CN107265493B - A kind of method that microwave radiation prepares nano zine oxide - Google Patents
A kind of method that microwave radiation prepares nano zine oxide Download PDFInfo
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- CN107265493B CN107265493B CN201710416128.XA CN201710416128A CN107265493B CN 107265493 B CN107265493 B CN 107265493B CN 201710416128 A CN201710416128 A CN 201710416128A CN 107265493 B CN107265493 B CN 107265493B
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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Abstract
The present invention discloses a kind of method that microwave radiation thermal decomposition prepares nano zine oxide, including following operating procedure：（1）Prepare nano zine oxide predecessor；（2）By nano zine oxide predecessor and alcohols material ground and mixed；（3）By step（2）The substance of gained and 1,1 cyclopropyl dicarboxylic acids, 3 carboxylic acid ground and mixed of quinoline；（4）By step（3）The modified Nano oxidisability predecessor of gained carries out microwave radiation thermal decomposition, and nano zine oxide is made.The method that microwave radiation provided by the invention prepares nano zine oxide, operating procedure is simple, and process stabilizing is, it can be achieved that continuous industrialized production.
Description
Technical field
The invention belongs to field of nanometer technology, and in particular to a kind of method that microwave radiation prepares nano zine oxide.
Background technology
Nano zine oxide is a kind of new inorganic material of multifunctionality, and granular size is about at 1-100 nanometers.Due to crystalline substance
The imperceptibility of grain, Electronic Structure and crystal structure change, produce skin effect that macro object do not have,
The features such as bulk effect, quantum size effect and macroscopical tunnel-effect and the high grade of transparency, polymolecularity.Discovered in recent years it
Catalysis, optics, magnetics, mechanics etc. show many specific functions, make it in ceramics, chemical industry, electronics, optics, biology, doctor
There is important application value in many fields such as medicine, the particularity and purposes that can not compare with common zinc oxide.It is nano oxidized
Zinc can be used for ultraviolet light masking material, antiseptic, fluorescent material, catalysis material etc. in fields such as weaving, coating.Due to nanometer
The a series of superiority of zinc oxide and very tempting application prospect, therefore research and develop nano zine oxide and have become many scientific and technical personnel
Focus of attention.Using being easily mixed into chemical method product, impurity, particle are easily reunited, there is pollutions etc. one in production process at present
Series of problems is to be resolved；Nanoscale cannot be fully achieved in the product that mechanical attrition method in physical preparation method obtains；Laser
Aggregation atom deposition method can not also accomplish industrialized production.
Microwave heating is a kind of heating means of green high-efficient, not only have selective heated material, heating rate fast plus
The advantages that thermal efficiency is high, and can also reduce reaction temperature, shorten reaction time, promote it is energy-saving.Although existing skill
Have in art and heating nanometer zinc oxide precursor is prepared using microwave radiation prepare the technique of nano zine oxide, but it is in practical behaviour
It is found in work, obtained nano zine oxide purity is inadequate, wherein containing more undecomposed nano zine oxide predecessor, seriously
Reduce the quality of nano zine oxide.
Invention content
In order to solve the deficiencies in the prior art, the present invention provides a kind of method that microwave radiation prepares nano zine oxide.
The present invention is achieved by the following technical solutions.
A kind of method that microwave radiation prepares nano zine oxide, including following operating procedure：
（1）Prepare nano zine oxide predecessor；
（2）By nano zine oxide predecessor and alcohols material ground and mixed；
（3）By step（2）The substance of gained and 1,1- cyclopropyl dicarboxylic acids, quinoline-3-carboxylic acid ground and mixed；
（4）By step（3）The modified Nano oxidisability predecessor of gained carries out microwave radiation thermal decomposition, is made nano oxidized
Zinc.
Specifically, the step（1）The middle method for preparing nano zine oxide predecessor is：The urine for being 70% by mass fraction
The solution of zinc sulfate that plain solution is 85% with mass fraction is 5-9 according to volume ratio:After 1 ratio mixing, by the temperature of mixture
After rising to 80 DEG C, 2 hours are kept the temperature, mixture is centrifuged, obtains nano zine oxide predecessor, then be baked to.
Specifically, the mass ratio of above-mentioned nano zine oxide predecessor and alcohols material is 1:4-10.
Specifically, above-mentioned alcohols material is any one in 1,2- ethohexadiols, season pentanediol.
Specifically, above-mentioned steps（2）The substance of middle gained and 1,1- cyclopropyl dicarboxylic acids, the mass ratio of quinoline-3-carboxylic acid
It is 15:4:2.
Specifically, above-mentioned steps（3）The time of middle ground and mixed is 15-30min.
Specifically, above-mentioned steps（4）It is middle radiation thermal decomposition condition be：Radiation frequency is 1700-1900MHz, thermal decomposition
Time be 15-20min.
