CN104071826A - Preparation method of modified nanometer ZnO powder - Google Patents
Preparation method of modified nanometer ZnO powder Download PDFInfo
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- CN104071826A CN104071826A CN201310107679.XA CN201310107679A CN104071826A CN 104071826 A CN104071826 A CN 104071826A CN 201310107679 A CN201310107679 A CN 201310107679A CN 104071826 A CN104071826 A CN 104071826A
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- zno powder
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
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Abstract
The invention discloses a preparation method of modified nanometer ZnO powder, and the preparation method solves the problems of easiness for agglomeration, difficulty in dispersion, poor polymer bonding property and the like of nanometer zinc oxide with higher specific surface energy. The preparation method is characterized by comprising the following steps: carrying out chemical reaction under the condition of high temperature by utilizing stearic acid and Zn(NO3)2.6H2O till a brown gas is emitted, and stopping heating; then calcining, cooling and grinding reactants, and placing the reactants into n-butyl alcohol by utilizing waste heat obtained through the heat treatment of a zinc oxide precursor for standing; AND then washing precipitates for several times by using absolute ethyl alcohol, drying in a vacuum drying oven at 50 DEG C, AND grinding to obtain the modified nanometer ZnO powder. The modified nanometer ZnO powder reduces the surface polarity of a nanometer material, enhances the dispersion capacity and affinity of a nanometer particle in an organic medium and enlarges the application range of the nanometer material.
Description
One, technical field
The present invention relates to a kind of preparation of chemical substance, especially relate to a kind of preparation method of modified nano-ZnO powder.
Two, background technology
Nano zine oxide (nano-ZnO) is a kind of novel high function fine inorganic product.Due to the nanometer of material, make nano zine oxide produce the not available surface effects of its body bulk material, small-size effect and macro quanta tunnel effect etc.Thereby nano zine oxide has the incomparable property of general zinc oxide product and purposes at aspects such as magnetic, optical, electrical, chemical, physics, perception.But, have compared with high-ratio surface can nano zine oxide easily reunite, be difficult to disperse in organic medium, be combined poor performance with polymkeric substance, directly affect its actual effect.In order to reduce the surface polarity of nano material, improve dispersive ability and the avidity of nanoparticle in organic medium, expand the range of application of nano material, nano-ZnO is carried out to surface modification significant.
Utilizing tensio-active agent is comparatively effective surface modification means.Conventional surface-modifying agent has silane coupling agent, titante coupling agent, stearic acid, organosilicon etc.Employing KH8454, the NDZ201 such as Geling Hill plum and NDZ311 are that properties-correcting agent carries out respectively surface modification to nano-ZnO, and modified effect is fine and be convenient to storage, and no longer reunites.The grand grade of kingdom is by orthogonal experiment taking sodium laurate as properties-correcting agent, and consumption is 15 %, and pH value is 6, and when modification time is 1.5 h, the lipophilic degree of the nano-ZnO after modification reaches 79.12 %, can be scattered in preferably in methyl alcohol and dimethylbenzene.Li Jianfengs etc. are by Zn (Ac)
2h
2o is dissolved in ethanol, having dissolved LiOHH
2the ethanolic soln of O dropwise joins, meanwhile, and vigorous stirring 1h under 273 K, then centrifugal 20 min.So just obtain the gelinite of ZnO, add the ethanolic soln of urea and boric acid, the content of boron nitride (BN) is adjusted to 90 %.Alcohol solvent is vapored away with rotatory evaporator, then in baking oven, dries, by the mixture of oven dry respectively under 473,673 and 973 K in air atmosphere 7 h that anneal.Experiment showed, that BN shell effectively restrained the overgrowth of nanoparticle and had higher catalytic activity as a kind of important semiconductor light-catalyst, the applied research of zinc oxide has caused people's extensive attention, and may become TiO
2surrogate because these two kinds of materials have identical photocatalytic mechanism.It is reported, ZnO compares TiO
2photocatalytic degradation efficiency is higher, as photocatalytic degradation pulp bleaching effluent, 2 – phenylphenols and phenol etc.
