content is the UV-Vis spectrogram of 0.1% vitreosol
The TEM figure of Fig. 2 transparent nano zinc oxide colloidal sol
The electron-diffraction diagram of Fig. 3 transparent nano zinc oxide colloidal sol
Embodiment
Below provide several exemplary embodiments, but the present invention is not confined in following examples.
Embodiment 1
68g zinc chloride two hydrates are added in the 1L beaker, then add 500g ethylene glycol, stirred～30 minutes under 90～100 ℃, preparation is into about the transparent zinc chloride ethylene glycol solution of 1mol/L.Get the beaker of another 1L, claim 40g sodium hydroxide, add 500g ethylene glycol, 70～80 ℃ of lower stirring and dissolving, preparation is into about the transparent sodium hydroxide ethylene glycol solution of 2mol/L.Under stirring state, the sodium hydroxide ethylene glycol solution is slowly joined in the zinc chloride ethylene glycol solution, utilize the pH meter Real-Time Monitoring, when the pH value is 10 left and right, stops this and add alkali lye, continue to stir 20 minutes, obtain to contain the neutralizer of zinc hydroxide flocks.
Half of neutralizer stirred～20 hours in room temperature (25 ℃) is lower, obtain transparent nano zinc oxide colloidal sol; Second half neutralizer heated 40 minutes under 95 ℃, can obtain transparent nano zinc oxide colloidal sol, and this moment, zinc oxide content was～3.8wt%, colloidal sol can stablize～5 months still transparent.
Get vitreosol 50g, add moisture 3% ethanol 300g, stirred～10 minutes, make the colloidal sol flocculation, by-product salt is fully dissolved, filter or centrifugation, then clean and separate with ethanol; Gained gel deposition thing is redispersible in polyvalent alcohols such as ethylene glycol, propylene glycol, butyleneglycol, glycerol and glycol ethers, in 60～70 ℃ of lower underpressure distillation, form the high transparent nano zinc oxide colloidal sol of purity, as seen from Figure 1, the colloidal sol that contains zinc oxide 0.1%, wavelength is had good absorption less than 370nm, and to wavelength greater than the visible light of 400nm almost all by (greater than 99%).Fig. 2 is the TEM figure of transparent nano zinc oxide colloidal sol, and the particle diameter of nano zine oxide is 5～7nm.The electron-diffraction diagram (Fig. 3) of transparent nano zinc oxide colloidal sol is indicated as the crystallization nano zine oxide.
Embodiment 2
136g zinc chloride two hydrates are added in the 1L beaker, then add 500g ethylene glycol, stirred～30 minutes under 90～100 ℃, preparation is into about the transparent zinc chloride ethylene glycol solution of 2mol/L.Get the beaker of another 1L, claim 80g sodium hydroxide, add 1000g ethylene glycol, 70～80 ℃ of lower stirring and dissolving, preparation is into about the transparent sodium hydroxide ethylene glycol solution of 2mol/L.Under stirring state, the sodium hydroxide ethylene glycol solution is slowly joined in the zinc chloride ethylene glycol solution, utilize the pH meter Real-Time Monitoring, when the pH value is 10 left and right, stops this and add alkali lye, continue to stir 20 minutes, obtain to contain the neutralizer of zinc hydroxide flocks.
Half of neutralizer stirred～25 hours in room temperature (25 ℃) is lower, obtain transparent nano zinc oxide colloidal sol; If still aging under room temperature, will need approximately 3～4 days, neutralizer is just understood bleach.Second half neutralizer heated under 95 ℃ approximately 50 minutes, can obtain transparent nano zinc oxide colloidal sol, and this moment, zinc oxide content was～5wt%, colloidal sol can stablize～5 months still transparent.
The purification of colloidal sol is with embodiment 1, and same gained gel deposition thing is redispersible in polyvalent alcohols such as ethylene glycol, propylene glycol, butyleneglycol, glycerol and glycol ethers.
Embodiment 3
The preparation of neutralizer is with embodiment 1, the neutralizer utilization is filtered or centrifugal remove most of ethylene glycol after, thickness settling with gained 160g carries out respectively ripening under room temperature and heating state again, at room temperature stirred～30 hours, and heated under 95 ℃ approximately 60 minutes, all can obtain transparent nano zinc oxide colloidal sol, this moment zinc oxide content be～25wt%, can stablize～2 months still transparent.
The purification of colloidal sol is with embodiment 1, and same gained gel deposition thing is redispersible in polyvalent alcohols such as ethylene glycol, propylene glycol, butyleneglycol, glycerol and glycol ethers.
