CN100364895C - Method for preparing nano zinc oxide powder - Google Patents
Method for preparing nano zinc oxide powder Download PDFInfo
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- CN100364895C CN100364895C CNB2005100274943A CN200510027494A CN100364895C CN 100364895 C CN100364895 C CN 100364895C CN B2005100274943 A CNB2005100274943 A CN B2005100274943A CN 200510027494 A CN200510027494 A CN 200510027494A CN 100364895 C CN100364895 C CN 100364895C
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Abstract
This invention relates to a preparation method for nm ZnO powder including: putting a soluble Zn salt, KOH or NaOH, KBH or NaBH in a container with solvent N and N-methyl formamide in the mol ratio of 1:0.66: (1-3) and mixing them to keep the temperature under 100-200deg. C for 2-48 hours then to be cooled to room temperature to clean the generated product to neutral PH value finally cleaning it with absolute alcohol, filtering and drying it, in which, the productivity of ZnO reaches to 100% by this invented preparation method.
Description
Technical field
The invention belongs to the preparation method field of nano zinc oxide powder.
Background technology
Nano-ZnO is a kind of Multifunction inorganic materials, has the incomparable property of common ZnO.Nano ZnO material not only substitutes common zinc oxide in traditional industry fields such as coating, rubber, potteries, and wide application prospect is arranged in the contour frontier of opto-electronic conversion, photochemical catalysis and transmitter, therefore study the synthetic of nano ZnO material and have great significance with character.The method for preparing at present nano-ZnO mainly contains sluggish precipitation, microemulsion method, solid reaction process and hydrothermal method etc., and these preparation methods have certain shortcoming, and are not high as productive rate, and size-grade distribution is wide in range etc.
Summary of the invention
Purpose of the present invention just provides the preparation method of a kind of high yield, high purity, even particle size distribution, superfine nano zinc oxide powder.
The preparation method of nano zinc oxide powder of the present invention is as follows:
With soluble zinc salt, potassium hydroxide or sodium hydroxide, POTASSIUM BOROHYDRIDE or sodium borohydride is 1: 0.66 in molar ratio: solvent N is equipped with in (1～3) adding, in the container of dinethylformamide, stir, be incubated 2～48 hours down for 100～200 ℃ in temperature, be cooled to room temperature then, clean resultant to pH value and be neutral, at last with dehydrated alcohol cleaning, filtration, dry getting final product.
The preparation method of nano zinc oxide powder of the present invention, wherein soluble zinc salt is meant zinc chloride, zinc nitrate, zinc sulfate, zinc acetate etc., is preferably zinc chloride.
The preparation method of nano zinc oxide powder of the present invention be to keep certain pressure, N wherein, and the amount of dinethylformamide is 80～90% of a reactor volume.
The preparation method of nano zinc oxide powder of the present invention, the addition sequence of its raw material does not have strict requirement.Consider the severe degree of reaction, more excellent order is to add soluble zinc salt earlier, stirs with glass stick, adds potassium hydroxide or sodium hydroxide then, adds POTASSIUM BOROHYDRIDE or sodium borohydride at last.
The preparation method of nano zinc oxide powder of the present invention, wherein employed reaction vessel needs corrosion-resistant and High Temperature High Pressure, is preferably polytetrafluoroethyltank tank.
The preparation method of nano zinc oxide powder of the present invention, wherein said that the resultant washing is extremely neutral, preferably adopt deionized water, dehydrated alcohol alternately to clean described resultant repeatedly until being neutral.
Beneficial effect of the present invention: adopt zinc oxide productive rate that the preparation method of nano zinc oxide powder of the present invention obtains near 100%, purity is also very high, to between tens nanometers, and method is simple in several nanometers for granularity, is the good processing method of preparation superfine nano zinc oxide high-end product.
Description of drawings
Fig. 1 is the transmission electron microscope photo of embodiment 1 products therefrom.
