CN1807254A - Zinc oxide hollow microsphere preparation method - Google Patents
Zinc oxide hollow microsphere preparation method Download PDFInfo
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- CN1807254A CN1807254A CN 200610003991 CN200610003991A CN1807254A CN 1807254 A CN1807254 A CN 1807254A CN 200610003991 CN200610003991 CN 200610003991 CN 200610003991 A CN200610003991 A CN 200610003991A CN 1807254 A CN1807254 A CN 1807254A
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Abstract
The invention provides a zinc oxide hollow microsphere preparation method, which consists of charging strong acid cationic ion-exchange resin into aqueous solution of zinc salts, oscillating 2-8 hours, and filtering, drying the filtered strong acid cationic ion-exchange resin at 60-100 deg C for 2-10 hours, sintering 2-8 hours at 450-90 deg. C, thus obtaining the zinc oxide hollow microballoon.
Description
(1) technical field:
The present invention relates to a kind of preparation method of metal oxide hollow microballoon, mainly relate to a kind of preparation method of Zinc oxide hollow microsphere.
(2) background technology:
Zinc oxide has higher chemical stability and thermostability, is used in various fields such as gas sensitive, photonic material, pottery, coating, catalysis as a kind of traditional functional materials.As utilize the broad stopband of zinc oxide, can obtain the emission from the redness to the ultraviolet, thereby zinc oxide there is good application prospects as aspects such as ultraviolet emission device under normal temperature and the high temperature and Ultra-Violet Laser devices.In recent years, the report of relevant Zinc oxide powder preparation and performance study thereof is more.Zinc oxide hollow microsphere is because its specific surface area is bigger, and is active higher, be expected to be widely used in fields such as chemistry, biological, material and environmental pollutant processing, but the preparation of at present relevant Zinc oxide hollow microsphere and study rarely found report.
(3) summary of the invention:
The object of the present invention is to provide the preparation method that a kind of cost is low, simple to operate, be fit to the Zinc oxide hollow microsphere of suitability for industrialized production.
For achieving the above object, the preparation method of Zinc oxide hollow microsphere of the present invention is: strong-acid cation-exchange resin is joined in the zinc salt solution, vibrated 2-8 hour, filter then; With the strong-acid cation-exchange resin after filtering under 60 ℃-100 ℃ temperature dry 2-10 hour; 450 ℃-900 ℃ roasting temperature 2-8 hour.
Wherein the concentration of zinc salt solution is 0.4-1M.
Wherein strong-acid cation-exchange resin is the hydrogen type strong acid Zeo-karb.
Owing to taked technique scheme, with the strong-acid cation-exchange resin template, by zine ion is switched directly on the strong-acid cation-exchange resin, prepared Zinc oxide hollow microsphere after drying, the roasting.The preparation method of this kind Zinc oxide hollow microsphere has advantages such as low, simple to operate, the suitable suitability for industrialized production of cost.Detection shows: the zinc oxide microballoon of the present invention's preparation is hollow structure, and diameter is a micron order, and its surface is made up of the nano zine oxide crystal grain ordered arrangement of densification.This kind Zinc oxide hollow microsphere has good catalytic performance and fluorescent emission performance, is expected to be widely used in fields such as chemistry, biology, material and environmental pollutant processing.We with this kind Zinc oxide hollow microsphere as photocatalyst, with organic dye such as tropeolin-Ds is research object, carry out the photochemical catalysis experiment under high voltage mercury lamp or solar light irradiation, the result shows: compare as photocatalyst with Zinc oxide powder, the Zinc oxide hollow microsphere photocatalytic activity obviously improves.
(4) description of drawings:
Fig. 1 is the prepared Zinc oxide hollow microsphere sem photograph of the preparation method of Zinc oxide hollow microsphere of the present invention.
(5) embodiment:
Below in conjunction with embodiment the present invention is described in further detail.
