CN101143974A - Method for preparing composite nano particle of silicon dioxide coated with zinc oxide - Google Patents
Method for preparing composite nano particle of silicon dioxide coated with zinc oxide Download PDFInfo
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- CN101143974A CN101143974A CNA2007101186703A CN200710118670A CN101143974A CN 101143974 A CN101143974 A CN 101143974A CN A2007101186703 A CNA2007101186703 A CN A2007101186703A CN 200710118670 A CN200710118670 A CN 200710118670A CN 101143974 A CN101143974 A CN 101143974A
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- zinc
- silicon dioxide
- zinc oxide
- preparation
- nano
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 81
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 38
- 235000012239 silicon dioxide Nutrition 0.000 title claims abstract description 30
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 25
- 239000002131 composite material Substances 0.000 title claims abstract description 17
- 239000002105 nanoparticle Substances 0.000 title abstract description 11
- 238000000034 method Methods 0.000 title abstract description 5
- 238000002360 preparation method Methods 0.000 claims abstract description 26
- 239000002245 particle Substances 0.000 claims abstract description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 150000003751 zinc Chemical class 0.000 claims abstract description 14
- 238000005406 washing Methods 0.000 claims abstract description 10
- 229910052751 metal Inorganic materials 0.000 claims abstract description 7
- 239000002184 metal Substances 0.000 claims abstract description 7
- 239000002114 nanocomposite Substances 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 4
- 229960001866 silicon dioxide Drugs 0.000 claims description 26
- 239000008187 granular material Substances 0.000 claims description 10
- 238000005245 sintering Methods 0.000 claims description 10
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical group [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 5
- 229960001763 zinc sulfate Drugs 0.000 claims description 5
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 5
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 4
- 229910052725 zinc Inorganic materials 0.000 claims description 4
- 239000011701 zinc Substances 0.000 claims description 4
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 2
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 239000004246 zinc acetate Substances 0.000 claims description 2
- 239000011592 zinc chloride Substances 0.000 claims description 2
- 235000005074 zinc chloride Nutrition 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 5
- 239000011248 coating agent Substances 0.000 abstract description 3
- 238000000576 coating method Methods 0.000 abstract description 3
- 239000004033 plastic Substances 0.000 abstract description 3
- 229920003023 plastic Polymers 0.000 abstract description 3
- 239000004753 textile Substances 0.000 abstract description 3
- 239000003513 alkali Substances 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 239000011246 composite particle Substances 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000002537 cosmetic Substances 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- 238000001556 precipitation Methods 0.000 description 13
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 6
- 238000013467 fragmentation Methods 0.000 description 6
- 238000006062 fragmentation reaction Methods 0.000 description 6
- 238000009413 insulation Methods 0.000 description 6
- 229910052710 silicon Inorganic materials 0.000 description 6
- 239000010703 silicon Substances 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000003643 water by type Substances 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000000844 anti-bacterial effect Effects 0.000 description 2
- 239000011858 nanopowder Substances 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Abstract
A method for nano-particles coated with zinc oxide on silicon dioxide surface relates to a method for preparing composite nano-particles used for cosmetic products, nano-functional textile products, functional plastics and coating etc., which is characterized in that the preparation process includes that silicon dioxide particles are homogeneously dispersed in lower alcohol solution, metal zinc salts are added and stirred at 20DGE C-60DGE C for 8-24h, silicon dioxide particles with metal zinc salt layer coated on the surface is sintered at temperature of 500-700DGE C for 3-5h after centrifugal separation, washing, and drying to obtain nano-composite particles. The invention has a simple preparation process and high composite particles activity, which is applicable to large-scale industrial production. The difference between the invention and conventional preparation method is that no alkali solution used in reaction ensures the high purity of the product.
Description
Technical field
The preparation method of the nano particle of silicon dioxide coated with zinc oxide relates to a kind of preparation method who is used for the Nano composite granules in fields such as makeup, nano-function textile, functional plastics and coating.
Background technology
Nano zine oxide is little owing to its particle diameter, specific surface area has small-size effect, surface and interface effect and macro quanta tunnel effect greatly, compare with common block zinc oxide, nano zine oxide has the unique piezo-electricity, high conductivity, photo-catalysis capability and scattering and the ultraviolet ability of absorption, can be widely used in ultraviolet screener, transmitter, many fields such as photocatalysis antibacterial.The best particle size of active zinc flower should be less than 50nm in theory, and nano zine oxide is because size is little, so surface energy is high very unstable, easily reunion also is to prepare the ubiquitous problem of nano zine oxide at present, and reunion has a strong impact on the physics and the chemical property of nano zine oxide.It is even that silicon-dioxide then has particle diameter, characteristics such as monodispersity is good, and silicon-dioxide itself also has very strong ultraviolet shielded effect, if the surface that Zinc oxide nanoparticle is coated on silicon-dioxide just can well solve the agglomeration traits of nano zine oxide, kept the high reactivity of nano zine oxide simultaneously again.
