CN101723437B - Method for preparing porous laminated zinc oxide sphere - Google Patents
Method for preparing porous laminated zinc oxide sphere Download PDFInfo
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- CN101723437B CN101723437B CN2009102596583A CN200910259658A CN101723437B CN 101723437 B CN101723437 B CN 101723437B CN 2009102596583 A CN2009102596583 A CN 2009102596583A CN 200910259658 A CN200910259658 A CN 200910259658A CN 101723437 B CN101723437 B CN 101723437B
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Abstract
The invention provides a method for preparing a porous laminated zinc oxide sphere. The method comprises the following steps: (1) dissolving glucose in aqueous solution of zinc salt to obtain mixed solution, wherein the concentration of the glucose in the mixed solution is between 0.05 and 0.2g/ml, and the concentration of zinc ions in the mixed solution is between 0.02 and 0.2mol/L; (2) filling the mixed solution in a reaction kettle, heating the mixed solution to between 120 and 140 DEG C, cooling the mixed solution to room temperature after the mixed solution reacts for 60 to 240 minutes; (3) after the product is taken out, dripping ammonia water into the solution while stirring until the pH value of the solution reaches 10 to 11, and heating the solution to between 80 and 90 DEG C, preserving the heat for 10 to 60 minutes, and naturally cooling the solution to room temperature; and (4) finally, calcining the solution at the temperature of between 400 and 600 DEG C for 30 to 120 minutes through washing, vacuum filtering and drying to obtain the porous laminated zinc oxide sphere. The method has the advantages of simple required equipment, simple production technology and low cost.
Description
Technical field
The present invention relates to a kind of preparation method of zinc oxide sphere, especially relate to a kind of preparation method of porous laminated zinc oxide sphere.
Background technology
ZnO is a kind of semiconductor material with piezoelectricity and photoelectric characteristic, and its structure is hexagonal (wurtzite) structure.Its energy gap at normal temperatures is 3.37eV, is typical direct band gap wide bandgap semiconductor, and ZnO at room temperature has the exciton binding energy up to 60meV.ZnO has higher conductivity, and chemicalstability is good, and material source is very abundant; Cheap, nontoxic, be prone to realize mixing; These excellent specific properties that ZnO has make it show noticeable application prospect at aspects such as photoabsorption, sensitivity, catalysis and other functional performances.
A large amount of in recent years research concentrates on the Zinc oxide particles of preparation different-shape and structure.And vesicular structure has a wide range of applications in fields such as support of the catalyst, pharmaceutical capsule, microreactors owing to having character such as low density, high-ratio surface.
Report and patented technology that many Zinc oxide hollow spheres have been arranged at present.Use maximum methods such as vapour deposition process, template that have.Wherein " vapour deposition process " is to obtain hollow structure through gas-phase reaction under the high temperature and deposition process.But temperature of reaction is high, and required equipment is expensive, needs atmosphere protection, so production cost is high, is inappropriate for scale prodn." template " promptly used zinc powder (Chinese invention patent: CN200710171003, a kind of method for preparing zinc oxide nano hollow spheres through caustic corrosion reaction; CN200510025825; With the zinc powder is the preparation method of the Zinc oxide hollow spheres of raw material), resin (Chinese invention patent: CN200610003991; The preparation method of Zinc oxide hollow microsphere) etc. be template, coat or surface reaction, obtain hollow ball through the surface; But gained zinc oxide sphere size is nano level mostly, and hollow ball is the individual layer spheroid.So far, still do not see the report of relevant layered porous zinc oxide sphere.
Summary of the invention
The technical problem that the present invention will solve provides a kind of porous laminated zinc oxide sphere preparation method; This method is a raw material with zinc salt, glucose and ammoniacal liquor, can obtain micron-sized layered porous zinc oxide sphere, and diameter dimension is between 3-10 μ m; Simultaneously, this method equipment input is little, technology is simple, cost is low, is suitable for large-scale industrial production.
For solving the problems of the technologies described above, the preparation method of a kind of layered porous zinc oxide sphere of the present invention comprises the steps:
(1) glucose is dissolved in the zinc salt solution, get mixed solution; Glucose concn in the said mixed solution is 0.05-0.6g/mL, and the zinc ion concentration in the said mixed solution is 0.02-0.2mol/L;
(2) above-mentioned mixed solution is packed in the reaction kettle, be heated to 120-140 ℃, behind the reaction 60-240min, be cooled to room temperature;
(3) dropping ammonia in solution while stirring reaches 10-11 until the pH value; Then solution is heated to 80-90 ℃, and insulation naturally cooled to room temperature after 10-60 minute;
(4) last, through washing, suction filtration and drying, 400-600 ℃ of calcining 30-120 minute down, get final product porous laminated zinc oxide sphere.
Further, said zinc salt is the mixture of one or more arbitrary proportions in zinc nitrate, zinc sulfate, zinc acetate, the zinc oxalate.
