CN101734711A - Method for synthesis of nano-zinc oxide powder through microwave solid state reaction - Google Patents
Method for synthesis of nano-zinc oxide powder through microwave solid state reaction Download PDFInfo
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- CN101734711A CN101734711A CN200810226786A CN200810226786A CN101734711A CN 101734711 A CN101734711 A CN 101734711A CN 200810226786 A CN200810226786 A CN 200810226786A CN 200810226786 A CN200810226786 A CN 200810226786A CN 101734711 A CN101734711 A CN 101734711A
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Abstract
The invention discloses a method for the synthesis of nano-zinc oxide powder through microwave solid state reaction, comprising the steps: the raw material, which is selected from oxalic acid and basic zinc carbonate (5ZnO.2CO2.4H2O), is sufficiently mixed and ground and then put in a microwave oven for being heated to 500 to 700 DEG C, and the nano-zinc oxide powder can be obtained by keeping the mixture of raw material at constant temperature for 10 to 30 minutes. On the basis of rapidness and evenness of microwave heating, the method greatly shortens the time for solid state reaction to further reduce agglomeration of products, and the size of the resultant zinc oxide grain is 10 to 40nm; the entire reaction course of the method is free from solvents, simple and convenient in operation and low in energy consumption, and has no or little pollution for environment and great easiness for the implementation of industrial production.
Description
Technical field
The invention belongs to the inorganic nanometer powder technical field of material, be specifically related to a kind of method of synthesis of nano-zinc oxide powder through microwave solid state reaction.
Background technology
Nano material is meant the ultrafine particulate material of particle size between 1～100nm, compare with the macrobead material, have special propertys such as small-size effect, surface effects, quantum size effect and macro quanta tunnel effect, therefore demonstrate excellent performance at aspects such as optics, electricity, magnetics and catalysis.Nano zine oxide is owing to its nontoxic, cheap and excellent performance is widely used in each field, and its preparation method is the focus that people study always.
At present, the method for preparing nanometer Zinc oxide powder mainly can be divided into physics method and chemical method.The physics method mainly adopts the mechanical ball milling method, and this method energy consumption is bigger, easily introduces impurity, and gained powder granule size is big, size distribution is inhomogeneous, is unsuitable for as the hyperfine material with property.The most frequently used in the chemical method is liquid phase method, as the precipitator method, sol-gel method, hydrolysis method, microemulsion method etc.These methods all are the control reaction conditions basically, and at first synthetic presoma (being labile salt) in liquid phase carries out thermolysis with these salt again and prepares nano-powder.Because the prepared presoma salt of liquid phase method needs through processes such as separation, filtration, washing and dryings, thus some water contained in these salt usually, and these water easily make the gained nano-powder produce hard aggregation owing to wicking action in the salt calcination process.Thereby, people usually select organic solvent washing for use or adopt special dry technology (as supercritical drying, azeotropic distillation drying and lyophilize etc.) to remove and anhydrate, this not only needs to consume a large amount of organic solvents, but also makes process complications, thereby increases product cost.In addition, also comprise solid reaction process in the chemical method, solid reaction process is a kind of novel method for preparing nano-powder that development in recent years is got up.This method is reflected in the solid phase carries out, and does not need solvent, has solved problem of environmental pollution to a certain extent.But most of solid state reaction exists the reaction required time longer, reacts problem such as inhomogeneous.
Take a broad view of above-mentioned these and prepare the method for nanometer Zinc oxide powder, part all comes with some shortcomings: the difficult control of reaction process complexity, technological process, energy consumption is big, cost is high, gained nano particle diameter skewness etc.
Summary of the invention
The objective of the invention is in order to overcome the existing defective that exists in the nanometer Zinc oxide powder technology for preparing, utilize the advantage of microwave heating technique aspect the extraordinary novel material of preparation, provide that a kind of technological process is simple, easy to control, energy consumption is low, environmentally safe or the method for preparing zinc oxide nano-powder of reduced contamination, the products therefrom size is less and size distribution is more even.
Purpose of the present invention is achieved through the following technical solutions:
A kind of method of synthesis of nano-zinc oxide powder through microwave solid state reaction: with oxalic acid and zinc subcarbonate (5ZnO2CO
24H
2O) be raw material, power and capacity according to microwave oven, take by weighing a certain amount of raw material in oxalate denominationby and 1: 1 ratio of zine ion mol ratio, to put into microwave oven behind the load weighted raw material mixed grinding, after being heated to 500～700 ℃, constant temperature 10～30min can obtain the Zinc oxide powder that grain-size is 10～40nm.
