CN1239395C - Process for preparing nano zinc oxide material - Google Patents
Process for preparing nano zinc oxide material Download PDFInfo
- Publication number
- CN1239395C CN1239395C CN 02109078 CN02109078A CN1239395C CN 1239395 C CN1239395 C CN 1239395C CN 02109078 CN02109078 CN 02109078 CN 02109078 A CN02109078 A CN 02109078A CN 1239395 C CN1239395 C CN 1239395C
- Authority
- CN
- China
- Prior art keywords
- zinc oxide
- oxide material
- nanometer zinc
- raw materials
- mixed solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 19
- 239000000463 material Substances 0.000 title claims abstract description 16
- 238000004519 manufacturing process Methods 0.000 title 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 27
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 4
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000001354 calcination Methods 0.000 claims abstract description 3
- 239000000706 filtrate Substances 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- AZHSSKPUVBVXLK-UHFFFAOYSA-N ethane-1,1-diol Chemical compound CC(O)O AZHSSKPUVBVXLK-UHFFFAOYSA-N 0.000 claims description 2
- 235000012204 lemonade/lime carbonate Nutrition 0.000 claims description 2
- 238000000197 pyrolysis Methods 0.000 claims description 2
- 238000010792 warming Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 14
- 238000006243 chemical reaction Methods 0.000 abstract description 11
- 239000000047 product Substances 0.000 abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 6
- 230000002776 aggregation Effects 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 239000002904 solvent Substances 0.000 abstract description 4
- 239000000919 ceramic Substances 0.000 abstract description 3
- 239000012065 filter cake Substances 0.000 abstract description 3
- 239000011521 glass Substances 0.000 abstract description 3
- 238000001035 drying Methods 0.000 abstract description 2
- 239000000835 fiber Substances 0.000 abstract description 2
- 239000011259 mixed solution Substances 0.000 abstract 3
- 239000002994 raw material Substances 0.000 abstract 3
- 238000004220 aggregation Methods 0.000 abstract 1
- 239000002537 cosmetic Substances 0.000 abstract 1
- 238000003746 solid phase reaction Methods 0.000 abstract 1
- 238000005979 thermal decomposition reaction Methods 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 238000005054 agglomeration Methods 0.000 description 4
- 239000007791 liquid phase Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000000498 ball milling Methods 0.000 description 3
- 230000001954 sterilising effect Effects 0.000 description 3
- 238000004659 sterilization and disinfection Methods 0.000 description 3
- 239000011701 zinc Substances 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000011858 nanopowder Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 2
- 206010013786 Dry skin Diseases 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000006136 alcoholysis reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000012254 powdered material Substances 0.000 description 1
- 230000002940 repellent Effects 0.000 description 1
- 239000005871 repellent Substances 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000004317 sodium nitrate Substances 0.000 description 1
- 229940001516 sodium nitrate Drugs 0.000 description 1
- 235000010344 sodium nitrate Nutrition 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000001149 thermolysis Methods 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention discloses a preparation process of nanometer zinc oxide material, which relates to the nanometer zinc oxide material and the preparation process thereof. The present invention mainly adopts a gas-solid phase reaction method, and zinc nitrate Zn(NO3)2 and sodium hydroxide NaOH as main raw materials; the raw materials are mixed and ground at normal temperature, and mixed solution is obtained by the thermal decomposition of the raw materials; then, deionized water and ethanol are added in the mixed solution for washing, then the mixed solution is filtered, and the powdery nanometer zinc oxide material is obtained by drying and calcining filter cake. The present invention has the advantages of small energy consumption, simple equipment, no aggregation phenomenon, no need of solvent, high yield and controllable reaction conditions; the prepared nanometer zinc oxide material is applied to the products in the fields of fiber, glass, ceramic, cosmetic, etc., the light property, the electric property, the magnetic property, etc. of the existing products can be changed greatly, and the application range of the products in the existing fields can be expanded.