How to reduce the preparation cost of the materials such as nano zine oxide, the photocatalyst material that obtains excellent performance is the focus of current researcher research, also be that can nano zine oxide be applied to one of the key factor that environmental pollutant are administered, therefore between the preparation of nano zine oxide and its photocatalysis performance, be related to that tool is of great significance.
Three, summary of the invention
The object of the invention is to utilize the waste heat of thermal treatment zinc oxide precursor to prepare modified nano-ZnO powder.
The technical scheme that patent of the present invention adopts is: it is to be that raw material through chemical reaction is prepared from by adopting stearic acid and zinc nitrate, and concrete steps are as follows:
(1) in heating container, add appropriate stearic acid, be placed on CL-4 type constant-temperature heating magnetic stirring apparatus and be heated to melt completely;
(2) under constantly stirring, in liquation, add appropriate Zn (NO
3)
26H
2o continues reacting by heating after it dissolves completely, until there is the gas of reddish-brown to come out from beaker, stops heating;
(3) reacted solution pour out be cooled to completely curing;
(4) cooling curing thing is proceeded to roasting in retort furnace, when temperature rises to 600
owhen C, take out from crucible;
(5) fixed compound is ground to Powdered, is placed in retort furnace 600
ounder C, after roasting 2 h, take out, utilize the waste heat of thermal treatment zinc oxide precursor, while hot by powder to entering in propyl carbinol, leave standstill;
(6) with absolute ethanol washing throw out for several times, to remove propyl carbinol, then in vacuum drying oven 50
oc is dried, and grinds to obtain modified nano-ZnO powder.
Tool of the present invention has the following advantages and beneficial effect: simple to the method for ZnO Modified with propyl carbinol, be similar to the quench treatment process of metal.This method of modifying is environmentally friendly, and when preparation, alcoholic solution used can recycling, and does not need additional energy source, directly utilizes the waste heat of preparing Zinc oxide powder to react and obtains modified product.The photocatalysis effect of modified nano zinc oxide is obvious, its organic dye pollutant such as tropeolin-D of just directly degrading under sunlight, modified nano zinc oxide can be suspended in the top layer of tropeolin-D or other waste water for a long time simultaneously, can make full use of external light source, this may to directly utilizing in the future sunlight degrading waste water to provide.
Four, embodiment
Below by embodiment, the present invention is further illustrated.
Embodiment 1:
First in beaker, add 13 ~ 15g stearic acid, be placed on CL-4 type constant-temperature heating magnetic stirring apparatus and be heated to melt completely, under constantly stirring, in liquation, add 15 g Zn (NO
3)
26H
2o continues reacting by heating after it dissolves completely, until there is the gas of reddish-brown to come out from beaker, stops heating.Reacted solution is poured in crucible cooling, proceeds to roasting in retort furnace after solidifying completely, when temperature rises to 600
owhen C, take out crucible, be ground to Powderedly with mortar, the powder of gained is placed in to retort furnace, 600
ounder C, after roasting 2 h, take out, utilize the waste heat of thermal treatment zinc oxide precursor, while hot by powder to entering in 50 mL propyl carbinols, leave standstill, with absolute ethanol washing precipitation for several times, to remove propyl carbinol, in vacuum drying oven 50
oc is dried, and grinds to obtain modified nano-ZnO powder.
Embodiment 2:
First in reactor, add 13 ~ 15kg stearic acid, be heated to melt completely, under constantly stirring, in liquation, add 15 kg Zn (NO
3)
26H
2o continues reacting by heating after it dissolves completely, until there is the gas of reddish-brown to come out from beaker, stops heating.It is cooling that reacted solution is put into cooling pool, proceeds to roasting kiln roasting after solidifying completely, when temperature rises to 600
owhen C, stop heating.After cooling, taking-up pulverizes, is ground to Powdered, the powder of gained is placed in to stoving oven, 600
ounder C, after roasting 2 h, take out, utilize the waste heat of thermal treatment zinc oxide precursor, while hot by powder to entering in 50 L propyl carbinols, leave standstill, with absolute ethanol washing precipitation for several times, to remove propyl carbinol, in vacuum drying oven 50
oc is dried, and grinds to obtain modified nano-ZnO powder.