Embodiment one
Restraining sodium type strong-acid cation-exchange resins with 10 in beaker is to soak 2 times in 8% sulphuric acid soln at 250 milliliters of weight percents, each 2 hours, with other positively charged ion in the hydrogen ion wholly replace sodium type strong-acid cation-exchange resin, use deionized water thorough washing, drying then, can obtain the hydrogen type strong acid Zeo-karb.In beaker, 10 gram hydrogen type strong acid Zeo-karbs are joined in 250 milliliters, the zinc nitrate solution of 0.5M, M is a volumetric molar concentration, and on oscillator, shook 6 hours, the hydrogen ion on zine ion and the hydrogen type strong acid Zeo-karb is fully exchanged, filter then; With exchange and the hydrogen type strong acid Zeo-karb after filtering put into baking oven under 100 ℃ temperature dry 2 hours, remove moisture; Then in muffle furnace with 730 ℃ of roastings 4 hours, get final product 3.9 gram left and right sides Zinc oxide hollow microspheres.Measurement result: the Zinc oxide hollow microsphere of preparation by day island proper Tianjin-6000X x ray diffractometer x analyzed the zinc oxide crystal formation, the Holland Philips XL30 of company scanning electron microscopic observation the microsphere surface pattern, the result shows: as seen from Figure 1, prepared zinc oxide microballoon, be hollow structure, diameter between 300-500 μ m, belongs to hexagonal system greatly.
Embodiment two
Restraining sodium type strong-acid cation-exchange resins with 10 in beaker is to soak 2 times in 8% hydrochloric acid soln at 250 milliliters of weight percents, each 2 hours, with other positively charged ion in the hydrogen ion wholly replace sodium type strong-acid cation-exchange resin, use deionized water thorough washing, drying then, can obtain the hydrogen type strong acid Zeo-karb.In beaker, 10 gram hydrogen type strong acid Zeo-karbs are joined in 250 milliliters, the zinc acetate solution of 0.4M, and placed on the oscillator concussion 6 hours, the hydrogen ion on zine ion and the hydrogen type strong acid Zeo-karb is fully exchanged, then filtration; With exchange and the hydrogen type strong acid Zeo-karb after filtering put into baking oven under 60 ℃ temperature dry 10 hours, remove moisture; Then in muffle furnace with 900 ℃ of roastings 2 hours, get final product 3.8 gram left and right sides Zinc oxide hollow microspheres.Measurement result: the Zinc oxide hollow microsphere of preparation by day island proper Tianjin-6000X x ray diffractometer x analyzed the zinc oxide crystal formation; The Holland Philips XL30 of company scanning electron microscopic observation the microsphere surface pattern, the result shows: prepared zinc oxide microballoon is hollow structure, diameter between 300-500 μ m, belongs to hexagonal system greatly.
Embodiment three
In beaker, 10 gram sodium type strong-acid cation-exchange resins are joined in 250 milliliters, the solution of zinc sulfate of 0.5M, and concussion 5 hours on oscillator, the sodium ion on zine ion and the sodium type strong-acid cation-exchange resin is fully exchanged, then filtration; With exchange and the sodium type strong-acid cation-exchange resin after filtering put into baking oven under 90 ℃ temperature dry 6 hours, remove moisture; Then in muffle furnace with 600 ℃ of roastings 5 hours, get final product 3.7 gram left and right sides Zinc oxide hollow microspheres.Measurement result: the Zinc oxide hollow microsphere of preparation by day island proper Tianjin-6000X x ray diffractometer x analyzed the zinc oxide crystal formation, the Holland Philips XL30 of company scanning electron microscopic observation the microsphere surface pattern, the result shows: prepared zinc oxide microballoon is hollow structure, diameter between 300-500 μ m, belongs to hexagonal system greatly.
Embodiment four
In beaker, 2 gram sodium type strong-acid cation-exchange resins are joined in 250 milliliters, the solution of zinc sulfate of 0.1M, and concussion 8 hours on oscillator, the sodium ion on zine ion and the sodium type strong-acid cation-exchange resin is fully exchanged, then filtration; With exchange and the sodium type strong-acid cation-exchange resin after filtering put into baking oven under 90 ℃ temperature dry 4 hours, remove moisture; Then in muffle furnace with 550 ℃ of roastings 6 hours, get final product 0.7 gram left and right sides Zinc oxide hollow microsphere.Measurement result: the Zinc oxide hollow microsphere of preparation by day island proper Tianjin-6000X x ray diffractometer x analyzed the zinc oxide crystal formation, the Holland Philips XL30 of company scanning electron microscopic observation the microsphere surface pattern, the result shows: prepared zinc oxide microballoon is hollow structure, diameter between 300-500 μ m, belongs to hexagonal system greatly.
