CN103145175B - Preparation method of small-size nano-zinc oxide powder - Google Patents
Preparation method of small-size nano-zinc oxide powder Download PDFInfo
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Abstract
The invention provides a preparation method of small-size nano-zinc oxide powder. The preparation method comprises the following steps of: 1, preparing bivalent zinc salt ethanol solution by utilizing absolute ethyl alcohol as a solvent, and marking as a solution A; 2, preparing NaOH ethanol solution by utilizing absolute ethyl alcohol as a solvent, and marking as a solution B; 3, adding the prepared solution B to the solution A in drops under magnetic stirring, heating and maintaining the temperature, so as to obtain a solid-liquid mixture containing zinc oxide precipitate; and 4, respectively and centrifugally washing the obtained solid-liquid mixture containing the zinc oxide precipitate by deionized water and absolute ethyl alcohol, and then drying the centrifugally washed product to obtain the nano-zinc oxide powder. The preparation method is low in cost, simple in process, and capable of preparing the nano-zinc oxide powder with size less than 10 nanometers; and the specific surface area of the nano-zinc oxide powder is increased and the nano-zinc oxide powder has excellent surface effect, small-size effect and macroscopic quantum tunneling effect.
Description
Technical field
The present invention relates to a kind of preparation method of Zinc oxide powder, be specifically related to a kind of preparation method of small-size nano-zinc oxide powder.
Background technology
Current large quantity research shows: the size of the performance of material and its microscopic structural units is closely related.Because the specific surface area of zinc oxide (ZnO) sharply increases with the reduction of its grain-size, nano zine oxide is made to create its special effects not available for body cake mass, as surface effects, small-size effect and macro quanta tunnel effect etc.So nano zine oxide has the incomparable property of general body block zinc oxide in solar cell, electron device, nano-device, catalyzer, sensor, antibacterial and deodorizing etc.Therefore, preparation size is even, monodispersity is good and the Zinc oxide powder with nanoscale has become a significant challenge of researcher.But still rare document regarding sizes is less than the research report of the nano-zinc oxide powder of 10nm at present.
Summary of the invention
For solving above-mentioned problems of the prior art, order of the present invention is the preparation method providing a kind of small-size nano-zinc oxide powder, preparation method of the present invention is with low cost, operation is simple and can prepare the nano-zinc oxide powder that size is less than 10nm, the specific surface area of nano-zinc oxide powder is increased, there is excellent surface effects, small-size effect and macro quanta tunnel effect.
For achieving the above object, the technical solution adopted in the present invention is:
A preparation method for small-size nano-zinc oxide powder, comprises the steps:
Step 1: the ethanol solution of preparation divalent zinc salt: utilize dehydrated alcohol to make the ethanolic soln of solvent preparation divalent zinc salt, its volumetric molar concentration is made to be 0.0001mol/L ~ 1.0mol/L, and divalent zinc salt solution magnetic agitation is heated to 65 ~ 78 DEG C and is incubated 1 ~ 10 minute, be denoted as solution A;
Step 2: the ethanol solution of preparation NaOH: utilize dehydrated alcohol to make the ethanolic soln of solvent preparation NaOH, the volumetric molar concentration of NaOH is made to be 0.001mol/L ~ 1.0mol/L, the mol ratio simultaneously making NaOH and divalent zinc salt is 50:1 ~ 1:1, is denoted as solution B;
Step 3: solution B step 2 configured dropwise joins in solution A, remains magnetic agitation in the process added, and is incubated 0.01h ~ 1h at being heated to 65 DEG C ~ 78 DEG C, obtains the solidliquid mixture containing zinc oxide precipitate;
Step 4: what step 3 obtained uses deionized water and dehydrated alcohol centrifuge washing 3 times ~ 5 times respectively containing the solidliquid mixture of zinc oxide precipitate, then by the dry 1h ~ 12h at 50 DEG C ~ 80 DEG C of the product after centrifuge washing, obtains nano-zinc oxide powder.
Divalent zinc salt described in step 1 is zinc nitrate, zinc acetate, zinc sulfate or zinc chloride.
The present invention adopt a kind of low cost, controllability and the good liquid phase synthesizing method of operability, by zinc salt kind, reactant concn, temperature of reaction and the regulation and control in reaction times, the high and nano-zinc oxide powder of size uniform of output can be prepared.The nano-zinc oxide powder obtained is that size is less than 10nm, and the specific surface area of nano-zinc oxide powder is increased, and has excellent surface effects, small-size effect and macro quanta tunnel effect.
Accompanying drawing explanation
Fig. 1 is the transmission electron micrograph of nano-zinc oxide powder prepared by embodiment one.
Fig. 2 is the transmission electron micrograph of nano-zinc oxide powder prepared by embodiment two.
Embodiment
Below structure of the present invention is described in further detail.