Claims (1)
1. a preparation method for modified nano-ZnO powder, is characterized in that: it is to be prepared from by chemical reaction by stearic acid and zinc nitrate, and concrete steps are as follows:
(1) in heating container, add stearic acid, be placed on CL-4 type constant-temperature heating magnetic stirring apparatus and be heated to melt completely;
(2) under constantly stirring, in liquation, add Zn (NO
3)
26H
2o continues reacting by heating after it dissolves completely, until there is the gas of reddish-brown to come out from beaker, stops heating;
(3) reacted solution pour out be cooled to completely curing;
(4) cooling curing thing is proceeded to roasting in retort furnace, when temperature rises to 600
owhen C, take out from crucible;
(5) cured article is ground to Powdered, is placed in retort furnace 600
ounder C, after roasting 2 h, take out, utilize the waste heat of thermal treatment zinc oxide precursor, while hot by powder to entering in propyl carbinol, leave standstill;
(6) with absolute ethanol washing throw out for several times, to remove propyl carbinol, then in vacuum drying oven 50
oc is dried, and grinds to obtain modified nano-ZnO powder.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310107679.XA CN104071826B (en) | 2013-03-31 | 2013-03-31 | Preparation method of modified nanometer ZnO powder |
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|---|---|---|---|
| CN201310107679.XA CN104071826B (en) | 2013-03-31 | 2013-03-31 | Preparation method of modified nanometer ZnO powder |
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| CN104071826A true CN104071826A (en) | 2014-10-01 |
| CN104071826B CN104071826B (en) | 2015-07-15 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107010651A (en) * | 2017-05-15 | 2017-08-04 | 广西放心源生物科技有限公司 | The surface modifying method of nano zine oxide |
| CN112625487A (en) * | 2021-01-14 | 2021-04-09 | 成都萃匀离环保科技有限公司 | Preparation method of antibacterial water-based wood composite coating |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101318690A (en) * | 2008-07-16 | 2008-12-10 | 武汉大学 | Stephanoporate zinc oxide nano-powder and preparation method thereof |
| CN101555035A (en) * | 2009-05-19 | 2009-10-14 | 上海工程技术大学 | Preparation and application of local surface-modified nanometre zinc oxide by sol-gel method |
| CN101885508A (en) * | 2009-05-14 | 2010-11-17 | 中国科学院宁波材料技术与工程研究所 | Method for preparing zinc oxide-doped nano powder controllably on large scale |
| CN102167530A (en) * | 2010-12-23 | 2011-08-31 | 西南科技大学 | Vermiculite expansion and organic modification integrated preparation process |
-
2013
- 2013-03-31 CN CN201310107679.XA patent/CN104071826B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101318690A (en) * | 2008-07-16 | 2008-12-10 | 武汉大学 | Stephanoporate zinc oxide nano-powder and preparation method thereof |
| CN101885508A (en) * | 2009-05-14 | 2010-11-17 | 中国科学院宁波材料技术与工程研究所 | Method for preparing zinc oxide-doped nano powder controllably on large scale |
| CN101555035A (en) * | 2009-05-19 | 2009-10-14 | 上海工程技术大学 | Preparation and application of local surface-modified nanometre zinc oxide by sol-gel method |
| CN102167530A (en) * | 2010-12-23 | 2011-08-31 | 西南科技大学 | Vermiculite expansion and organic modification integrated preparation process |
Non-Patent Citations (1)
| Title |
|---|
| 季敏霞: "溶胶凝胶法制备纳米氧化物的研究", 《中国优秀博硕士学位论文全文数据库（硕士） 工程科技I辑》, no. 07, 15 November 2005 (2005-11-15) * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107010651A (en) * | 2017-05-15 | 2017-08-04 | 广西放心源生物科技有限公司 | The surface modifying method of nano zine oxide |
| CN112625487A (en) * | 2021-01-14 | 2021-04-09 | 成都萃匀离环保科技有限公司 | Preparation method of antibacterial water-based wood composite coating |
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| CN104071826B (en) | 2015-07-15 |
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