Inventive principle: the present invention utilizes solid state reaction and microwave heating technique principle.Utilize the solid state reaction nano materials can overcome traditional liquid phase method and prepare the ion aggregation phenomenon that exists in the nano material; Do not need solvent in the reaction process, not only reduce production costs, and be difficult in the reaction process introducing impurity, the purity of products therefrom is higher.The characteristics of microwave heating are to improve rate of heating greatly, are easy to automatic control.In addition, microwave heating also has characteristics such as pollution-free, no waste heat, floor space be little.Microwave heating technique is applied in the solid state reaction, utilizes microwave heating advantage fast, can shorten the solid state reaction time greatly, can effectively control the growth of product particulate, thereby easily obtain small sized particles.In addition, utilize the homogeneity of microwave heating, can make whole solid state reaction even, can not only control particle size distribution effectively, can also reduce the agglomeration of product.
Oxalic acid and zinc subcarbonate (5ZnO2CO
24H
2O) solid state reaction is slower, so have only small part to react in the mixed grinding process.Mixture after grinding is placed microwave oven, and under the condition of microwave heating, the very fast generation solid state reaction of oxalic acid and zinc subcarbonate generates zinc oxalate, and its reaction is as follows:
5(H
2C
2O
4·2H
2O)+(5ZnO·2CO
2·4H
2O)→5(ZnC
2O
4·2H
2O)+9H
2O↑+2CO
2↑
Along with the carrying out of microwave heating, zinc oxalate decomposes generation zinc oxide in the time of 500～700 ℃, and its reaction formula is:
ZnC
2O
4·2H
2O→ZnO+2H
2O↑+CO
2↑+CO↑
The present invention compared with prior art has following advantage:
(1) the present invention adopts microwave auxiliary solid phase reaction method synthesis of nano-zinc oxide powder, entire reaction course does not need solvent, do not need tensio-active agent, be reflected in the solid phase and carry out, effectively avoided in the liquid phase reaction owing to there is the nano-powder agglomeration that causes in water.
(2) to select oxalic acid and zinc subcarbonate for use be raw material in the present invention, mix back heating in microwave oven and prepare the precursor zinc oxalate fast, the further again decomposes of zinc oxalate prepares Zinc oxide powder, and entire reaction course does not need processes such as washing, filtration and separation, and technological process is simple and easy to control.And the by product that two-step reaction generated all is H
2O and CO or CO
2, they can be overflowed with gas form in presoma preparation and presoma decomposition course, and prepared powder is played loose effect, thereby reduce the agglomeration of powder.Not having strong acid, alkali or organic solvent in the entire reaction course and participate in, reduced the pollution to environment, is a kind of " green " synthetic method.
(3) solid state reaction is slower usually, and mesoxalic acid of the present invention and zinc subcarbonate generation solid state reaction required time are longer, but utilize the instantaneity and the homogeneity of microwave heating, mixed raw material is reacted rapidly in microwave oven generate the presoma zinc oxalate.
(4) zinc oxalate further decomposes in microwave oven generates zinc oxide, should process compare than the conventional high-temperature calcination process, has saved the reaction times greatly, has reduced energy consumption.And microwave heating has rapidity, the effectively growth of inhibited oxidation zinc particle size; Microwave heating does not need heat passage, and direct heating can react evenly, thereby the products therefrom particle size distribution is narrower from inside to outside.
Description of drawings
Fig. 1 is the X-ray diffractogram of the ZnO of the embodiment of the invention 1～3 preparation.
Among Fig. 1, ordinate is (I) intensity, and abscissa is 2 θ (degree).
Embodiment
In order better to understand the present invention, the invention will be further described below in conjunction with embodiment, but the scope of protection of present invention is not limited to the scope that embodiment represents.
Take by weighing oxalic acid and zinc subcarbonate (5ZnO2CO respectively
24H
2O) each 52.6g and 47.4g will put into microwave oven behind two kinds of raw material mixed grindings, and at microwave oven internal heating to 500 ℃, constant temperature 30min can prepare Zinc oxide powder.Curve 1 is the X-ray diffractogram of product in the accompanying drawing 1, and as can be seen from the figure, the peak position of each diffraction peak and the standard card of ZnO (JCPDS No.36-1451) match, and does not have unnecessary dephasign peak appearance, illustrates that product is the ZnO pure phase.By the halfwidth of diffraction peak, be about 15.5nm with Scherrer formula estimation grain-size.
Take by weighing oxalic acid and zinc subcarbonate (5ZnO2CO respectively
24H
2O) each 52.6g and 47.4g will put into microwave oven behind two kinds of raw material mixed grindings, and at microwave oven internal heating to 600 ℃, constant temperature 20min can prepare Zinc oxide powder.Curve 2 is the X-ray diffractogram of product in the accompanying drawing 1, and as can be seen from the figure, the peak position of each diffraction peak and the standard card of ZnO (JCPDS No.36-1451) match, and does not have unnecessary dephasign peak appearance, illustrates that product is the ZnO pure phase.By the halfwidth of diffraction peak, be about 23.6nm with Scherrer formula estimation grain-size.