Embodiment 1
Embodiment one
The preparation method of a kind of small-size nano-zinc oxide powder of the present embodiment, comprises the steps:
Step 1: 0.0357g zinc nitrate and 30ml dehydrated alcohol are mixed with solution, and zinc nitrate ethanolic soln magnetic agitation is heated to 75 DEG C and is incubated 10 minutes, be denoted as solution A, the speed of magnetic agitation is 4000 revs/min;
Step 2: 0.024g sodium hydroxide and 30mL dehydrated alcohol are mixed with solution, are denoted as solution B;
Step 3: solution B is dropwise joined in solution A, this process keeps magnetic agitation to be heated to 75 DEG C, and the speed of magnetic agitation is 4000 revs/min, and is incubated 0.5h, obtains the solidliquid mixture containing zinc oxide precipitate;
Step 4: what step 3 obtained uses deionized water and dehydrated alcohol centrifuge washing 3 times, then by the dry 6h at 60 DEG C of the oxidized zinc products after centrifuge washing respectively containing the solidliquid mixture of zinc oxide precipitate.
The present embodiment size that can obtain as shown in Figure 1 is less than the nano-zinc oxide powder of 10nm, and mean particle size is 6.6nm.
Embodiment two
The preparation method of a kind of small-size nano-zinc oxide powder of the present embodiment, comprises the steps:
Step 1: 0.357g zinc nitrate and 30ml dehydrated alcohol are mixed with solution, and zinc nitrate ethanolic soln magnetic agitation is heated to 75 DEG C and is incubated 5 minutes, be denoted as solution A, the speed of magnetic agitation is 3000 revs/min;
Step 2: 0.24g sodium hydroxide and 90mL dehydrated alcohol are mixed with solution, are denoted as solution B;
Step 3: solution B is dropwise joined in solution A, this process keeps magnetic agitation to be heated to 75 DEG C, and the speed of magnetic agitation is 3000 revs/min, and is incubated 0.5h, obtains the solidliquid mixture containing zinc oxide precipitate;
Step 4: what step 3 obtained uses deionized water and dehydrated alcohol centrifuge washing 3 times, then by the dry 5h at 60 DEG C of the oxidized zinc products after centrifuge washing respectively containing the solidliquid mixture of zinc oxide precipitate.
The present embodiment size that can obtain as shown in Figure 2 is less than the nano-zinc oxide powder of 10nm, and its mean particle size is 8.0nm.
Embodiment three
The preparation method of a kind of small-size nano-zinc oxide powder of the present embodiment, comprises the steps:
Step 1: 0.346g zinc sulfate and 30ml dehydrated alcohol are mixed with solution, and zinc sulfate ethanolic soln magnetic agitation is heated to 75 DEG C and is incubated 7 minutes, be denoted as solution A, the speed of magnetic agitation is 3000 revs/min;
Step 2: 0.24g sodium hydroxide and 90mL dehydrated alcohol are mixed with solution, are denoted as solution B;
Step 3: solution B is dropwise joined in solution A, this process keeps magnetic agitation to be heated to 75 DEG C, and the speed of magnetic agitation is 3000 revs/min, and is incubated 0.4h, obtains the solidliquid mixture containing zinc oxide precipitate;
Step 4: what step 3 obtained uses deionized water and dehydrated alcohol centrifuge washing 4 times, then by the dry 3h at 70 DEG C of the oxidized zinc products after centrifuge washing respectively containing the solidliquid mixture of zinc oxide precipitate.
Embodiment four
The preparation method of a kind of small-size nano-zinc oxide powder of the present embodiment, comprises the steps:
Step 1: 0.15g zinc chloride and 30ml dehydrated alcohol are mixed with solution, and zinc chloride ethanolic soln magnetic agitation is heated to 78 DEG C and is incubated 5 minutes, be denoted as solution A, the speed of magnetic agitation is 2500 revs/min;
Step 2: 0.24g sodium hydroxide and 90mL dehydrated alcohol are mixed with solution, are denoted as solution B;
Step 3: solution B is dropwise joined in solution A, this process keeps magnetic agitation to be heated to 77 DEG C, and the speed of magnetic agitation is 2500 revs/min, and is incubated 0.01h, obtains the solidliquid mixture containing zinc oxide precipitate;
Step 4: what step 3 obtained uses deionized water and dehydrated alcohol centrifuge washing 4 times, then by the dry 12h at 50 DEG C of the oxidized zinc products after centrifuge washing respectively containing the solidliquid mixture of zinc oxide precipitate.
