CN106517302A - Preparation method of nanoscale zinc oxide crystals - Google Patents
Preparation method of nanoscale zinc oxide crystals Download PDFInfo
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- CN106517302A CN106517302A CN201610923108.7A CN201610923108A CN106517302A CN 106517302 A CN106517302 A CN 106517302A CN 201610923108 A CN201610923108 A CN 201610923108A CN 106517302 A CN106517302 A CN 106517302A
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- zinc
- zinc oxide
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a preparation method of nanoscale zinc oxide crystals, and belongs to the technical field of chemical engineering. The preparation method comprises the following steps that 1, the concentration of a zinc salt solution is adjusted to be 0.8-1.8 mol/L, the zinc salt solution is heated to 35-75 DEG C, an alkaline solution is added to enable the PH of the zinc salt solution to be 11-12, a surfactant and a chemical-resistant modifying agent are added, and after reacting is conducted for 2-4 hours at the constant temperature ranging from 30 DEG C to 60 DEG C, precipitates of zinc hydroxide and zinc oxide are obtained; 2, filtering and separating are conducted to obtain a solid zinc hydroxide and zinc oxide mixture, and the zinc hydroxide and zinc oxide mixture is washed till no zinc salt negative ion is contained in washing liquid; 3, the solid mixture obtained in the step 2 is put into a flash evaporation dryer, flash evaporating, drying and crushing are conducted at the temperature of 180 DEG C to 280 DEG C, and nanoscale zinc oxide powder with the purity ranging from 96% to 99% is obtained. Modification treatment is conducted on the obtained nanoscale zinc oxide powder, and then the problem that an existing zinc oxide preparation method is high in cost is solved.
Description
Technical field
The present invention relates to chemical technology field, in particular to a kind of preparation method of Nano-class zinc oxide crystal.
Background technology
Nano-scale oxidized zinc powder is mainly used in the fields such as rubber tyre, catalyst, ceramics, uvioresistant；Particularly exist
Rubber tyre field is the important materials for manufacturing high-speed abrasion-proof tire, and the sector market capacity is huge, has very much Development volue.
The method for preparing nanometer Zinc oxide powder is divided into dry and wet, dry method mainly under certain condition by evaporate zinc ingot metal or
Zinc ore generates zinc fume, then is passed through oxygen generation Zinc Oxide, obtains finished product through trapping.Also high temperature pyrolytic cracking (HTP), by solid phase
Or liquid-phase chemical reaction prepares zinc compound, zinc compound is decomposed and obtains zinc oxide nano-powder.Moist chemical synthesis have much
Kind, mainly use precipitation pyrolysismethod and hydrothermal synthesis method.Precipitation pyrolysismethod is to add carbonate or urine in zinc solution
Element etc. is settled out basic zinc carbonate, and heating basic zinc carbonate decomposition is obtained Zinc oxide powder or produced using ammonia process；Hydro-thermal is closed
It is, with zinc hydroxide as presoma, to obtain through dehydration crystallization with a temperature of in certain pressure, need High Temperature High Pressure ability into method
Complete.From the foregoing, all there is the harsher situation of reaction condition in dry and wet, and high energy consumption is unfavorable for industrial metaplasia
Produce.
The content of the invention
It is an object of the invention to provide a kind of preparation method of Nano-class zinc oxide crystal is easy to industrial metaplasia to reach
The purpose of product, the process route of low cost, solves the problems, such as that the preparation method of existing Zinc Oxide is relatively costly.
