CN106064828A - Solid phase method prepares the method for Zinc oxide powder - Google Patents
Solid phase method prepares the method for Zinc oxide powder Download PDFInfo
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- CN106064828A CN106064828A CN201610606642.5A CN201610606642A CN106064828A CN 106064828 A CN106064828 A CN 106064828A CN 201610606642 A CN201610606642 A CN 201610606642A CN 106064828 A CN106064828 A CN 106064828A
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- zinc oxide
- oxide powder
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- phase method
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention relates to the preparation of Zinc oxide powder, the method that specifically solid phase method prepares Zinc oxide powder, it includes zinc nitrate hexahydrate and sodium carbonate solid mixed grinding；Then mixture is placed in ammonia spirit washing, then uses dehydrated alcohol drip washing；Then carry out being aged, sucking filtration, obtain presoma；Presoma is dried, calcines, obtain nanometer Zinc oxide powder.The present invention uses zinc nitrate hexahydrate and sodium carbonate solid and series of processes condition, can prepare Nano-class zinc oxide, and it is compared with the techniques such as liquid phase method, not only low cost, good process repeatability, and mass particle is higher.
Description
Technical field
The present invention relates to Zinc oxide powder prepare, the method that specifically solid phase method prepares Zinc oxide powder.
Background technology
Zinc oxide is a kind of new and high technology material of discovered in recent years, and being that only a few is several can realize quantum size effect
Oxide semiconductor material.Traditional zinc oxide material is widely used in pottery, piezoelectric transducer, catalyst and luminous organ
The fields such as part.Along with the further investigation of nano zine oxide preparation technology, the super-refinement of zinc oxide particles so that it is present tradition oxygen
Change property not available for zinc, such as nontoxic and non-migratory, fluorescence, piezoelectricity, absorption and scatters ultraviolet ability etc.,
Thus have broad application prospects.
For the application of nano-powder, its dispersibility and stability are most important.But owing to nano particle diameter is little,
Specific surface area is big, and interface atoms number is many, there is a large amount of unsaturated bond and dangling bond, and chemism is high, adds intergranular model moral
Hua Li, electrostatic force and surface tension etc., easily make nano-particle form larger-size aggregate.Nano powder after reunion
Body, has excellent specific property by the many losing himself so that it is usefulness cannot give full play to, and also will have a strong impact on nano-powder
Use value and application prospect.At present, the technology of preparing of Zinc oxide powder is more at liquid phase method area research, but prepared by solid phase method
Zinc oxide powder particle diameter relatively big, be difficult to meet the demand of nano material.
Summary of the invention
For above-mentioned technical problem, the present invention provides a kind of solid phase method preparing nanometer particle to prepare Zinc oxide powder
Method.
The technical solution used in the present invention is: solid phase method prepares the method for Zinc oxide powder, and it comprises the following steps:
(1) by zinc nitrate hexahydrate and sodium carbonate solid mixed grinding；
(2) then mixture is placed in ammonia spirit washing, then uses dehydrated alcohol drip washing；
(3) then carry out being aged, sucking filtration, obtain presoma；
(4) presoma is dried, calcines, obtain nanometer Zinc oxide powder.
As preferably, zinc nitrate hexahydrate is 1:(1.2 1.8 with the ratio of the amount of the material of sodium carbonate).
As preferably, milling time is 20 40min.
As preferably, the pH value of ammonia spirit is 10 11.
As preferably, during washing, ammonia spirit adds 0.5wt% surfactant.
As preferably, digestion time is 50 70min.
As preferably, temperature when presoma is dried is 70 90 DEG C.
As preferably, temperature during calcining is 400 500 DEG C, and the time is 80 100min.
As can be known from the above technical solutions, the present invention uses zinc nitrate hexahydrate and sodium carbonate solid and series of processes condition,
Can prepare Nano-class zinc oxide, it is compared with the techniques such as liquid phase method, not only low cost, good process repeatability, and mass particle
Higher.
Detailed description of the invention
The present invention is described more detail below, and illustrative examples and explanation in this present invention are used for explaining the present invention,
But it is not as a limitation of the invention.