Find relevant patent CN01792809A and CN1381426A, what adopt all is conventional Preparation by Uniform Precipitation composite particles, the problem that this method exists be nano-powder reunite be difficult to overcome, production cost height, efficient are low, be not suitable for large-scale commercial production, be difficult to prepare and have the high reactivity composite nanometer particle, and use the positively charged ion of alkali lye introducing to be difficult to remove in the reaction, can pollute final product.
Summary of the invention
The objective of the invention is deficiency at above-mentioned prior art existence; provide a kind of and can overcome effectively that nano-powder is reunited, production cost is low, efficient is high, be fit to large-scale commercial production, the preparation method of the composite nanometer particle of the silicon dioxide coated with zinc oxide of active high, the no cation contamination of composite nanometer particle.
The objective of the invention is to be achieved through the following technical solutions.
The preparation method of the composite nanometer particle of silicon dioxide coated with zinc oxide, it is characterized in that its preparation process is that silica dioxide granule is uniformly dispersed in low-alcohol solution, add the metal zinc salt again, under 20 ℃ of-60 ℃ of temperature, stir 8-24h, the silica dioxide granule that surface adsorption is had the metallic zinc salt deposit is after centrifugation, washing, drying, at 500-700 ℃ of sintering temperature 3-5h, obtain Nano composite granules.
The preparation method of the composite nanometer particle of silicon dioxide coated with zinc oxide of the present invention is characterized in that its metal zinc salt is inorganic zinc salts such as zinc nitrate, zinc sulfate, zinc acetate or zinc chloride.
The preparation method of the composite nanometer particle of silicon dioxide coated with zinc oxide of the present invention is characterized in that its lower alcohol is one or more the pure mixtures in methyl alcohol, ethanol, the Virahol.
The preparation method of the composite nanometer particle of silicon dioxide coated with zinc oxide of the present invention is characterized in that in its preparation process that silicon-dioxide is dispersed in that concentration is 0.2-1mol/L in the low-alcohol solution.
The preparation method of the composite nanometer particle of silicon dioxide coated with zinc oxide of the present invention is characterized in that the metallic zinc salt formation concentration that adds in its preparation process is the zinc solution of 0.5-3mol/L in low-alcohol solution.
Method of the present invention, by changing churning time, parameters such as sintering temperature can be controlled the size of silica sphere nano zine oxide, and preparation process is simple, the product purity height that makes, good crystallinity is fit to industrial production very much.The nano composite material that makes has shown than single zinc oxide or stronger ultraviolet radiation absorption shielding and the sterilization antibacterial ability of silicon-dioxide, is highly suitable for fields such as makeup, nano-function textile, functional plastics and coating.
Embodiment
The preparation method of the composite nanometer particle of silicon dioxide coated with zinc oxide is uniformly dispersed nano SiO 2 particle in low-alcohol solution, dispersive silica granules amount is 0.2-1mol/L in low-alcohol solution. Add the metal zinc salt again, the metallic zinc salt formation concentration that adds in low-alcohol solution is the zinc solution of 0.5-3mol/L, under 20 ℃ of-60 ℃ of temperature, stir 8-24h, the silica dioxide granule that table is coated with the metallic zinc salt deposit is after centrifugation, washing, drying, at 500-700 ℃ of sintering temperature 3-5h, obtain Nano composite granules.
Now embodiments of the invention are specifically described as follows:
Embodiment 1
At first 1.5g silicon-dioxide is added in the ethanol, being made into concentration is the solution 50ml of 0.5mol/L, the 6.35g zinc nitrate is joined in the silicon dioxde solution at 60 ℃ of constant temperature stirring 8h, centrifuge washing obtains solid precipitation 2 times under the 4000r/min, throw out is at 100 ℃ of dry 8h, then precipitation is put into the retort furnace sintering, set 1h and be raised to 400 ℃ from room temperature, be warmed up to 600 ℃ of insulations 1 hour with 100 ℃/h speed after 400 ℃, fragmentation is dispersed in to observe under the TEM and finds Zinc oxide nanoparticle at the silica sphere homodisperse, calculates nano zine oxide median size 7.1nm according to the sherrer formula.