For realizing the object of the invention, the technical scheme for adopting for：A kind of preparation method of Nano-class zinc oxide crystal, including
The following steps：
（1）Zinc solution concentration is adjusted to into 0.8-1.8mol L, 35-75 DEG C is heated to, adds aqueous slkali to make zinc salt molten to which
The PH of liquid is 11-12, surfactant and chemically-resistant modifying agent, and after isothermal reaction 2-4 hours under the conditions of 30-60 DEG C, is obtained
To zinc hydroxide and the precipitation of Zinc Oxide；
（2）It is separated by filtration and obtains solid zinc hydroxide and zinc oxide mix, zinc hydroxide and zinc oxide mix is washed
Wash, till not containing zinc salt anion in cleaning mixture；
（3）By step（2）The solid mixture for obtaining is put in flash dryer, flash distillation, drying, crushing in 180-280 DEG C,
The nano-scale oxidized zinc powder of 96-99 is obtained, nano-scale oxidized zinc powder will be obtained and be modified process.
Further, the zinc salt is one or more mixture in zinc sulfate, zinc nitrate or zinc chloride.
Further, mixed liquor of the aqueous slkali for sodium hydroxide or potassium hydroxide solution or both, its concentration are 25-
50；The concentration of the surfactant and chemically-resistant modifying agent is 5% ~ 8%.
Using the invention has the advantages that：
1. the nano-scale oxidized zinc powder for preparing is mono-crystalline structures, and structure is circular entity；Purity is high（Can reach
99%）, grain diameter is little（Individual particle TEM is in 50 ~ 100 nm）.Reaction temperature is low, and the response time is shorter, powder whiteness be 8 grades with
On；
2. the nano-scale oxidized zinc powder for preparing has activity well, is particularly well-suited to rubber tyre industry；
3. this process route material is cheap and easy to get, simple production process, working condition are gentle, do not produce pollution, easy to operate, easy
In realizing industrialized production.
Specific embodiment
The present invention is described in further detail below by specific embodiment.
Embodiment 1：
（1）The solution of zinc sulfate of 0.8mo/L and 30% sodium hydroxide solution is prepared, under 35 DEG C of water bath conditions, by 30% hydrogen
Sodium hydroxide solution, 5% surfactant and 5% chemically-resistant modifying agent are slowly added in solution of zinc sulfate, make solution PH be 11（Instead
During answering, PH is not less than 11）, 400 revs/min of mixing speed, and isothermal reaction obtained hydrogen-oxygen after 2 hours under the conditions of 35 DEG C
Change the precipitation of zinc and Zinc Oxide；
（2）It is separated by filtration and obtains solid zinc hydroxide and zinc oxide mix, by the solid mixture for obtaining distilled water wash 7
~ 8 times, till sulfate radical-free ion in filtrate；
（3）By step（2）The solid mixture for obtaining is put in flash dryer, and in 180 DEG C, flash distillation, drying, crushing, obtain
97 nano-scale oxidized zinc powder, a diameter of 75nm of powder granule, powder whiteness are 8.5 grades.
Embodiment 2：
（1）Prepare zinc sulfate, the zinc chloride mixed solution of 1.8mo/L（Both proportionings can be it is arbitrary, in the present embodiment for
1:1）, and 50% potassium hydroxide solution, under 75 DEG C of water bath conditions, by 35% potassium hydroxide solution, 8% surfactant and
8% chemically-resistant modifying agent is slowly added in zinc sulfate, zinc chloride mixed solution, makes solution PH be 12,400 revs/min of mixing speed
Clock, and after reacting 4 hours at 75 DEG C, obtain the precipitation of zinc hydroxide and Zinc Oxide；
（2）It is separated by filtration and obtains solid zinc hydroxide and zinc oxide mix, by the solid mixture for obtaining distilled water wash 7
~ 8 times, till sulfate radical-free ion in filtrate；
（3）By step（2）The solid mixture for obtaining is put in flash dryer, and in 280 DEG C, flash distillation, drying, crushing, obtain
99 nano-scale oxidized zinc powder, a diameter of 65nm of powder granule, powder whiteness are 8.8 grades.
The preferred embodiments of the present invention are the foregoing is only, the present invention is not limited to, for the skill of this area
For art personnel, the present invention can have various modifications and variations.It is all within the spirit and principles in the present invention, made any repair
Change, equivalent, improvement etc., should be included within the scope of the present invention.