Fig. 2 is the transmission electron microscope photo of embodiment 2 products therefroms.
Fig. 3 is the transmission electron microscope photo of embodiment 3 products therefroms.
Embodiment
Embodiment 1
Measure the N of 85ml with graduated cylinder, it is in the polytetrafluoroethyltank tank of 100ml that dinethylformamide adds volume.Weighing 3.326gZnCl
2Join in the polytetrafluoroethyltank tank, stir a moment, weighing 0.896g KOH (0.016mol) and 3.960g KBH again with glass stick
4Join successively in the polytetrafluoroethyltank tank, i.e. ZnCl
2, KOH and KBH
4Mol ratio be respectively 1: 0.66: 3.The polytetrafluoroethyltank tank good seal is put into autoclave, autoclave is put into constant temperature oven, 100 ℃ of holding temperatures are set, be incubated 48 hours, naturally cool to room temperature then.Is neutral with the product in the polytetrafluoroethyltank tank with washed with de-ionized water to potential of hydrogen, cleans and filters with dehydrated alcohol at last.With final product in air or in the loft drier 30～60 ℃ of heat dryings just obtain the zinc oxide that granularity is about 25 nanometers, productive rate 〉=99%, purity 〉=99.8%.The transmission electron microscope photo of product is seen Fig. 1.
Embodiment 2
Measure the N of 85ml with graduated cylinder, it is in the polytetrafluoroethyltank tank of 100ml that dinethylformamide adds volume.Weighing 3.946gZnCl
2Join in the polytetrafluoroethyltank tank, stir a moment, weighing 0.896g KOH and 2.640g KBH again with glass stick
4Join successively in the polytetrafluoroethyltank tank, i.e. ZnCl
2, KOH and KBH
4Mol ratio be respectively 1: 0.66: 2.。The polytetrafluoroethyltank tank good seal is put into autoclave, autoclave is put into constant temperature oven, 150 ℃ of holding temperatures are set, be incubated 24 hours, naturally cool to room temperature then.Is neutral with the product in the polytetrafluoroethyltank tank with washed with de-ionized water to potential of hydrogen, cleans and filters with dehydrated alcohol at last.With final product in air or in the loft drier 30～60 ℃ of heat dryings just obtain the zinc oxide that granularity is about 30 nanometers, productive rate 〉=99%, purity 〉=99.8%.The transmission electron microscope photo of product is seen Fig. 2.
Embodiment 3
Measure the N of 85ml with graduated cylinder, it is in the polytetrafluoroethyltank tank of 100ml that dinethylformamide adds volume.Weighing 3.326gZnCl
2Join in the polytetrafluoroethyltank tank, stir a moment, weighing 0.896g KOH and 1.320g KBH again with glass stick
4Join successively in the polytetrafluoroethyltank tank, i.e. ZnCl
2, KOH and KBH
4Mol ratio be respectively 1: 0.66: 1.The polytetrafluoroethyltank tank good seal is put into autoclave, autoclave is put into constant temperature oven, 200 ℃ of holding temperatures are set, be incubated 2 hours, naturally cool to room temperature then.Is neutral with the product in the polytetrafluoroethyltank tank with washed with de-ionized water to potential of hydrogen, cleans and filters with dehydrated alcohol at last.With final product in air or in the loft drier 30～60 ℃ of heat dryings just obtain the zinc oxide that granularity is about 25 nanometers, productive rate 〉=99%, purity 〉=99.8%.The transmission electron microscope photo of product is seen Fig. 3.
Claims (8)
1. the preparation method of a nano zinc oxide powder, this method is: with soluble zinc salt, potassium hydroxide or sodium hydroxide and POTASSIUM BOROHYDRIDE or sodium borohydride is 1: 0.66 in molar ratio: the amount of (1～3) adds solvent N is housed, in the container of dinethylformamide, stir, be incubated 2～48 hours down for 100～200 ℃ in temperature, be cooled to room temperature then, clean resultant to pH value and be neutral, at last with dehydrated alcohol cleaning, filtration, dry getting final product.