Embodiment 2
At first 1.5g silicon-dioxide is added in the ethanol, being made into concentration is the solution 50ml of 0.5mol/L, the 12.7g zinc nitrate is joined in the silicon dioxde solution at 60 ℃ of constant temperature stirring 12h, centrifuge washing obtains solid precipitation 2 times under the 4000r/min, throw out is at 100 ℃ of dry 8h, then precipitation is put into the retort furnace sintering, set 1h and be raised to 400 ℃ from room temperature, be warmed up to 600 ℃ of insulations 1 hour with 100 ℃/h speed after 400 ℃, fragmentation is dispersed in to observe under the TEM and finds Zinc oxide nanoparticle at the silica sphere homodisperse, calculates nano zine oxide median size 8.2nm according to the sherrer formula.
Embodiment 3
At first 1.5g silicon-dioxide is added in the ethanol, being made into concentration is the solution 50ml of 0.5mol/L, the 12.7g zinc nitrate is joined in the silicon dioxde solution at 60 ℃ of constant temperature stirring 12h, centrifuge washing obtains solid precipitation 2 times under the 4000r/min, throw out is at 100 ℃ of dry 8h, then precipitation is put into the retort furnace sintering, set 1h and be raised to 400 ℃ from room temperature, be warmed up to 700 ℃ of insulations 1 hour with 100 ℃/h speed after 400 ℃, fragmentation is dispersed in to observe under the TEM and finds Zinc oxide nanoparticle at the silica sphere homodisperse, calculates nano zine oxide median size 8.7nm according to the sherrer formula.
Embodiment 4
At first 1.5g silicon-dioxide is added in the ethanol, being made into concentration is the solution 50ml of 0.5mol/L, 8.35g zinc sulfate joined in the silicon dioxde solution in 60 ℃ of waters bath with thermostatic control, stir 8h, centrifuge washing obtains solid precipitation 2 times under the 4000r/min, throw out is at 100 ℃ of dry 8h, then precipitation is put into the retort furnace sintering, set 1h and be raised to 400 ℃ from room temperature, be warmed up to 600 ℃ of insulations 1 hour with 100 ℃/h speed after 400 ℃, fragmentation is dispersed in to observe under the TEM and finds Zinc oxide nanoparticle at the silica sphere homodisperse, calculates nano zine oxide median size 7.3nm according to the sherrer formula.
Embodiment 5
At first 1.5g silicon-dioxide is added in the ethanol, being made into concentration is the solution 50ml of 0.5mol/L, 8.35g zinc sulfate joined in the silicon dioxde solution in 20 ℃ of waters bath with thermostatic control, stir 8h, centrifuge washing obtains solid precipitation 2 times under the 4000r/min, throw out is at 100 ℃ of dry 8h, then precipitation is put into the retort furnace sintering, set lh and be raised to 400 ℃ from room temperature, be warmed up to 600 ℃ of insulations 1 hour with 100 ℃/h speed after 400 ℃, fragmentation is dispersed in to observe under the TEM and finds Zinc oxide nanoparticle at the silica sphere homodisperse, calculates nano zine oxide median size 7.6nm according to the sherrer formula.
Embodiment 6
At first 2.4g silicon-dioxide is added in the ethanol, being made into concentration is the solution 50ml of 0.5mol/L, 8.35g zinc sulfate joined in the silicon dioxde solution in 60 ℃ of waters bath with thermostatic control, stir 8h, centrifuge washing obtains solid precipitation 2 times under the 4000r/min, throw out is at 100 ℃ of dry 8h, then precipitation is put into the retort furnace sintering, set lh and be raised to 400 ℃ from room temperature, be warmed up to 600 ℃ of insulations 1 hour with 100 ℃/h speed after 400 ℃, fragmentation is dispersed in to observe under the TEM and finds Zinc oxide nanoparticle at the silica sphere homodisperse, calculates nano zine oxide median size 8.4nm according to the sherrer formula.
Claims (5)
1. the preparation method of the composite nanometer particle of silicon dioxide coated with zinc oxide, it is characterized in that its preparation process is that silica dioxide granule is uniformly dispersed in low-alcohol solution, add the metal zinc salt again, under 20 ℃ of-60 ℃ of temperature, stir 8-24h, the silica dioxide granule that table is coated with the metallic zinc salt deposit at 500-700 ℃ of sintering temperature 3-5h, obtains Nano composite granules after centrifugation, washing, drying.
2. the preparation method of the composite nanometer particle of silicon dioxide coated with zinc oxide according to claim 1 is characterized in that its metal zinc salt is zinc nitrate, zinc sulfate, zinc acetate or zinc chloride.
3. the preparation method of the composite nanometer particle of silicon dioxide coated with zinc oxide according to claim 1 is characterized in that its lower alcohol is one or more the pure mixtures in methyl alcohol, ethanol, the Virahol.
4. the preparation method of the composite nanometer particle of silicon dioxide coated with zinc oxide according to claim 1 is characterized in that in its preparation process that silicon-dioxide is dispersed in that concentration is 0.2-1mol/L in the low-alcohol solution.