The present invention has following beneficial effect:
(1) be raw material with zinc salt, glucose and ammoniacal liquor, with low cost;
(2) this preparation has advantages such as reaction conditions gentleness, required equipment is simple, technological operation is simple.
Description of drawings
Fig. 1 is ESEM (SEM) photo of instance 1 prepared layered porous zinc oxide sphere.
Fig. 2 is the X ray diffracting spectrum of instance 1 prepared layered porous zinc oxide sphere.
Fig. 3 is instance 1 a prepared layered porous zinc oxide sphere EDS power spectrum.
Embodiment
In order to show substantive distinguishing features of the present invention and marked improvement, further specify embodiment and effect with following indefiniteness embodiment.
Embodiment 1
A kind of preparation method of layered porous zinc oxide sphere comprises the steps:
(1) glucose is dissolved in the zinc nitrate aqueous solution, get mixed solution; Glucose concn in the said mixed solution is 0.1g/mL, and the zinc ion concentration in the said mixed solution is 0.05mol/L;
(2) above-mentioned mixed solution is packed in the reaction kettle, be heated to 130 ℃, react after 180 minutes, be cooled to room temperature;
(3) dropping ammonia in mixed solution while stirring reaches 10.5 until the pH value; Then mixed solution is heated to 80-90 ℃, and is incubated 60 minutes; Then, naturally cool to room temperature;
(4) product is taken out, after washing, suction filtration and drying, 600 ℃ of calcinings got final product in 2 hours porous laminated zinc oxide sphere.
Characterize (Fig. 1) through sem, the diameter of zinc oxide porous ball is at 2-12um, and has tangible porous laminated structure.Obtain its structure through X-ray diffraction analysis and belong to six side's phase oxidation zinc structures (Fig. 2).Obtain prepared zinc oxide through the EDS energy spectrum analysis and do not contain other element, have high purity (Fig. 3).
A kind of preparation method of porous laminated zinc oxide sphere comprises the steps:
(1) glucose is dissolved in the zinc sulfate solution, get mixed solution; Glucose concn in the said mixed solution is 0.05g/mL, and the zinc ion concentration in the said mixed solution is 0.06mol/L;
(2) above-mentioned mixed solution is packed in the reaction kettle, be heated to 140 ℃, be incubated after 240 minutes, be cooled to room temperature;
(3) dropping ammonia in mixed solution while stirring reaches 11 until the pH value, then mixed solution is heated to 90 ℃, and is incubated 10 minutes; Then, mixed solution is naturally cooled to room temperature;
(4) product is taken out, through washing, suction filtration and drying process, then 500 ℃ of calcinings got final product in 2 hours porous laminated zinc oxide sphere.
Embodiment 3
A kind of preparation method of porous laminated zinc oxide sphere comprises the steps:
(1) glucose is dissolved in the zinc acetate aqueous solution, get mixed solution; Glucose concn in the said mixed solution is 0.05g/mL, and the zinc ion concentration in the said mixed solution is 0.2mol/L;
(2) above-mentioned mixed solution is packed in the reaction kettle, be heated to 120 ℃, reacted 60 minutes, be cooled to room temperature;
(3) dropping ammonia in mixed solution while stirring reaches 10.5 until the pH value, then mixed solution is heated to 90 ℃, and is incubated 15 minutes; Then, solution is naturally cooled to room temperature;
(4) product is taken out, through washing, suction filtration and drying process, then 400 ℃ of calcinings got final product in 2 hours porous laminated zinc oxide sphere.
A kind of preparation method of porous laminated zinc oxide sphere comprises the steps:
(1) glucose is dissolved in zinc acetate and the zinc oxalate mixed aqueous solution, get mixed solution; The mol ratio of zinc acetate and zinc oxalate is that 3: 7 glucose concn in the said mixed solution are 0.6g/mL, and the zinc ion concentration in the said mixed solution is 0.05mol/L;
(2) above-mentioned mixed solution is packed in the reaction kettle, be heated to 130 ℃, reacted 180 minutes, be cooled to room temperature;
(3) dropping ammonia in mixed solution while stirring reaches 11 until the pH value, then mixed solution is heated to 90 ℃, and is incubated 30 minutes; Then, solution is naturally cooled to room temperature;
(4) product is taken out, through washing, suction filtration and drying process, then 600 ℃ of calcinings got final product in 2 hours porous laminated zinc oxide sphere.
Embodiment 5
A kind of preparation method of porous laminated zinc oxide sphere comprises the steps:
(1) glucose is dissolved in the mixed aqueous solution of zinc nitrate, zinc sulfate and zinc acetate, get mixed solution; The mol ratio of zinc nitrate, zinc sulfate and zinc acetate is 6: 3: 1.Glucose concn in the said mixed solution is 0.07g/mL, and the zinc ion concentration in the said mixed solution is 0.05mol/L;
(2) above-mentioned mixed solution is packed in the reaction kettle, be heated to 130 ℃, be incubated 180 minutes, be cooled to room temperature;
(3) dropping ammonia in mixed solution while stirring reaches 11 until the pH value, then mixed solution is heated to 85 ℃, and is incubated 60 minutes; Then, solution is naturally cooled to room temperature;
(4) product is taken out, through washing, suction filtration and drying process, then 600 ℃ of calcinings got final product in 2 hours porous laminated zinc oxide sphere.