Solid phase method prepares the method for Zinc oxide powder, and it comprises the following steps:
First, by zinc nitrate hexahydrate and sodium carbonate solid mixed grinding；These two kinds of reactants grind after being sufficiently mixed, and can release
, quickly there is pasty mixture in heat.This is because the structure of zinc nitrate hexahydrate has easy reactivity, once reaction starts,
Water of crystallization in zinc nitrate structure discharges, and reactant is easy capacitive material, discharges so solid matter is partly dissolved
In the water come, with the mixture that the product produced is mixed to form pasty state.In implementation process, preferably two reactants are first carried out pre-
Mill, then crosses 100 mesh sieves, then is ground.So reactant granule after pre-grinding is sieved is little, when grinding between reactant
Contact surface is big, and diffusion is accelerated, and reaction rate is also accelerated, so the product grain obtained is less.Usually, zinc nitrate hexahydrate with
The ratio of the amount of the material of sodium carbonate is 1:(1.2 1.8), milling time is 20 40min.Due to nitric hydrate zinc and sodium carbonate
Discharge water of crystallization, approximation concentrated solution reaction during reaction, use said ratio, the agglomeration of granule can be slowed down, improve reaction
Diffusion rate between thing, the basic zinc carbonate nucleus that suppression generates continues to grow up.
Then mixture is placed in ammonia spirit washing, then uses dehydrated alcohol drip washing；The pH value of ammonia spirit is 10
11, use this pH value, the absolute value of presoma grain surface current potential increases, and repulsive force increases, thus dispersibility improves so that grain
Footpath diminishes；Washing process the most just removes the process of foreign ion, is also to manage to reduce the process reunited between granule simultaneously.Adopt
When using ammonia scrubbing, the electric charge on precursor compound surface moves due to the existence of ion concentration difference, needs the certain time could
Reach balance；And during dehydrated alcohol drip washing, due to absorption water and constitution water with capillary form exist, ethanol dilution absorption water and
Destruction constitution water reaches poised state and needs also exist for certain time；Therefore, can reduce and reunite between granule.During washing, at ammonia
Adding 0.5wt%PAA surfactant in solution, it has dispersion effect to lead compound, and its dispersion effect is to make granule
Surface produces protective layer.
Then carry out being aged, sucking filtration, obtain presoma；Digestion time is 50 70min, and ageing contributes to the shape of protective layer
Become and reinforce；Finally being dried by presoma, calcine, obtain nanometer Zinc oxide powder, temperature when presoma is dried is 70 90
DEG C, temperature during calcining is 400 500 DEG C, and the time is 80 100min.Being dried to make the particle diameter of product become less, calcining
Basic zinc carbonate can be made to decompose, reach the Zinc oxide particles of relatively small particle.
Embodiment 1
It is grinding 20min after 1:1.2 mixes by zinc nitrate hexahydrate and sodium carbonate solid by the ratio of the amount of material；Then will
Mixture is placed in the ammonia spirit that pH value is 10 washing, adds 0.5wt%PAA surfactant in ammonia spirit, then with anhydrous
Ethanol rinse；Then it is aged 50min, then sucking filtration, obtains presoma；Presoma is dried with 70 DEG C, is then 400 in temperature
Calcine 80min at DEG C, obtain Zinc oxide particles.The particle diameter measuring Zinc oxide particles is 35nm.
Embodiment 2
It is that 1:1.5 carries out mixing pre-grinding, after 100 mesh sieves by zinc nitrate hexahydrate and sodium carbonate solid by the ratio of the amount of material
Grind 30min；Then mixture is placed in the ammonia spirit that pH value is 10.8 washing, ammonia spirit adds 0.5wt%PAA
Surfactant, then use dehydrated alcohol drip washing；Then it is aged 60min, then sucking filtration, obtains presoma；By presoma with 80 DEG C
It is dried, at temperature is 450 DEG C, then calcines 90min, obtains Zinc oxide particles.The particle diameter measuring Zinc oxide particles is
21.6nm。
Embodiment 3
It is that 1:1.8 carries out mixing pre-grinding, after 100 mesh sieves by zinc nitrate hexahydrate and sodium carbonate solid by the ratio of the amount of material
Grind 40min；Then mixture is placed in the ammonia spirit that pH value is 11 washing, ammonia spirit adds 0.5wt%PAA table
Face activating agent, then use dehydrated alcohol drip washing；Then it is aged 70min, then sucking filtration, obtains presoma；Presoma is done with 90 DEG C
Dry, at temperature is 500 DEG C, then calcines 100min, obtains Zinc oxide particles.The particle diameter measuring Zinc oxide particles is 23nm.
The technical scheme provided the embodiment of the present invention above is described in detail, specific case used herein
Principle and embodiment to the embodiment of the present invention are set forth, and the explanation of above example is only applicable to help to understand this
The principle of inventive embodiments；Simultaneously for one of ordinary skill in the art, according to the embodiment of the present invention, in specific embodiment party
All will change in formula and range of application, in sum, this specification content should not be construed as limitation of the present invention.
