CN101704544B - Method for preparing zinc oxide nano rod applied to sewage treatment - Google Patents
Method for preparing zinc oxide nano rod applied to sewage treatment Download PDFInfo
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- CN101704544B CN101704544B CN2009102125867A CN200910212586A CN101704544B CN 101704544 B CN101704544 B CN 101704544B CN 2009102125867 A CN2009102125867 A CN 2009102125867A CN 200910212586 A CN200910212586 A CN 200910212586A CN 101704544 B CN101704544 B CN 101704544B
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Abstract
The invention relates to a method for preparing a zinc oxide nano rod applied to sewage treatment, which adopts the following processing steps: dissolving zinc acetate into a glass beaker of anhydrous ethanol or anhydrous methanol to prepare suspension; putting deionized water into the prepared suspension to prepare mixed solution; preparing evenly mixed solution by n-propyl alcohol and caprolactam at the room temperature; pouring the prepared solution into the prepared mixed solution in equal volume at the room temperature, and mechanically stirring the solution to obtain white colloid mixed solution; putting the white colloid mixed solution into a hydrothermal reaction kettle, preserving the heat of the sealed reaction kettle, and then taking the reaction solution out; and centrifugal separating the rest solid-liquid mixture, washing the separated solid by water, and drying the solid to obtain the ZnO nano rod.
Description
Technical field
The present invention relates to a kind of preparation method who is applied to the zinc oxide nano rod of WWT, belong to new material technology field.
Background technology
In energetic 21 century; The high speed development of information, biotechnology, the energy, environment, advanced manufacturing technology and national defence must propose new demand to material, and the miniaturized of element, intellectuality, high integrated, high-density storage and ultrafast transmission etc. are more and more littler to the dimensional requirement of material; Aerospace, novel military equipment and advanced manufacturing technology etc. are increasingly high to material performance requirement.The innovation of novel material, and the new technology of bringing out on this basis.The innovation of product innovation is 10 years futures social development, economic revival, national power to be strengthened the most influential Strategic research area, and nano material will be one of critical material that plays an important role.Nano material and nanostructure be the most dynamic in the current novel material research field, the future economy and social development are had the very research object of material impact, also be the most active in the nanosecond science and technology, near the important component part of using.In recent years, nano material and nanostructure have obtained conspicuous achievement.Nanotechnology is irreplaceable technology to the degraded of 200 nanometer pollutents in 20 nanometers and the water in the air.Want environment purification, must use nanotechnology.Utilize TiO
2, ZnO makes up photocatalysis nano material, successfully is used for the organic degraded of sewage, the organic pollutant that the Pyrogentisinic Acid waits other conventional art to be difficult to degrade has good degradation effect.In recent years, many companies are devoted to be transplanted to the water treatment industry to nanotechnologies such as photochemical catalysis, are used to improve the quality of water, win initial success.But these all are TiO
2With ZnO nanoparticle technology, also the ZnO nanometer rod is not applied to the WWT aspect so far.Method through gas phase or chemistry has prepared various nano zine oxide structures at present.Hydrothermal method have equipment and simple to operate, environmental pollution is little and the characteristics of suitable scale operation, has become the important method of preparation ZnO nanometer rod.
Summary of the invention
The objective of the invention is to overcome above-mentioned weak point, thereby a kind of preparation method who is applied to the zinc oxide nano rod of WWT is provided, preparation technology is simple, the diameter of particle narrow distribution, and good dispersivity, the degradation rate of tropeolin-D reaches 99.50%.