Description
Technical field
The present invention relates to nano zinc oxide material and preparation method thereof.
Background technology
Nano zinc oxide material is a kind of nanosize metal oxide powder, grain-size is below 100nm, particulate state is spherical, appearance color is flaxen powder, possesses the not available light of common zinc oxide block materials,, magnetic, heat, performances such as sensitivity, be widely used in rubber industry, improve the coke burning performance of rubber item, improve the wear resistance of rubber product, be applied to ceramic industry, reduce the clean temperature of burning of ceramic, and generation sterilization, self-cleaning effect is applied to glass industry, in the time of shielding ultraviolet rays, all right sterilization, self-cleaning, be applied to weave and the product of day chemical industry, have antibiotic, sterilization, the de-odorised function.In addition, nano zine oxide all has extremely important application in numerous inside, field such as chemical industry catalysis, gas sensing, image recording, building decoration, germ repellent paint, radar wave absorption and conduction, luminescent materials.
Along with going deep into to the nano-powder performance study, the preparation method of nano-powder arises at the historic moment, and summarizes to get up can be divided into physics method and chemical method, and its physics method majority will use high valuable instrument, equipment, energy consumption is also very huge, we can say still blank in China.Chemical method mainly contains colloidal sol---gel method, micro emulsion method, chemical precipitation method, alcoholysis method etc.Though each tool relative merits and characteristics all are to carry out in liquid phase.The common feature of prepared in reaction nano-ZnO has two in the liquid phase, one, and agglomeration is difficult to overcome in the reaction.Its two, concentration of reactants lower (efficient is low).Produce the shortcoming of nano-ZnO in order to overcome liquid phase method, low temperature solid-phase coordination chemical reaction method occurred, have the shortcoming of agglomeration though this method has overcome liquid phase method, and possess the solvent of need not, productive rate advantages of higher from the early 1990s.But equally also exist shortcoming: owing to will make reactant spread the generation chemical reaction mutually by ball milling, therefore it brings equal chance will inevitably for the generation of product nuclear and the growth of nucleus, so there will be two kinds of situations: one, the ball milling deficiency of time causes reaction not exclusively.Its two, ball milling is excessive, the nucleus growth process is fast, thereby causes the unmanageable shortcoming of reaction conditions.For overcoming the shortcoming of above-mentioned low temperature homophase reaction method, keep wherein advantage again simultaneously, we have invented gas-solid reaction process on this method basis.
Summary of the invention
The preparation method of the nano zinc oxide material that the purpose of this invention is to provide that a kind of energy consumption is little, equipment is simple, do not have agglomeration, need not solvent, productive rate height, reaction conditions can be controlled.
Technical solution of the present invention is, under normal temperature, the normal pressure, with zinc nitrate Zn (NO
3)
2Mix with sodium hydroxide NaOH mill, be warming up at 360 ℃～400 ℃ and carry out pyrolysis, be cooled to 60 ℃～80 ℃, add deionized water and wash, wash with ethanol alcohol again, after filtration, add lime carbonate in the filtrate, be dried to granular, 650 ℃～800 ℃ down calcinings, grind then, disperse, obtain nano zinc oxide material.
Make nano zinc oxide material, press mass ratio, wherein, sodium hydroxide NaOH is 71～72.7%, zinc nitrate Zn (NO
3)
2Be 27.3～29%.
The invention has the beneficial effects as follows that energy consumption is little, equipment is simple, do not have agglomeration, need not solvent, productive rate height, reaction conditions can be controlled.The nano zinc oxide material of preparation is applied on the product in fields such as fiber, glass, pottery, makeup, can change the performances such as light, electricity, magnetic of existing product widely, enlarges the range of application of original field product.
