CN103145175A - 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 zine oxide powder.
Background technology
Present studies show that in a large number: the size of the performance of material and its microtexture unit is closely related.With the reducing and sharply increase of its grain-size, make nano zine oxide produce the not available special effects of its body cake mass, as surface effects, small-size effect and macro quanta tunnel effect etc. due to the specific surface area of zinc oxide (ZnO).So nano zine oxide has the incomparable property of general body piece zinc oxide at aspects such as solar cell, electron device, nano-device, catalyzer, sensor, antibiotic and deodorizing.Therefore, the Zinc oxide powder that preparation size is even, monodispersity is good and have a nanoscale has become a significant challenge of researcher.Yet still the relevant size of rare document is reported less than the research of the nano zine 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 to provide a kind of preparation method of small size nano zine oxide powder, preparation method of the present invention is with low cost, operation simple and can prepare size less than the nano zine oxide powder of 10nm, the specific surface area of nano zine oxide powder is increased, have 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 kind of preparation method of small size nano zine 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, making its volumetric molar concentration is 0.0001mol/L～1.0mol/L, and divalent zinc salt solution magnetic agitation is heated to 65～78 ℃ and be 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 that makes NaOH is 0.001mol/L～1.0mol/L, making simultaneously the mol ratio of NaOH and divalent zinc salt is 50:1～1:1, is denoted as solution B;
Step 3: the solution B that step 2 is configured dropwise joins in solution A, remains magnetic agitation in the process that adds, and is heated under 65 ℃～78 ℃ and is incubated 0.01h～1h, obtains containing the solidliquid mixture of zinc oxide precipitation;
Step 4: the solidliquid mixture that contains zinc oxide precipitation that step 3 is obtained is used respectively deionized water and dehydrated alcohol centrifuge washing 3 times～5 times, then with the dry 1h～12h under 50 ℃～80 ℃ of the product after centrifuge washing, obtains the nano zine oxide powder.
The described divalent zinc salt of step 1 is zinc nitrate, zinc acetate, zinc sulfate or zinc chloride.
The present invention adopt a kind of cheaply, controllability and the good liquid phase synthesizing method of operability, by the regulation and control to zinc salt kind, reactant concn, temperature of reaction and reaction times, can prepare the nano zine oxide powder of the high and size uniform of output.The nano zine oxide powder that obtains be size less than 10nm, the specific surface area of nano zine oxide powder is increased, have excellent surface effects, small-size effect and macro quanta tunnel effect.
Description of drawings
Fig. 1 is the transmission electron micrograph of the nano zine oxide powder of embodiment one preparation.
Fig. 2 is the transmission electron micrograph of the nano zine oxide powder of embodiment two preparations.
Embodiment
The below is described in further detail structure of the present invention.
Embodiment 1
Embodiment one
The preparation method of a kind of small size nano zine oxide of the present embodiment powder 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 ℃ and be incubated 10 minutes, be denoted as solution A, the speed of magnetic agitation is 4000 rev/mins;
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, and this process keeps magnetic agitation to be heated to 75 ℃, and the speed of magnetic agitation is 4000 rev/mins, and insulation 0.5h, obtains containing the solidliquid mixture of zinc oxide precipitation;
Step 4: the solidliquid mixture that contains zinc oxide precipitation that step 3 is obtained is used respectively deionized water and dehydrated alcohol centrifuge washing 3 times, then with the dry 6h under 60 ℃ of the oxidized zinc products after centrifuge washing.
The present embodiment can obtain as shown in Figure 1 size less than the nano zine oxide powder of 10nm, and particle diameter mean value is 6.6nm.
Embodiment two
The preparation method of a kind of small size nano zine oxide of the present embodiment powder 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 ℃ and be incubated 5 minutes, be denoted as solution A, the speed of magnetic agitation is 3000 rev/mins;
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, and this process keeps magnetic agitation to be heated to 75 ℃, and the speed of magnetic agitation is 3000 rev/mins, and insulation 0.5h, obtains containing the solidliquid mixture of zinc oxide precipitation;
Step 4: the solidliquid mixture that contains zinc oxide precipitation that step 3 is obtained is used respectively deionized water and dehydrated alcohol centrifuge washing 3 times, then with the dry 5h under 60 ℃ of the oxidized zinc products after centrifuge washing.
The present embodiment can obtain as shown in Figure 2 size less than the nano zine oxide powder of 10nm, and its particle diameter mean value is 8.0nm.