Take by weighing oxalic acid and zinc subcarbonate (5ZnO2CO respectively
24H
2O) each 52.6g and 47.4g will put into microwave oven behind two kinds of raw material mixed grindings, and at microwave oven internal heating to 700 ℃, constant temperature 10min can prepare Zinc oxide powder.Curve 3 is the X-ray diffractogram of product in the accompanying drawing 1, and as can be seen from the figure, the peak position of each diffraction peak and the standard card of ZnO (JCPDS No.36-1451) match, and does not have unnecessary dephasign peak appearance, illustrates that product is the ZnO pure phase.By the halfwidth of diffraction peak, be about 36.8nm with Scherrer formula estimation grain-size.
Claims (3)
1. the method for a synthesis of nano-zinc oxide powder through microwave solid state reaction is characterized in that: adopting oxalic acid and molecular formula is 5ZnO2CO
24H
2The zinc subcarbonate of O is a raw material, after raw material is ground in oxalate denominationby and 1: 1 ratio thorough mixing of zine ion mol ratio, puts into microwave oven, heating, and constant temperature, obtaining grain-size is the Zinc oxide powder of 10～40nm.
2. the method for synthesis of nano-zinc oxide powder through microwave solid state reaction according to claim 1 is characterized in that, described microwave heating temperature is 500～700 ℃.
3. the method for synthesis of nano-zinc oxide powder through microwave solid state reaction according to claim 1 and 2 is characterized in that, constant temperature time is 10～30min in the described microwave oven, and obtaining grain-size is the Zinc oxide powder of 10～40nm.
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|---|---|---|---|
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102703134A (en) * | 2012-05-14 | 2012-10-03 | 太原理工大学 | Method for preparing medium-high temperature gas desulfurizing agent by microwave radiation |
| CN102989526A (en) * | 2012-12-25 | 2013-03-27 | 东北石油大学 | Method of preparing body catalyst for distillate oil depth hydrofining by utilizing microwave method |
| CN103182301A (en) * | 2011-12-29 | 2013-07-03 | 吉林师范大学 | Controllable growing method of hamburger shaped ZnO nano-photocatalyst |
| CN103241765A (en) * | 2013-04-26 | 2013-08-14 | 湖南凯新陶瓷科技有限公司 | Microwave synthesis method of superfine zinc oxide powder |
| CN107162042A (en) * | 2017-05-27 | 2017-09-15 | 安徽锦华氧化锌有限公司 | A kind of preparation method of nano zine oxide |
| CN107624788A (en) * | 2017-09-20 | 2018-01-26 | 山东星美新材料股份有限公司 | A kind of Nano composite granules, its preparation method and the application of antibacterial and mouldproof smelly eliminating |
| CN111872414A (en) * | 2020-06-12 | 2020-11-03 | 辽宁科技大学 | Preparation method of micro-nano pre-alloyed powder |
-
2008
- 2008-11-24 CN CN200810226786A patent/CN101734711A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103182301A (en) * | 2011-12-29 | 2013-07-03 | 吉林师范大学 | Controllable growing method of hamburger shaped ZnO nano-photocatalyst |
| CN102703134A (en) * | 2012-05-14 | 2012-10-03 | 太原理工大学 | Method for preparing medium-high temperature gas desulfurizing agent by microwave radiation |
| CN102703134B (en) * | 2012-05-14 | 2013-12-11 | 太原理工大学 | Method for preparing medium-high temperature gas desulfurizing agent by microwave radiation |
| CN102989526A (en) * | 2012-12-25 | 2013-03-27 | 东北石油大学 | Method of preparing body catalyst for distillate oil depth hydrofining by utilizing microwave method |
| CN103241765A (en) * | 2013-04-26 | 2013-08-14 | 湖南凯新陶瓷科技有限公司 | Microwave synthesis method of superfine zinc oxide powder |
| CN107162042A (en) * | 2017-05-27 | 2017-09-15 | 安徽锦华氧化锌有限公司 | A kind of preparation method of nano zine oxide |
| CN107624788A (en) * | 2017-09-20 | 2018-01-26 | 山东星美新材料股份有限公司 | A kind of Nano composite granules, its preparation method and the application of antibacterial and mouldproof smelly eliminating |
| CN111872414A (en) * | 2020-06-12 | 2020-11-03 | 辽宁科技大学 | Preparation method of micro-nano pre-alloyed powder |
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Open date: 20100616 |