Embodiment 4
68g zinc chloride two hydrates are added in the 1L beaker, add again 500g ethylene glycol, stirred～30 minutes under 90～100 ℃, preparation is into about the transparent zinc chloride ethylene glycol solution of 1mol/L, then is 1: 1.8 preparation sodium hydroxide ethylene glycol solution (sodium hydroxide ethylene glycol solution of 2mol/L～486g) by the mol ratio of zinc and alkali.Under high degree of agitation, alkali lye is poured in the zinc chloride ethylene glycol solution fast, continues to stir 20 minutes, this moment, the pH value of gained neutralizer was～10.
Identical with the method for embodiment 1, under room temperature and heating state, neutralizer is carried out ripening, all can obtain transparent nano zinc oxide colloidal sol, this moment zinc oxide content be～3.8wt%, can stablize～5 months still transparent.
The purification of colloidal sol is with embodiment 1, and same gained gel deposition thing is redispersible in polyvalent alcohols such as ethylene glycol, propylene glycol, butyleneglycol, glycerol and glycol ethers.
Embodiment 5
Identical with embodiment 4, the mol ratio of zinc and alkali is 1: 1.8, when being neutralization reaction, fast the zinc chloride ethylene glycol solution is poured in caustic lye of soda, continues to stir 20 minutes, and this moment, the pH value of gained neutralizer was～10.Under room temperature and heating state, neutralizer is carried out ripening, all can obtain zinc oxide content and be the transparent nano zinc oxide colloidal sol of～3.8wt%, can stablize equally～5 months still transparent.Identical with the method for purification of embodiment 1, gained gel deposition thing is redispersible in polyvalent alcohols such as ethylene glycol, propylene glycol, butyleneglycol, glycerol and glycol ethers.
Embodiment 6
Identical with embodiment 4, just the mol ratio of zinc and alkali is 1: 2, under high degree of agitation, alkali lye is poured in the zinc chloride ethylene glycol solution fast, continues to stir 20 minutes, and this moment, the pH value of gained neutralizer was～11.5.Under 95 ℃, neutralizer is carried out heat treated～60 minute, can obtain zinc oxide content and be the transparent nano zinc oxide colloidal sol of～3.7wt%, standing～3 are month still transparent.Identical with the method for purification of embodiment 1, gained gel deposition thing is redispersible in polyvalent alcohols such as ethylene glycol, propylene glycol, butyleneglycol, glycerol and glycol ethers
Embodiment 7
109.6g zinc acetate two hydrates are added in the 1L beaker, then add 500g ethylene glycol, stirred～30 minutes under 90～100 ℃, preparation is into about the transparent zinc acetate ethylene glycol solution of 1mol/L.Get the beaker of another 1L, claim 40g sodium hydroxide, add 500g ethylene glycol, 70～80 ℃ of lower stirring and dissolving, preparation is into about the transparent sodium hydroxide ethylene glycol solution of 2mol/L.Under stirring state, the sodium hydroxide ethylene glycol solution is slowly joined in the zinc acetate ethylene glycol solution, utilize the pH meter Real-Time Monitoring, when the pH value is 8 left and right, stop this and add alkali lye, this moment, the mol ratio of zinc and alkali was 1: 1, continued to stir 20 minutes, obtained to contain the neutralizer of zinc hydroxide flocks.
Under room temperature and heating state, neutralizer is carried out ripening, all can obtain transparent nano zinc oxide colloidal sol, this moment, zinc oxide content was～2.8wt%.Identical with the method for purification of embodiment 1, gained gel deposition thing is redispersible in polyvalent alcohols such as ethylene glycol, propylene glycol, butyleneglycol, glycerol and glycol ethers.
Embodiment 8
148.5g zinc nitrate six hydrates are added in the 1L beaker, then add 500g ethylene glycol, stirred～30 minutes under 90～100 ℃, preparation is into about the transparent zinc nitrate ethylene glycol solution of 1mol/L.Get the beaker of another 1L, claim 40g sodium hydroxide, add 500g ethylene glycol, 70～80 ℃ of lower stirring and dissolving, preparation is into about the transparent sodium hydroxide ethylene glycol solution of 2mol/L.Under stirring state, the sodium hydroxide ethylene glycol solution is slowly joined in the zinc nitrate ethylene glycol solution, utilize the pH meter Real-Time Monitoring, when the pH value is 8.5 left and right, stop this and add alkali lye, this moment, the mol ratio of zinc and alkali was 1: 1.8, continued to stir 20 minutes, obtained to contain the neutralizer of zinc hydroxide flocks.
Under room temperature and heating state, neutralizer is carried out ripening, all can obtain transparent nano zinc oxide colloidal sol, this moment, zinc oxide content was～3.5wt%.Identical with the method for purification of embodiment 1, gained gel deposition thing is redispersible in polyvalent alcohols such as ethylene glycol, propylene glycol, butyleneglycol, glycerol and glycol ethers.