Claims (8)
1. the method that solid phase method prepares Zinc oxide powder, it comprises the following steps:
(1) by zinc nitrate hexahydrate and sodium carbonate solid mixed grinding；
(2) then mixture is placed in ammonia spirit washing, then uses dehydrated alcohol drip washing；
(3) then carry out being aged, sucking filtration, obtain presoma；
(4) presoma is dried, calcines, obtain nanometer Zinc oxide powder.
The method that the most according to claim 1, solid phase method prepares Zinc oxide powder, it is characterised in that: zinc nitrate hexahydrate and carbon
The ratio of the amount of the material of acid sodium is 1:(1.2 1.8).
3. the method that solid phase method prepares Zinc oxide powder as claimed in claim 1, it is characterised in that: milling time is 20
40min。
4. the method that solid phase method prepares Zinc oxide powder as claimed in claim 1, it is characterised in that: the pH value of ammonia spirit is
10—11。
5. the method that solid phase method prepares Zinc oxide powder as claimed in claim 1, it is characterised in that: during washing, at ammonia spirit
Middle interpolation 0.5wt% surfactant.
6. the method that solid phase method prepares Zinc oxide powder as claimed in claim 1, it is characterised in that: digestion time is 50
70min。
7. the method that solid phase method prepares Zinc oxide powder as claimed in claim 1, it is characterised in that: temperature when presoma is dried
It it is 70 90 DEG C.
8. the method that solid phase method prepares Zinc oxide powder as claimed in claim 1, it is characterised in that: temperature during calcining is
400 500 DEG C, the time is 80 100min.
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| CN201610606642.5A CN106064828A (en) | 2016-07-29 | 2016-07-29 | Solid phase method prepares the method for Zinc oxide powder |
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| CN201610606642.5A CN106064828A (en) | 2016-07-29 | 2016-07-29 | Solid phase method prepares the method for Zinc oxide powder |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109903883A (en) * | 2019-02-28 | 2019-06-18 | 东莞理工学院 | A kind of ZnO superfine nano particle, ZnO slurry and preparation method and application |
| CN110724831A (en) * | 2019-10-31 | 2020-01-24 | 重庆赛迪热工环保工程技术有限公司 | Carbon circulating system and method for producing zinc oxide by industrially recycling zinc |
| CN111675238A (en) * | 2020-08-03 | 2020-09-18 | 安徽景成新材料有限公司 | Method for preparing multi-morphology nano zinc oxide by solid phase method |
| CN111747441A (en) * | 2020-06-19 | 2020-10-09 | 安徽景成新材料有限公司 | Method for solid-phase synthesis of nano zinc oxide by utilizing alcohol amine compound |
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| JPH04280814A (en) * | 1991-03-11 | 1992-10-06 | Hayashi Kinzoku Kogyosho:Kk | Production of ultrafine particulate zinc white |
| CN1389404A (en) * | 2002-07-12 | 2003-01-08 | 中国科学院上海硅酸盐研究所 | Prepn. of nano-level zinc oxide powder easy to be sintered at relatively lower temperature |
| CN1548376A (en) * | 2003-05-09 | 2004-11-24 | 新疆大学 | One-step solid reaction process of preparing nano zinc oxide ball and rod at near room temperature condition |
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2016
- 2016-07-29 CN CN201610606642.5A patent/CN106064828A/en active Pending
Patent Citations (3)
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|---|---|---|---|---|
| JPH04280814A (en) * | 1991-03-11 | 1992-10-06 | Hayashi Kinzoku Kogyosho:Kk | Production of ultrafine particulate zinc white |
| CN1389404A (en) * | 2002-07-12 | 2003-01-08 | 中国科学院上海硅酸盐研究所 | Prepn. of nano-level zinc oxide powder easy to be sintered at relatively lower temperature |
| CN1548376A (en) * | 2003-05-09 | 2004-11-24 | 新疆大学 | One-step solid reaction process of preparing nano zinc oxide ball and rod at near room temperature condition |
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| Title |
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| 朱钰方: "纳米氧化锌的制备研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109903883A (en) * | 2019-02-28 | 2019-06-18 | 东莞理工学院 | A kind of ZnO superfine nano particle, ZnO slurry and preparation method and application |
| CN110724831A (en) * | 2019-10-31 | 2020-01-24 | 重庆赛迪热工环保工程技术有限公司 | Carbon circulating system and method for producing zinc oxide by industrially recycling zinc |
| CN111747441A (en) * | 2020-06-19 | 2020-10-09 | 安徽景成新材料有限公司 | Method for solid-phase synthesis of nano zinc oxide by utilizing alcohol amine compound |
| CN111675238A (en) * | 2020-08-03 | 2020-09-18 | 安徽景成新材料有限公司 | Method for preparing multi-morphology nano zinc oxide by solid phase method |
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