Embodiment five
The preparation method of a kind of small-size nano-zinc oxide powder of the present embodiment, comprises the steps:
Step 1: 0.20g zinc acetate and 30ml dehydrated alcohol are mixed with solution, and zinc acetate ethanolic soln magnetic agitation is heated to 65 DEG C and is incubated 1 minute, be denoted as solution A, the speed of magnetic agitation is 3000 revs/min;
Step 2: 0.24g sodium hydroxide and 60mL dehydrated alcohol are mixed with solution, are denoted as solution B;
Step 3: solution B is dropwise joined in solution A, this process keeps magnetic agitation to be heated to 65 DEG C, and the speed of magnetic agitation is 3000 revs/min, and is incubated 1h, obtains the solidliquid mixture containing zinc oxide precipitate;
Step 4: what step 3 obtained uses deionized water and dehydrated alcohol centrifuge washing 5 times, then by the dry 1h at 80 DEG C of the oxidized zinc products after centrifuge washing respectively containing the solidliquid mixture of zinc oxide precipitate.
Claims (1)
1. size is less than a preparation method for the nano-zinc oxide powder of 10nm, it is characterized in that: comprise the steps:
Step 1: the ethanol solution of preparation divalent zinc salt: utilize dehydrated alcohol to make the ethanolic soln of solvent preparation divalent zinc salt, its volumetric molar concentration is made to be 0.0001mol/L ~ 1.0mol/L, and divalent zinc salt solution magnetic agitation is heated to 65 DEG C ~ 78 DEG C and is incubated 1 ~ 10 minute, be denoted as solution A;
Step 2: the ethanol solution of preparation NaOH: utilize dehydrated alcohol to make the ethanolic soln of solvent preparation NaOH, the volumetric molar concentration of NaOH is made to be 0.001mol/L ~ 1.0mol/L, the mol ratio simultaneously making NaOH and divalent zinc salt is 50:1 ~ 1:1, is denoted as solution B;
Step 3: solution B step 2 configured dropwise joins in solution A, remains magnetic agitation in the process added, and is incubated 0.01h ~ 1h at being heated to 65 DEG C ~ 78 DEG C, obtains the solidliquid mixture containing zinc oxide precipitate;
Step 4: what step 3 obtained uses deionized water and dehydrated alcohol centrifuge washing 3 times ~ 5 times respectively containing the solidliquid mixture of zinc oxide precipitate, then by the dry 1h ~ 12h at 50 DEG C ~ 80 DEG C of the product after centrifuge washing, obtains nano-zinc oxide powder;
Divalent zinc salt described in step 1 is zinc nitrate, zinc acetate, zinc sulfate or zinc chloride.
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| CN104076073A (en) * | 2014-07-10 | 2014-10-01 | 南京理工大学 | Short-bar-shaped nano-zinc oxide/graphene compound and preparation method thereof |
| CN104445362A (en) * | 2014-11-03 | 2015-03-25 | 苏州市泽镁新材料科技有限公司 | Preparation method of nano zinc carbonate |
| CN104843767B (en) * | 2015-05-13 | 2017-04-12 | 湖南尔康制药股份有限公司 | Preparation method of officinal nano-zinc oxide |
| CN106477620A (en) * | 2016-09-26 | 2017-03-08 | 广西科技大学 | A kind of preparation method of the transparent alcoholic solution of nano zine oxide |
| CN106830921B (en) * | 2017-01-23 | 2019-11-15 | 九江学院 | A kind of ZnO transparent ceramics and preparation method thereof |
| CN108246245A (en) * | 2018-03-06 | 2018-07-06 | 成都理工大学 | A kind of preparation method of nano zinc oxide modified vermiculite |
| CN110651899A (en) * | 2019-10-10 | 2020-01-07 | 仲恺农业工程学院 | Phospholipid encapsulated nano zinc oxide and preparation method thereof |
| CN111573712B (en) * | 2020-05-26 | 2022-07-26 | 安徽锦华氧化锌有限公司 | Preparation method for improving antibacterial property of nano zinc oxide |
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| CN102161499A (en) * | 2011-01-14 | 2011-08-24 | 北京化工大学 | Quantum size zinc oxide and preparation method and application thereof |
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| US20070004840A1 (en) * | 2004-05-19 | 2007-01-04 | Texas A&M University | Zinc oxide polymer nanocomposites and methods of producing zinc oxide polymer nanocomposites |
| JP2009215342A (en) * | 2008-03-07 | 2009-09-24 | Tokyo Institute Of Technology | Method for producing fluorescent particle |
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| CN102101692A (en) * | 2010-11-26 | 2011-06-22 | 西安理工大学 | Chemical synthesis method of zinc oxide nano crystal based on alcohol-water system |
| CN102161499A (en) * | 2011-01-14 | 2011-08-24 | 北京化工大学 | Quantum size zinc oxide and preparation method and application thereof |
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| "不同醇溶剂中氧化锌纳米晶的可控制备";李奉杰等;《硅酸盐通报》;20120229;第31卷(第1期);第145-149页 * |
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