5. the preparation method of the composite nanometer particle of silicon dioxide coated with zinc oxide according to claim 1 is characterized in that the metallic zinc salt formation concentration that adds in its preparation process is the zinc solution of 0.5-3mol/L in low-alcohol solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101186703A CN101143974A (en) | 2007-07-12 | 2007-07-12 | Method for preparing composite nano particle of silicon dioxide coated with zinc oxide |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101186703A CN101143974A (en) | 2007-07-12 | 2007-07-12 | Method for preparing composite nano particle of silicon dioxide coated with zinc oxide |
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| Publication Number | Publication Date |
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| CN101143974A true CN101143974A (en) | 2008-03-19 |
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|---|---|---|---|
| CNA2007101186703A Pending CN101143974A (en) | 2007-07-12 | 2007-07-12 | Method for preparing composite nano particle of silicon dioxide coated with zinc oxide |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102108256A (en) * | 2010-12-31 | 2011-06-29 | 哈尔滨工业大学深圳研究生院 | Inorganic-organic superhydrophobic nanocomposite for stone historical relics and preparation method thereof |
| CN103050640A (en) * | 2013-01-29 | 2013-04-17 | 哈尔滨工业大学 | Preparation method of nanorod with zinc oxide nano-particle/silicon dioxide composite structure |
| CN105228954A (en) * | 2013-04-19 | 2016-01-06 | 住友大阪水泥株式会社 | Silicon oxide coating zinc oxide and its manufacture method and the composition and the cosmetic that contain silica coating zinc oxide |
| CN107500555A (en) * | 2017-07-31 | 2017-12-22 | 重庆市中光电显示技术有限公司 | Durable coated glass of a kind of antibacterial for touch-screen and preparation method thereof |
| CN108002432A (en) * | 2017-12-14 | 2018-05-08 | 苏州中科纳福材料科技有限公司 | The preparation method of spherical composite material |
| CN110876689A (en) * | 2019-09-30 | 2020-03-13 | 成都理工大学 | Calcined kaolin loaded nano ZnO composite anti-ultraviolet agent and preparation technology thereof |
| CN114702763A (en) * | 2022-05-09 | 2022-07-05 | 宁国九鼎橡塑制品有限公司 | Rubber driving disc material of air-conditioning compressor and preparation process thereof |
| WO2023088088A1 (en) * | 2021-11-19 | 2023-05-25 | Tcl科技集团股份有限公司 | Nanoparticle, preparation method therefor, and light-emitting diode |
| CN116590070A (en) * | 2023-05-06 | 2023-08-15 | 杭州电子科技大学 | ZnO coated SiO 2 Composite nanoparticle preparation method and application of lubricating additive |
-
2007
- 2007-07-12 CN CNA2007101186703A patent/CN101143974A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102108256A (en) * | 2010-12-31 | 2011-06-29 | 哈尔滨工业大学深圳研究生院 | Inorganic-organic superhydrophobic nanocomposite for stone historical relics and preparation method thereof |
| CN103050640A (en) * | 2013-01-29 | 2013-04-17 | 哈尔滨工业大学 | Preparation method of nanorod with zinc oxide nano-particle/silicon dioxide composite structure |
| CN103050640B (en) * | 2013-01-29 | 2015-08-19 | 哈尔滨工业大学 | A kind of preparation method of nanorod with zinc oxide nano-particle/silicodioxide dioxide composite structure |
| CN105228954A (en) * | 2013-04-19 | 2016-01-06 | 住友大阪水泥株式会社 | Silicon oxide coating zinc oxide and its manufacture method and the composition and the cosmetic that contain silica coating zinc oxide |
| CN107500555A (en) * | 2017-07-31 | 2017-12-22 | 重庆市中光电显示技术有限公司 | Durable coated glass of a kind of antibacterial for touch-screen and preparation method thereof |
| CN108002432A (en) * | 2017-12-14 | 2018-05-08 | 苏州中科纳福材料科技有限公司 | The preparation method of spherical composite material |
| CN110876689A (en) * | 2019-09-30 | 2020-03-13 | 成都理工大学 | Calcined kaolin loaded nano ZnO composite anti-ultraviolet agent and preparation technology thereof |
| WO2023088088A1 (en) * | 2021-11-19 | 2023-05-25 | Tcl科技集团股份有限公司 | Nanoparticle, preparation method therefor, and light-emitting diode |
| CN114702763A (en) * | 2022-05-09 | 2022-07-05 | 宁国九鼎橡塑制品有限公司 | Rubber driving disc material of air-conditioning compressor and preparation process thereof |
| CN116590070A (en) * | 2023-05-06 | 2023-08-15 | 杭州电子科技大学 | ZnO coated SiO 2 Composite nanoparticle preparation method and application of lubricating additive |
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