Embodiment 9
68g zinc chloride two hydrates are added in the 1L beaker, then add the 500g propylene glycol, stirred～30 minutes under 90～100 ℃, preparation is into about the transparent zinc chloride propylene glycol solution of 1mol/L.Get the beaker of another 1L, claim 40g sodium hydroxide, add 500g ethylene glycol, 70～80 ℃ of lower stirring and dissolving, preparation is into about the transparent sodium hydroxide ethylene glycol solution of 2mol/L.Under stirring state, the sodium hydroxide ethylene glycol solution is slowly joined in the zinc chloride propylene glycol solution, utilize the pH meter Real-Time Monitoring, when the pH value is 8 left and right, stop this and add alkali lye, this moment, the mol ratio of zinc and alkali was 1: 1.25, continued to stir 20 minutes, obtained to contain the neutralizer of zinc hydroxide flocks.
Under room temperature and heating state, neutralizer is carried out ripening, all can obtain transparent nano zinc oxide colloidal sol, this moment, zinc oxide content was～3wt%.Identical with the method for purification of embodiment 1, gained gel deposition thing is redispersible in polyvalent alcohols such as ethylene glycol, propylene glycol, butyleneglycol, glycerol and glycol ethers.
204g zinc chloride two hydrates are added in the 1L beaker, then add 500g ethylene glycol and glycerol mixing solutions (mass ratio is 80: 20), stirred～30 minutes under 90～100 ℃, preparation is into about the transparent liquor zinci chloridi of 3mol/L.Claim 120g sodium hydroxide, add 1000g ethylene glycol and glycerol mixing solutions (mass ratio is 80: 20), 70～80 ℃ of lower stirring and dissolving, preparation is into about the transparent sodium hydroxide ethylene glycol solution of 3mol/L.Under stirring state, sodium hydroxide solution is slowly joined in liquor zinci chloridi, utilize the pH meter Real-Time Monitoring, when the pH value is 9 left and right, stop this and add alkali lye, this moment, the mol ratio of zinc and alkali was 1: 1.5, continue to stir 20 minutes, obtain to contain the neutralizer of zinc hydroxide flocks.
Under room temperature and heating state, neutralizer is carried out ripening, all can obtain transparent nano zinc oxide colloidal sol, this moment, zinc oxide content was～7.5wt%.Identical with the method for purification of embodiment 1, gained gel deposition thing is redispersible in polyvalent alcohols such as ethylene glycol, propylene glycol, butyleneglycol, glycerol and glycol ethers.
Claims (8)
1. preparation and the method for purification of a transparent nano zinc oxide colloidal sol is characterized in that:
(1) soluble zinc salt is dissolved in polyvalent alcohol, through 70～100 ℃ of heated and stirred dissolvings, is mixed with the clear solution that concentration is 0.1～3mol/L, cool to room temperature is stand-by.In another container, alkali is dissolved in polyvalent alcohol in 70～85 ℃ of heated and stirred situations, to be mixed with concentration be the faint yellow or henna clear solution of 0.1～3mol/L, and cool to room temperature is stand-by.
(2) mol ratio by zinc and alkali is 1: 1～1: 2, under stirring state, zinc solution is directly poured in the alkali lye that measures, or alkali lye is directly poured into (or splashing into) in the zinc solution that measures, continue again to stir 30 minutes gained neutralizer pH:7～11.5 after adding.
(3) neutralizer is removed by filter partial solvent after or directly stirred 15～30 hours in room temperature (25 ℃), can get zinc carbonate colloidal sol; Or heated under 60～100 ℃ 0.5～4 hour, also can obtain zinc carbonate colloidal sol.
(4) add water content to be less than or equal to 3% unary alcohol solvent in vitreosol, make the colloidal sol flocculation, stirred～10 minutes, and carried out rapidly centrifugation or filtration, gained gel deposition thing can be scattered in and form the transparent or semitransparent colloidal sol that contains zinc oxide 1%～30% in polyvalent alcohol.Wherein contain water inventory and calculate with saltiness in colloidal sol and the solubleness in water thereof, guarantee that byproduct salt can dissolve fully.
2. by preparation and the method for purification of a kind of transparent nano zinc oxide colloidal sol claimed in claim 1, it is characterized in that described zinc salt is selected from the zinc salts such as zinc acetate, zinc chloride, zinc nitrate.Described alkali is sodium hydroxide, potassium hydroxide, and Ammonia mineral alkali.
3. by preparation and the method for purification of a kind of transparent nano zinc oxide colloidal sol claimed in claim 1, it is characterized in that described polyhydric alcohol solutions is one or more mixing solutionss of ethylene glycol, propylene glycol, butyleneglycol, glycerol and glycol ether etc.Described monohydroxy-alcohol for flocculation is one or more mixed solvents of methyl alcohol, ethanol, Virahol.