Embodiment five
In beaker, 10 gram hydrogen type strong acid Zeo-karbs are joined in 250 milliliters, the solution of zinc sulfate of 1M, and concussion 4 hours on oscillator, the hydrogen ion on zine ion and the hydrogen type strong acid Zeo-karb is fully exchanged, then filtration; With exchange and the hydrogen type strong acid Zeo-karb after filtering put into baking oven under 70 ℃ temperature dry 9 hours, remove moisture; Then in muffle furnace with 450 ℃ of roastings 8 hours, get final product 4.1 the gram about Zinc oxide hollow microsphere.Measurement result: the Zinc oxide hollow microsphere of preparation by day island proper Tianjin-6000X x ray diffractometer x analyzed the zinc oxide crystal formation, the Holland Philips XL30 of company scanning electron microscopic observation the microsphere surface pattern, the result shows: prepared zinc oxide microballoon is hollow structure, and diameter is greatly between 300-500 μ m.
Embodiment six
In beaker, 10 gram sodium type strong-acid cation-exchange resins are joined in 250 milliliters, the liquor zinci chloridi of 10M, and concussion 2 hours on oscillator, the sodium ion on zine ion and the sodium type strong-acid cation-exchange resin is fully exchanged, then filtration; With exchange and the sodium type strong-acid cation-exchange resin after filtering put into baking oven under 70 ℃ temperature dry 8 hours, remove moisture; Then in muffle furnace with 650 ℃ of roastings 4 hours, get final product 3.7 gram left and right sides Zinc oxide hollow microspheres.Measurement result: the Zinc oxide hollow microsphere of preparation by day island proper Tianjin-6000X x ray diffractometer x analyzed the zinc oxide crystal formation, the Holland Philips XL30 of company scanning electron microscopic observation the microsphere surface pattern, the result shows: prepared zinc oxide microballoon is hollow structure, and diameter is greatly between 300-500 μ m.
Claims (3)
1, a kind of preparation method of Zinc oxide hollow microsphere:
Strong-acid cation-exchange resin is joined in the zinc salt solution, vibrated 2-8 hour, filter then; With the strong-acid cation-exchange resin after filtering under 60 ℃-100 ℃ temperature dry 2-10 hour; 450 ℃-900 ℃ roasting temperature 2-8 hour.
2, the preparation method of Zinc oxide hollow microsphere according to claim 1, wherein the concentration of zinc salt solution is 0.4-1M.
3, the preparation method of Zinc oxide hollow microsphere according to claim 1, wherein strong-acid cation-exchange resin is the hydrogen type strong acid Zeo-karb.
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| CNB2006100039914A CN100357186C (en) | 2006-01-26 | 2006-01-26 | Zinc oxide hollow microsphere preparation method |
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| CNB2006100039914A CN100357186C (en) | 2006-01-26 | 2006-01-26 | Zinc oxide hollow microsphere preparation method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101559974B (en) * | 2009-05-14 | 2010-08-18 | 浙江理工大学 | Method for preparing zinc oxide hollow microspheres |
| CN101311119B (en) * | 2007-05-25 | 2010-09-08 | 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 |
| WO2010121488A1 (en) | 2009-04-21 | 2010-10-28 | 河北勇龙邦大新材料有限公司 | Method and device for producing hollow microspheres |
| CN102101695A (en) * | 2011-04-07 | 2011-06-22 | 青岛科技大学 | Preparation method of hierarchical structural zinc oxide hollow microsphere |
| CN111715308A (en) * | 2020-06-10 | 2020-09-29 | 安庆师范大学 | ZnO/carbonized ion exchange resin and preparation method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1211280C (en) * | 2002-12-11 | 2005-07-20 | 中国石油化工股份有限公司 | Process of preparing hollow zeolite microsphere |
-
2006
- 2006-01-26 CN CNB2006100039914A patent/CN100357186C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101311119B (en) * | 2007-05-25 | 2010-09-08 | 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 |
| WO2010121488A1 (en) | 2009-04-21 | 2010-10-28 | 河北勇龙邦大新材料有限公司 | Method and device for producing hollow microspheres |
| CN101559974B (en) * | 2009-05-14 | 2010-08-18 | 浙江理工大学 | Method for preparing zinc oxide hollow microspheres |
| CN102101695A (en) * | 2011-04-07 | 2011-06-22 | 青岛科技大学 | Preparation method of hierarchical structural zinc oxide hollow microsphere |
| CN111715308A (en) * | 2020-06-10 | 2020-09-29 | 安庆师范大学 | ZnO/carbonized ion exchange resin and preparation method thereof |
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| CN100357186C (en) | 2007-12-26 |
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