2. the preparation method of nano zinc oxide powder as claimed in claim 1 is characterized in that the addition sequence of its raw material adds soluble zinc salt for elder generation, stirs, and adds potassium hydroxide or sodium hydroxide then, adds POTASSIUM BOROHYDRIDE or sodium borohydride at last.
3. the preparation method of nano zinc oxide powder as claimed in claim 1 is characterized in that said N, and the amount of dinethylformamide is 80～90% of a reactor volume.
4. the preparation method of nano zinc oxide powder as claimed in claim 1 is characterized in that said soluble zinc salt is meant zinc chloride, zinc nitrate, zinc sulfate or zinc acetate.
5. the preparation method of nano zinc oxide powder as claimed in claim 4 is characterized in that said soluble zinc salt is meant zinc chloride.
6. the preparation method of nano zinc oxide powder as claimed in claim 1 is characterized in that said reaction vessel is corrosion-resistant and the high temperature high voltage resistant container.
7. the preparation method of nano zinc oxide powder as claimed in claim 6 is characterized in that said reaction vessel is a polytetrafluoroethyltank tank.
8. the preparation method of nano zinc oxide powder as claimed in claim 1 is characterized in that said cleaning resultant to pH value is neutral, and method is to adopt deionized water, dehydrated alcohol alternately to clean described resultant repeatedly until being neutral.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2005100274943A CN100364895C (en) | 2005-07-04 | 2005-07-04 | Method for preparing nano zinc oxide powder |
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| CNB2005100274943A CN100364895C (en) | 2005-07-04 | 2005-07-04 | Method for preparing nano zinc oxide powder |
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| CN1891632A CN1891632A (en) | 2007-01-10 |
| CN100364895C true CN100364895C (en) | 2008-01-30 |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101628731B (en) * | 2009-07-28 | 2011-04-27 | 西北工业大学 | Zinc oxide nanoparticle preparation method |
| CN102303896B (en) * | 2011-05-25 | 2013-09-18 | 云南大学 | Method for preparing zinc oxide with hollow flower-like micrometer structure |
| CN102807249B (en) * | 2011-06-01 | 2014-04-16 | 国家纳米科学中心 | Method for controlling shapes of zinc oxide nanoparticles |
| CN103433062B (en) * | 2013-08-27 | 2016-02-10 | 安徽大学 | A kind of preparation method of zinc oxide/silver bromide nanometer composite |
| CN106467316A (en) * | 2016-10-13 | 2017-03-01 | 哈尔滨工业大学 | A kind of method of the oxide with sodium borohydride for raw material preparation hydrogenation |
| CN107673398B (en) * | 2017-10-11 | 2019-05-14 | 北京振兴华龙制冷设备有限责任公司 | A kind of preparation method of Nanometer-sized Rods ZnO and its application for being used to prepare ventilating duct for air-conditioner |
| CN112341680A (en) * | 2020-12-14 | 2021-02-09 | 华东理工大学 | Method for preparing anti-aging nitrile rubber from modified carbon nano tubes |
| CN114394615A (en) * | 2021-12-31 | 2022-04-26 | 苏州明德新能源技术有限公司 | Slow-release hydrogen material and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5672427A (en) * | 1993-08-31 | 1997-09-30 | Mitsubishi Materials Corporation | Zinc oxide powder having high dispersibility |
| CN1613774A (en) * | 2004-11-16 | 2005-05-11 | 浙江大学 | Preparation for zinc oxide nanometer material |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5672427A (en) * | 1993-08-31 | 1997-09-30 | Mitsubishi Materials Corporation | Zinc oxide powder having high dispersibility |
| CN1613774A (en) * | 2004-11-16 | 2005-05-11 | 浙江大学 | Preparation for zinc oxide nanometer material |
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