Embodiment
The present invention is further illustrated below in conjunction with embodiment,
Press mass ratio, with 72.7% sodium hydroxide NaOH, 27.3% zinc nitrate Zn (NO
3)
2Mix at normal temperatures, mill mixed after 40 minutes, heated to 380 ℃ and carried out thermolysis, obtained zinc oxide, SODIUMNITRATE NaNO
3Mixing solutions, be cooled to 70 ℃, add 5% deionized water and wash, sedimentation and filtration obtains containing the filter cake of ZnO.Filter cake is cooled to 35 ℃, adds 10% ethanol and carries out alcohol and washed 5 hours, and filter under normal pressure, adds The addition of C aCO in the filtrate
3, alcohol is washed cake 45 ℃ of dryings 2 hours, calcines at 750 ℃ then, can obtain the nano zine oxide powdered material.
Claims (1)
1. the preparation method of nano zinc oxide material is characterized in that, under normal temperature, the normal pressure, press mass ratio, the zinc nitrate with 27.3～29% and 71～72.7% sodium hydroxide mill mixes, be warming up to 360 ℃～400 ℃ carry out pyrolysis after, be cooled to 60 ℃～80 ℃, add deionized water and wash, wash with ethanol alcohol again, after filtration, add lime carbonate in the filtrate, be dried to granular, 650 ℃～800 ℃ down calcinings, grind then, disperse, obtain nano zinc oxide material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02109078 CN1239395C (en) | 2002-01-22 | 2002-01-22 | Process for preparing nano zinc oxide material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02109078 CN1239395C (en) | 2002-01-22 | 2002-01-22 | Process for preparing nano zinc oxide material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1433966A CN1433966A (en) | 2003-08-06 |
| CN1239395C true CN1239395C (en) | 2006-02-01 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 02109078 Expired - Fee Related CN1239395C (en) | 2002-01-22 | 2002-01-22 | Process for preparing nano zinc oxide material |
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| Country | Link |
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| CN (1) | CN1239395C (en) |
Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1305773C (en) * | 2004-11-16 | 2007-03-21 | 浙江大学 | Preparation for zinc oxide nanometer material |
| CN100509612C (en) * | 2005-10-10 | 2009-07-08 | 中国科学院合肥物质科学研究院 | Single crystal zinc oxide nano yarn array/polycrystalline aluminum substrate composite and preparation method thereof |
| CN100344542C (en) * | 2005-12-16 | 2007-10-24 | 厦门大学 | Method for inhibiting C axial growth of zinc oxide nano-wire |
| CN100503741C (en) * | 2006-05-12 | 2009-06-24 | 中国科学院理化技术研究所 | Dumbbell-shaped zinc oxide particles, preparation method and use thereof |
| CN100408480C (en) * | 2006-07-26 | 2008-08-06 | 中国科学院上海硅酸盐研究所 | A kind of preparation method of nano zinc oxide powder |
| CN100357499C (en) * | 2006-07-26 | 2007-12-26 | 北京科技大学 | Method of preparing room temperature ferromagnetism Zn(1-X)Mn(X)O diluted magnetic semiconductor nano-line |
| CN101319369B (en) * | 2008-04-15 | 2011-06-22 | 辽宁师范大学 | A kind of preparation method of p-type ZnO nanowire |
| WO2013025744A2 (en) | 2011-08-15 | 2013-02-21 | The Procter & Gamble Company | Personal care methods |
| CN102659170A (en) * | 2012-05-03 | 2012-09-12 | 西北工业大学 | Room temperature solid-phase synthesis method for platy zinc oxide nanometer powder |
| CN111675238A (en) * | 2020-08-03 | 2020-09-18 | 安徽景成新材料有限公司 | Method for preparing multi-morphology nano zinc oxide by solid phase method |
| TWI787091B (en) * | 2022-02-24 | 2022-12-11 | 臺灣塑膠工業股份有限公司 | Oyster shell powder and manufacture method thereof |
-
2002
- 2002-01-22 CN CN 02109078 patent/CN1239395C/en not_active Expired - Fee Related
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| Publication number | Publication date |
|---|---|
| CN1433966A (en) | 2003-08-06 |
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