Embodiment three
The preparation method of a kind of small size nano zine oxide of the present embodiment powder 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 ℃ and be incubated 7 minutes, be denoted as solution A, the speed of magnetic agitation is 3000 rev/mins;
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, and this process keeps magnetic agitation to be heated to 75 ℃, and the speed of magnetic agitation is 3000 rev/mins, and insulation 0.4h, obtains containing the solidliquid mixture of zinc oxide precipitation;
Step 4: the solidliquid mixture that contains zinc oxide precipitation that step 3 is obtained is used respectively deionized water and dehydrated alcohol centrifuge washing 4 times, then with the dry 3h under 70 ℃ of the oxidized zinc products after centrifuge washing.
Embodiment four
The preparation method of a kind of small size nano zine oxide of the present embodiment powder 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 ℃ and be incubated 5 minutes, be denoted as solution A, the speed of magnetic agitation is 2500 rev/mins;
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, and this process keeps magnetic agitation to be heated to 77 ℃, and the speed of magnetic agitation is 2500 rev/mins, and insulation 0.01h, obtains containing the solidliquid mixture of zinc oxide precipitation;
Step 4: the solidliquid mixture that contains zinc oxide precipitation that step 3 is obtained is used respectively deionized water and dehydrated alcohol centrifuge washing 4 times, then with the dry 12h under 50 ℃ of the oxidized zinc products after centrifuge washing.
Embodiment five
The preparation method of a kind of small size nano zine oxide of the present embodiment powder 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 ℃ and be incubated 1 minute, be denoted as solution A, the speed of magnetic agitation is 3000 rev/mins;
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, and this process keeps magnetic agitation to be heated to 65 ℃, and the speed of magnetic agitation is 3000 rev/mins, and insulation 1h, obtains containing the solidliquid mixture of zinc oxide precipitation;
Step 4: the solidliquid mixture that contains zinc oxide precipitation that step 3 is obtained is used respectively deionized water and dehydrated alcohol centrifuge washing 5 times, then with the dry 1h under 80 ℃ of the oxidized zinc products after centrifuge washing.
Claims (2)
1. the preparation method of a small size nano zine oxide powder, 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, making its volumetric molar concentration is 0.0001mol/L～1.0mol/L, and divalent zinc salt solution magnetic agitation is heated to 65 ℃～78 ℃ and be 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 that makes NaOH is 0.001mol/L～1.0mol/L, making simultaneously the mol ratio of NaOH and divalent zinc salt is 50:1～1:1, is denoted as solution B;
Step 3: the solution B that step 2 is configured dropwise joins in solution A, remains magnetic agitation in the process that adds, and is heated under 65 ℃～78 ℃ and is incubated 0.01h～1h, obtains containing the solidliquid mixture of zinc oxide precipitation;
Step 4: the solidliquid mixture that contains zinc oxide precipitation that step 3 is obtained is used respectively deionized water and dehydrated alcohol centrifuge washing 3 times～5 times, then with the dry 1h～12h under 50 ℃～80 ℃ of the product after centrifuge washing, obtains the nano zine oxide powder.
2. preparation method according to claim 1, it is characterized in that: the described divalent zinc salt of step 1 is zinc nitrate, zinc acetate, zinc sulfate or zinc chloride.
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Cited By (8)
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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 |
| CN104843767A (en) * | 2015-05-13 | 2015-08-19 | 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 |
| CN106830921A (en) * | 2017-01-23 | 2017-06-13 | 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 |
| CN111573712A (en) * | 2020-05-26 | 2020-08-25 | 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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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104843767A (en) * | 2015-05-13 | 2015-08-19 | 湖南尔康制药股份有限公司 | Preparation method of officinal nano-zinc oxide |
| 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 |
| CN106830921A (en) * | 2017-01-23 | 2017-06-13 | 九江学院 | A kind of ZnO transparent ceramics and preparation method thereof |
| 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 |
| CN111573712A (en) * | 2020-05-26 | 2020-08-25 | 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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Effective date of registration: 20230607 Address after: 225125 Yangzhou Environmental Protection Entrepreneurship Park, Suzhou City, Jiangsu Province Patentee after: Yangzhou love new Mstar Technology Ltd. Address before: 710049 No. 28, Xianning Road, Xi'an, Shaanxi Patentee before: XI'AN JIAOTONG University |