A kind of preparation method of porous laminated zinc oxide sphere comprises the steps:
(1) glucose is dissolved in the mixed aqueous solution of zinc nitrate, zinc sulfate, zinc acetate and zinc oxalate, get mixed solution; The mol ratio of zinc nitrate, zinc sulfate, zinc acetate and zinc oxalate is: 2: 3: 3: 2; Glucose concn in the said mixed solution is 0.06g/mL, and the zinc ion concentration in the said mixed solution is 0.06mol/L;
(2) above-mentioned mixed solution is packed in the reaction kettle, be heated to 140 ℃, reacted 240 minutes, be cooled to room temperature;
(3) dropping ammonia in mixed solution while stirring reaches 10 until the pH value, then mixed solution is heated to 90 ℃, and is incubated 50 minutes, and solution is naturally cooled to room temperature;
(4) product is taken out, through washing, suction filtration and drying process, then 550 ℃ of calcinings got final product in 2 hours porous laminated zinc oxide sphere.
Obviously, the above embodiment of the present invention only be for clearly the present invention is described and is done for example, and be not to be qualification to embodiment of the present invention.For the those of ordinary skill in affiliated field, on the basis of above-mentioned explanation, can also make other multi-form variation or change.Here can't give exhaustive to all embodiments.Everyly belong to the row that conspicuous variation that technical scheme of the present invention extends out or change still are in protection scope of the present invention.
Claims (1)
1. a porous laminated zinc oxide sphere preparation method is characterized in that, comprises the steps:
(1) glucose is dissolved in the zinc salt solution, get mixed solution; Glucose concn in the said mixed solution is 0.05-0.6g/mL, and the zinc ion concentration in the said mixed solution is 0.02-0.2mol/L;
(2) above-mentioned mixed solution is packed in the reaction kettle, be heated to 120-140 ℃, behind the reaction 60-240min, be cooled to room temperature;
(3) dropping ammonia in mixed solution while stirring reaches 10-11 until the pH value; Then mixed solution is heated to 80-90 ℃, and insulation naturally cooled to room temperature after 10-60 minute;
(4) last, through washing, suction filtration and drying, 400-600 ℃ of calcining 30-120 minute down, get final product porous laminated zinc oxide sphere;
Said zinc salt is the mixture of one or more arbitrary proportions in zinc nitrate, zinc sulfate, zinc acetate, the zinc oxalate.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103318941B (en) * | 2012-09-12 | 2014-09-03 | 上海工程技术大学 | Synthetic method of porous ZnO three-dimensional superstructure assembled by nano-sheets |
| CN107082445A (en) * | 2016-02-14 | 2017-08-22 | 云南民族大学 | A kind of fast preparation method of polycrystalline ZnO powders |
| CN109873147B (en) * | 2019-03-04 | 2021-08-24 | 湘潭大学 | Carbon-modified porous ZnO nano material and preparation method and application thereof |
| CN111333102A (en) * | 2020-04-22 | 2020-06-26 | 安徽锦华氧化锌有限公司 | Preparation method of zinc oxide for sulfur removal agent |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101311119A (en) * | 2007-05-25 | 2008-11-26 | 中国科学院合肥物质科学研究院 | Reticular nano hole zinc oxide micron hollow ball and preparation method thereof |
| CN101497457A (en) * | 2009-02-27 | 2009-08-05 | 天津大学 | Method for preparing nano zinc oxide compound powder using natural polysaccharide |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101311119A (en) * | 2007-05-25 | 2008-11-26 | 中国科学院合肥物质科学研究院 | Reticular nano hole zinc oxide micron hollow ball and preparation method thereof |
| CN101497457A (en) * | 2009-02-27 | 2009-08-05 | 天津大学 | Method for preparing nano zinc oxide compound powder using natural polysaccharide |
Non-Patent Citations (5)
| Title |
|---|
| JIAGUO YU et al..Hydrothermal Synthesis and Photocatalytic Activity of Zinc Oxide Hollow Spheres.《ENVIRONMENTAL SCIENCE & TECHNOLOGY》.2008,第42卷(第13期),4902-4907. |
| JIAGUO YU et al..Hydrothermal Synthesis and Photocatalytic Activity of Zinc Oxide Hollow Spheres.《ENVIRONMENTAL SCIENCE & * |
| Jun Zhang et al..ZnO hollow spheres: Preparation, characterization, and gas sensing properties.《Sensors and Actuators B》.2009,第139卷411-417. * |
| TECHNOLOGY》.2008,第42卷(第13期),4902-4907. * |
| 邓文雅等.氧化锌空心球的制备及光致发光特征.《功能材料》.2007,第38卷(第9期),1559-1562. * |
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