Claims (3)
1. a kind of preparation method of Nano-class zinc oxide crystal, comprises the following steps：
（1）Zinc solution concentration is adjusted to into 0.8-1.8mol L, 35-75 DEG C is heated to, adds aqueous slkali to make zinc salt molten to which
The PH of liquid is 11-12, surfactant and chemically-resistant modifying agent, and after isothermal reaction 2-4 hours under the conditions of 30-60 DEG C, is obtained
To zinc hydroxide and the precipitation of Zinc Oxide；
（2）It is separated by filtration and obtains solid zinc hydroxide and zinc oxide mix, zinc hydroxide and zinc oxide mix is washed
Wash, till not containing zinc salt anion in cleaning mixture；
（3）By step（2）The solid mixture for obtaining is put in flash dryer, flash distillation, drying, crushing in 180-280 DEG C,
The nano-scale oxidized zinc powder of 96-99 is obtained, nano-scale oxidized zinc powder will be obtained and be modified process.
2. the preparation method of Nano-class zinc oxide crystal according to claim 1, it is characterised in that the zinc salt is sulphuric acid
One or more mixture in zinc, zinc nitrate or zinc chloride.
3. the preparation method of Nano-class zinc oxide crystal according to claim 1, it is characterised in that the aqueous slkali is hydrogen
The mixed liquor of sodium oxide or potassium hydroxide solution or both, its concentration are 25-50；The surfactant and chemically-resistant are modified
The concentration of agent is 5% ~ 8%.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610923108.7A CN106517302A (en) | 2016-10-29 | 2016-10-29 | Preparation method of nanoscale zinc oxide crystals |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610923108.7A CN106517302A (en) | 2016-10-29 | 2016-10-29 | Preparation method of nanoscale zinc oxide crystals |
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| CN201610923108.7A Pending CN106517302A (en) | 2016-10-29 | 2016-10-29 | Preparation method of nanoscale zinc oxide crystals |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108059184A (en) * | 2017-12-28 | 2018-05-22 | 兰州大学 | A kind of method that ZnO nanoparticle is prepared using recombined collagen as biomineralization template |
| CN109369994A (en) * | 2018-11-15 | 2019-02-22 | 赛轮集团股份有限公司 | A kind of low zinc rubber composition |
| CN111573711A (en) * | 2020-05-12 | 2020-08-25 | 张家港凯铭锌业有限公司 | Preparation method of zinc oxide |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101591037A (en) * | 2009-07-03 | 2009-12-02 | 北京化工大学 | A kind of one-dimensional zinc oxide nanometer material and preparation method thereof |
| CN102531037A (en) * | 2012-01-16 | 2012-07-04 | 沭阳县飞宏金属新材料有限公司 | Chemical preparation method of nanoscale zinc oxide powder |
-
2016
- 2016-10-29 CN CN201610923108.7A patent/CN106517302A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101591037A (en) * | 2009-07-03 | 2009-12-02 | 北京化工大学 | A kind of one-dimensional zinc oxide nanometer material and preparation method thereof |
| CN102531037A (en) * | 2012-01-16 | 2012-07-04 | 沭阳县飞宏金属新材料有限公司 | Chemical preparation method of nanoscale zinc oxide powder |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108059184A (en) * | 2017-12-28 | 2018-05-22 | 兰州大学 | A kind of method that ZnO nanoparticle is prepared using recombined collagen as biomineralization template |
| CN108059184B (en) * | 2017-12-28 | 2020-10-27 | 兰州大学 | Method for preparing ZnO nanoparticles by taking recombinant collagen as biomineralization template |
| CN109369994A (en) * | 2018-11-15 | 2019-02-22 | 赛轮集团股份有限公司 | A kind of low zinc rubber composition |
| CN111573711A (en) * | 2020-05-12 | 2020-08-25 | 张家港凯铭锌业有限公司 | Preparation method of zinc oxide |
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Application publication date: 20170322 |
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