According to technical scheme provided by the invention, a kind of preparation method who is applied to the zinc oxide nano rod of WWT, adopt following process step:
A, be dissolved in zinc acetate 20-30 weight part in the glass beaker of absolute ethyl alcohol 100-200 weight part or anhydrous methanol 100-150 weight part, fully stir under the room temperature, be mixed with mass percentage concentration and be 1～40% suspension liquid;
B, process mixing solutions with putting into deionized water in the prepared suspension liquid of step a, the mass ratio of deionized water and suspension liquid is 2-3: 1;
Be 0.2-2 with n-propyl alcohol and hexanolactam by mass ratio under c, the room temperature: 1 processes the solution that mixes;
Under d, the room temperature, the solution that step c is made is isopyknic pours the mixing solutions that step b makes into, carries out mechanical stirring, white colloidal mixing solutions;
E, white colloidal mixing solutions is put into hydrothermal reaction kettle, with the reaction kettle after the sealing, in the insulation 3～18 hours down of 60～250 ℃ of temperature, take out reaction soln, remaining solidliquid mixture gets into centrifuge separator to be separated;
6, the solid that the solidliquid mixture spinning is gone out was dried 3～15 hours under 30～70 ℃ of conditions of temperature with water washing 20 minutes, obtained the ZnO nanometer rod.The particle diameter of said ZnO nanometer rod is 50-300nm:
Compared with present technology the present invention has the following advantages:
The effect of the photocatalysis degradation organic contaminant tropeolin-D of zinc oxide nano rod of the present invention is superior to existing titanium dioxide nano-particle (particle diameter＜30nm) and common zinc oxide nano-particle (particle diameter 8-35nm); When the consumption of ZnO nanometer rod was 3g/L, as the irradiation of 10mg/L methyl orange solution after 60 minutes, the degradation rate of tropeolin-D reached 99.50% to the uv lamp that uses 300W to concentration; Preparation technology is simple, the diameter of particle narrow distribution, and good dispersivity, industrial prospect is good, is the Perfected process of preparation nano zine oxide; Be not a kind of new material to be provided for WWT.
Embodiment
Embodiment one: a kind of preparation method who is applied to the zinc oxide nano rod of WWT of the present invention, adopt following process step:
1, is dissolved in zinc acetate 20 weight parts in the glass beaker of absolute ethyl alcohol 100 weight parts, fully stirs under the room temperature, be mixed with mass percentage concentration and be 1% suspension liquid;
2, process mixing solutions with putting into deionized water in the prepared suspension liquid of step 1, the mass ratio of deionized water and suspension liquid is 2: 1;
3, be to process the solution that mixes at 0.2: 1 with n-propyl alcohol and hexanolactam by mass ratio under the room temperature;
4, under the room temperature, the solution that step 3 is made is isopyknic pours the mixing solutions that step 2 makes into, carries out mechanical stirring, white colloidal mixing solutions;
5, white colloidal mixing solutions is put into hydrothermal reaction kettle, the hydrothermal reaction kettle model is KH-200, with the reaction kettle after the sealing, is incubated 3 hours down at 60 ℃, takes out reaction soln; Remaining solidliquid mixture gets into centrifuge separator to be separated;
6, with remaining solidliquid mixture spinning, the centrifuge separator model is TPR I-CY, and isolated solid is with water washing 20 minutes, is oven dry 3 hours under 30 ℃ the condition in temperature, obtains the ZnO nanometer rod.The particle diameter of said ZnO nanometer rod is 50nm:
Embodiment two:
1, is dissolved in zinc acetate 30 weight parts in the glass beaker of anhydrous methanol 150 weight parts, fully stirs under the room temperature, be mixed with mass percentage concentration and be 40% suspension liquid;
2, process mixing solutions with putting into deionized water in the prepared suspension liquid of step 1, the mass ratio of deionized water and suspension liquid is 3: 1;
3, be to process the solution that mixes at 2: 1 with n-propyl alcohol and hexanolactam by mass ratio under the room temperature;
4, under the room temperature, the solution that step 3 is made is isopyknic pours the mixing solutions that step 2 makes into, carries out mechanical stirring, white colloidal mixing solutions;
5, white colloidal mixing solutions is put into hydrothermal reaction kettle, the hydrothermal reaction kettle model is KH-200, with the reaction kettle after the sealing, is incubated 18 hours down at 250 ℃, takes out reaction soln; Remaining solidliquid mixture gets into centrifuge separator to be separated;