From the above technical scheme, it can be seen that the beneficial effects of the invention are as follows：
The method that microwave radiation provided by the invention prepares nano zine oxide, operating procedure is simple, process stabilizing, it can be achieved that
Continuous industrialized production.Wherein, the present invention first fixes alcohols material by the predecessor of nano zine oxide obtained,
Then it is grafted upper 1,1- cyclopropyl dicarboxylic acids or quinoline-3-carboxylic acid, passes through the work of its superficial molecular by esterification again
With can effectively promote the ability of nano zine oxide precursor adsorption microwave, reduce reflex of its surface to microwave, in turn
The decomposition temperature that nano zine oxide predecessor can be effectively reduced, accelerates its decomposition rate, and it also has prevents nano oxygen
Change zinc precursor object to assemble, causes its decomposition to be not thorough, the impure problem of nano zine oxide obtained.
Specific implementation mode
Following embodiment cannot be used for limiting the scope of the invention for illustrating the present invention.The reality used in embodiment
The condition of applying can be for further adjustments according to the condition of producer, and unaccounted implementation condition is usually conventional laboratory conditions.
Embodiment 1
A kind of method that microwave radiation prepares nano zine oxide, including following operating procedure：
（1）Prepare nano zine oxide predecessor；
（2）By nano zine oxide predecessor and alcohols material ground and mixed；
（3）By step（2）The substance of gained and 1,1- cyclopropyl dicarboxylic acids, quinoline-3-carboxylic acid ground and mixed；
（4）By step（3）The modified Nano oxidisability predecessor of gained carries out microwave radiation thermal decomposition, is made nano oxidized
Zinc.
Specifically, the step（1）The middle method for preparing nano zine oxide predecessor is：The urine for being 70% by mass fraction
The solution of zinc sulfate that plain solution is 85% with mass fraction is 5 according to volume ratio:After 1 ratio mixing, by the temperature liter of mixture
To after 80 DEG C, 2 hours are kept the temperature, mixture is centrifuged, obtains nano zine oxide predecessor, then be baked to.
Specifically, the mass ratio of above-mentioned nano zine oxide predecessor and alcohols material is 1:4.
Specifically, above-mentioned alcohols material is 1,2- ethohexadiols.
Specifically, above-mentioned steps（2）The substance of middle gained and 1,1- cyclopropyl dicarboxylic acids, the mass ratio of quinoline-3-carboxylic acid
It is 15:4:2.
Specifically, above-mentioned steps（3）The time of middle ground and mixed is 15min.
Specifically, above-mentioned steps（4）It is middle radiation thermal decomposition condition be：Radiation frequency is 1700MHz, the time of thermal decomposition
For 15min.
Embodiment 2
A kind of method that microwave radiation prepares nano zine oxide, including following operating procedure：
（1）Prepare nano zine oxide predecessor；
（2）By nano zine oxide predecessor and alcohols material ground and mixed；
（3）By step（2）The substance of gained and 1,1- cyclopropyl dicarboxylic acids, quinoline-3-carboxylic acid ground and mixed；
（4）By step（3）The modified Nano oxidisability predecessor of gained carries out microwave radiation thermal decomposition, is made nano oxidized
Zinc.
Specifically, the step（1）The middle method for preparing nano zine oxide predecessor is：The urine for being 70% by mass fraction
The solution of zinc sulfate that plain solution is 85% with mass fraction is 7 according to volume ratio:After 1 ratio mixing, by the temperature liter of mixture
To after 80 DEG C, 2 hours are kept the temperature, mixture is centrifuged, obtains nano zine oxide predecessor, then be baked to.
Specifically, the mass ratio of above-mentioned nano zine oxide predecessor and alcohols material is 1:6.
Specifically, above-mentioned alcohols material is season pentanediol.
Specifically, above-mentioned steps（2）The substance of middle gained and 1,1- cyclopropyl dicarboxylic acids, the mass ratio of quinoline-3-carboxylic acid
It is 15:4:2.
Specifically, above-mentioned steps（3）The time of middle ground and mixed is 20min.
Specifically, above-mentioned steps（4）It is middle radiation thermal decomposition condition be：Radiation frequency is 1800MHz, the time of thermal decomposition
For 18min.
Embodiment 3
A kind of method that microwave radiation prepares nano zine oxide, including following operating procedure：
（1）Prepare nano zine oxide predecessor；
（2）By nano zine oxide predecessor and alcohols material ground and mixed；
（3）By step（2）The substance of gained and 1,1- cyclopropyl dicarboxylic acids, quinoline-3-carboxylic acid ground and mixed；
（4）By step（3）The modified Nano oxidisability predecessor of gained carries out microwave radiation thermal decomposition, is made nano oxidized
Zinc.
Specifically, the step（1）The middle method for preparing nano zine oxide predecessor is：The urine for being 70% by mass fraction
The solution of zinc sulfate that plain solution is 85% with mass fraction is 9 according to volume ratio:After 1 ratio mixing, by the temperature liter of mixture
To after 80 DEG C, 2 hours are kept the temperature, mixture is centrifuged, obtains nano zine oxide predecessor, then be baked to.
Specifically, the mass ratio of above-mentioned nano zine oxide predecessor and alcohols material is 1:10.
Specifically, above-mentioned alcohols material is season pentanediol.
Specifically, above-mentioned steps（2）The substance of middle gained and 1,1- cyclopropyl dicarboxylic acids, the mass ratio of quinoline-3-carboxylic acid
It is 15:4:2.