4. by preparation and the method for purification of a kind of transparent nano zinc oxide colloidal sol claimed in claim 1, the solvent temperature that it is characterized in that zinc salt is 70～100 ℃, and the best is 90 ℃, realizes vitreosol to improve zinc content and to be beneficial under normal temperature and pressure.
5. by preparation and the method for purification of a kind of transparent nano zinc oxide colloidal sol claimed in claim 1, the pH value that it is characterized in that the gained neutralizer is 7～11.5.
6. press preparation and the method for purification of a kind of transparent nano zinc oxide colloidal sol claimed in claim 1, it is characterized in that by the pH value of regulating neutralizer, Heating temperature and the heat-up time of neutralizer, can realize the regulation and control of Particle Size of Nanometer ZnO, it is changed between 5～50nm.
7. press preparation and the method for purification of a kind of transparent nano zinc oxide colloidal sol claimed in claim 1, it is characterized in that can be by certain mol ratio, under stirring state, zinc source (or alkali source) directly is poured in alkali source (or zinc source) fast reacts, also alkali source slowly can be poured in the zinc source, be realized the real-time adjusting of pH value.
8. press preparation and the method for purification of a kind of transparent nano zinc oxide colloidal sol claimed in claim 1, it is characterized in that prepared nano zine oxide colloidal sol can be dissolved in polyvalent alcohol (ethylene glycol, propylene glycol, butyleneglycol, glycerol, glycol ether) again after flocculation separation, and gained white powder after the colloidal sol drying, still can be scattered in polyvalent alcohol.
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Cited By (7)
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| CN103318945A (en) * | 2013-07-11 | 2013-09-25 | 苏州大学 | Preparation method of colloidal solution of nano-ZnO |
| CN103816885A (en) * | 2014-02-20 | 2014-05-28 | 阜阳师范学院 | Preparation and application of nano zinc oxide photocatalyst |
| CN104071827A (en) * | 2014-07-22 | 2014-10-01 | 天津工业大学 | Method for synthesizing ordered laminar nanometer zinc oxide by using sodium dodecyl sulfate as template |
| CN106106519A (en) * | 2016-06-25 | 2016-11-16 | 王赞 | Zinc oxide colloidal sol for ceramic tile and preparation method thereof |
| CN106986374A (en) * | 2017-05-08 | 2017-07-28 | 济南大学 | A kind of high specific surface area and mesoporous zinc-oxide nano cluster and preparation method thereof |
| CN113861966A (en) * | 2021-10-15 | 2021-12-31 | 吉隆达(成都)新材料科技有限公司 | Method for preparing high-purity zinc oxide quantum dots on large scale |
| CN115243660A (en) * | 2020-03-03 | 2022-10-25 | 联合利华知识产权控股有限公司 | Transparent dentifrice comprising zinc |
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| TWI257918B (en) * | 2005-03-29 | 2006-07-11 | Headway Advanced Materials Inc | A preparation method for nanometer grade zinc oxide crystalline (zincite) sol |
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| CN1587061A (en) * | 2004-08-26 | 2005-03-02 | 复旦大学 | Process for preparing sol-gel of nano zinc oxide by low temperature |
| TWI257918B (en) * | 2005-03-29 | 2006-07-11 | Headway Advanced Materials Inc | A preparation method for nanometer grade zinc oxide crystalline (zincite) sol |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103318945A (en) * | 2013-07-11 | 2013-09-25 | 苏州大学 | Preparation method of colloidal solution of nano-ZnO |
| CN103816885A (en) * | 2014-02-20 | 2014-05-28 | 阜阳师范学院 | Preparation and application of nano zinc oxide photocatalyst |
| CN103816885B (en) * | 2014-02-20 | 2015-11-11 | 阜阳师范学院 | A kind of preparations and applicatio of nano zinc oxide photocatalyst |
| CN104071827A (en) * | 2014-07-22 | 2014-10-01 | 天津工业大学 | Method for synthesizing ordered laminar nanometer zinc oxide by using sodium dodecyl sulfate as template |
| CN106106519A (en) * | 2016-06-25 | 2016-11-16 | 王赞 | Zinc oxide colloidal sol for ceramic tile and preparation method thereof |
| CN106986374A (en) * | 2017-05-08 | 2017-07-28 | 济南大学 | A kind of high specific surface area and mesoporous zinc-oxide nano cluster and preparation method thereof |
| CN106986374B (en) * | 2017-05-08 | 2018-11-16 | 济南大学 | A kind of high specific surface area and mesoporous zinc-oxide nano cluster and preparation method thereof |
| CN115243660A (en) * | 2020-03-03 | 2022-10-25 | 联合利华知识产权控股有限公司 | Transparent dentifrice comprising zinc |
| CN113861966A (en) * | 2021-10-15 | 2021-12-31 | 吉隆达(成都)新材料科技有限公司 | Method for preparing high-purity zinc oxide quantum dots on large scale |
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Application publication date: 20130515 |