6, with remaining solidliquid mixture spinning, the centrifuge separator model is TPRI-CY, and isolated solid is with water washing 20 minutes, is oven dry 15 hours under 70 ℃ the condition in temperature, obtains the ZnO nanometer rod.The particle diameter of said ZnO nanometer rod is 300nm:
Embodiment three:
1, is dissolved in zinc acetate 25 weight parts in the glass beaker of anhydrous methanol 150 weight parts, fully stirs under the room temperature, be mixed with mass percentage concentration and be 20% suspension liquid;
2, process mixing solutions with putting into deionized water in the prepared suspension liquid of step 1, the mass ratio of deionized water and suspension liquid is 2.5: 1;
3, be to process the solution that mixes at 1.2: 1 with n-propyl alcohol and hexanolactam by mass ratio under the room temperature;
4, under the room temperature, the solution that step 3 is made is isopyknic pours the mixing solutions that step 2 makes into, carries out mechanical stirring, white colloidal mixing solutions;
5, white colloidal mixing solutions is put into hydrothermal reaction kettle, the hydrothermal reaction kettle model is KH-200, with the reaction kettle after the sealing, is incubated 12 hours down at 120 ℃, takes out reaction soln; Remaining solidliquid mixture gets into centrifuge separator to be separated;
6, with the solidliquid mixture spinning, the centrifuge separator model is TPRI-CY, and isolated solid is with water washing 20 minutes, is oven dry 8 hours under 50 ℃ the condition in temperature, obtains the ZnO nanometer rod.The particle diameter 150nm of said ZnO nanometer rod:
Claims (2)
1. preparation method who is applied to the zinc oxide nano rod of WWT is characterized in that: adopt following process step:
A, be dissolved in zinc acetate 20-30 weight part in the glass beaker of absolute ethyl alcohol 100-200 weight part or anhydrous methanol 100-150 weight part, fully stir under the room temperature, be mixed with mass percentage concentration and be 20% suspension liquid;
B, process mixing solutions with putting into deionized water in the prepared suspension liquid of step a, the mass ratio of deionized water and suspension liquid is 2-3: 1;
C, at room temperature be 0.2-2 with n-propyl alcohol and hexanolactam by mass ratio: 1 processes the solution that mixes;
D, at room temperature, the solution that step c is made is isopyknic pours the mixing solutions that step b makes into, carries out mechanical stirring, white colloidal mixing solutions;
E, white colloidal mixing solutions is put into hydrothermal reaction kettle, with the reaction kettle after the sealing, in the insulation 3～18 hours down of 60～250 ℃ of temperature, take out reaction soln, remaining solidliquid mixture gets into centrifuge separator to be separated;
F, solid that the solidliquid mixture spinning is gone out were dried 3～15 hours under 30～70 ℃ of conditions of temperature with water washing 20 minutes, obtained the ZnO nanometer rod.
2. a kind of preparation method who is applied to the zinc oxide nano rod of WWT according to claim 1, the particle diameter that it is characterized in that described ZnO nanometer rod is 50-300nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2009102125867A CN101704544B (en) | 2009-11-13 | 2009-11-13 | Method for preparing zinc oxide nano rod applied to sewage treatment |
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| CN2009102125867A CN101704544B (en) | 2009-11-13 | 2009-11-13 | Method for preparing zinc oxide nano rod applied to sewage treatment |
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| CN101704544A CN101704544A (en) | 2010-05-12 |
| CN101704544B true CN101704544B (en) | 2012-01-18 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103224249B (en) * | 2013-05-20 | 2014-12-31 | 重庆大学 | Synthesis method of zinc oxide aggregate |
| CN105174300A (en) * | 2015-09-30 | 2015-12-23 | 景德镇陶瓷学院 | Preparation method of ZnO micro-nano ball powder with multilevel structure and product prepared with method |
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Effective date of registration: 20180725 Address after: 213025 the standard workshop of Hutang science and Technology Industrial Park Industrial Park, Hutang Town, Wujin District, Changzhou, Jiangsu Patentee after: JIANGSU NATURAL TEXTILE TECHNOLOGY Co.,Ltd. Address before: 214101 99 Xishan road three, Xishan Economic Development Zone, Wuxi, Jiangsu Patentee before: Wuxi Taida Textile Technology Co.,Ltd. |
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