Specifically, above-mentioned steps（3）The time of middle ground and mixed is 30min.
Specifically, above-mentioned steps（4）It is middle radiation thermal decomposition condition be：Radiation frequency is 1900MHz, the time of thermal decomposition
For 20min.
Comparative example 1
By nano zine oxide predecessor obtained in embodiment 2, directly use radiation frequency for the microwave radiation of 1800MHz
18min is thermally decomposed, remaining processing step is identical with embodiment 2.
Character analysis, the result such as table 1 of analysis are carried out to nano zine oxide obtained in each embodiment and comparative example respectively
It is shown：
1 nano zine oxide character analysis of table
| Project | Average grain diameter/nm | Purity |
| Embodiment 1 | 35 | 99.89 |
| Embodiment 2 | 32 | 99.91 |
| Comparative example 1 | 49 | 94.28 |
| Embodiment 3 | 31 | 99.92 |
As shown in Table 1, using method provided by the invention, nano zine oxide obtained, average grain diameter is smaller, and purity compared with
The discomposing effect of height, nano zine oxide predecessor is preferable.
It should be noted that the above examples are only used to illustrate the technical scheme of the present invention and are not limiting.Although with reference to compared with
Good embodiment describes the invention in detail, it will be understood by those of ordinary skill in the art that, it can be to the technology of invention
Scheme is modified or replaced equivalently, and without departing from the range of technical solution of the present invention, should all cover the power in the present invention
In sharp claimed range.
Claims (3)
1. a kind of method that microwave radiation prepares nano zine oxide, which is characterized in that including following operating procedure：
（1）Prepare nano zine oxide predecessor；
（2）By nano zine oxide predecessor and alcohols material ground and mixed；
（3）By step（2）The substance of gained and 1,1- cyclopropyl dicarboxylic acids, quinoline-3-carboxylic acid ground and mixed；
（4）By step（3）The modified nano zinc oxide predecessor of gained carries out microwave radiation thermal decomposition, and nano zine oxide is made；
The mass ratio of wherein above-mentioned nano zine oxide predecessor and alcohols material is 1:4-10, above-mentioned alcohols material be 1,2- ethohexadiols,
Any one in season pentanediol, above-mentioned steps（2）The substance of middle gained and 1,1- cyclopropyl dicarboxylic acids, quinoline-3-carboxylic acid
Mass ratio is 15:4:2, above-mentioned steps（4）It is middle radiation thermal decomposition condition be：Radiation frequency is 1700-1900MHz, thermal decomposition
Time be 15-20min.
2. the method for preparing nano zine oxide according to a kind of microwave radiation described in claim 1, which is characterized in that step
（1）The middle method for preparing nano zine oxide predecessor is：It is 85% by urea liquid and mass fraction that mass fraction is 70%
Solution of zinc sulfate is 5-9 according to volume ratio:After 1 ratio mixing, after the temperature of mixture is risen to 80 DEG C, 2 hours are kept the temperature, it will
Mixture centrifuges, and obtains nano zine oxide predecessor, then be baked to.
3. the method for preparing nano zine oxide according to a kind of microwave radiation described in claim 1, which is characterized in that above-mentioned step
Suddenly（3）The time of middle ground and mixed is 15-30min.
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| CN108951110A (en) * | 2018-07-20 | 2018-12-07 | 安徽锦华氧化锌有限公司 | A kind of preparation method of Uvr Protective Fabric modified nano zinc oxide |
| CN109133150B (en) * | 2018-10-25 | 2021-07-09 | 河北宏贸环保科技有限公司 | Preparation method of high-purity nano zinc oxide |
| CN110787787B (en) * | 2019-10-28 | 2022-10-11 | 安徽锦华氧化锌有限公司 | Preparation method of nano zinc oxide with good photocatalytic effect performance |
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| CN1657415A (en) * | 2005-02-02 | 2005-08-24 | 苏州大学 | Preparation method of nanometer zinc oxide |
| CN106379930A (en) * | 2016-11-09 | 2017-02-08 | 上海天地涂料有限公司 | Interface microwave preparation method of zinc oxide nanometer material |
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| KR101542660B1 (en) * | 2013-09-30 | 2015-08-06 | 전북대학교산학협력단 | Manufacturing method for metal-doped ZnO (Zinc Oxide) ultra-fine powders by using plasmas |
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Patent Citations (2)
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|---|---|---|---|---|
| CN1657415A (en) * | 2005-02-02 | 2005-08-24 | 苏州大学 | Preparation method of nanometer zinc oxide |
| CN106379930A (en) * | 2016-11-09 | 2017-02-08 | 上海天地涂料有限公司 | Interface microwave preparation method of zinc oxide nanometer material |
Non-Patent Citations (2)
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| Kinetic and Thermodynamic Aspects in the Microwave-Assisted Synthesis of ZnO Nanoparticles in Benzyl Alcohol;Idalia Bilecka et al.;《ACSNANO》;20090224;第3卷(第2期);467-477 * |
| 浅谈纳米氧化锌材料的制备方式;王靖喜;《内蒙古科技与经济》;20160930(第18期);106 * |
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