CN107867712A - A kind of active nano-ZnO - Google Patents
A kind of active nano-ZnO Download PDFInfo
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- CN107867712A CN107867712A CN201711025034.6A CN201711025034A CN107867712A CN 107867712 A CN107867712 A CN 107867712A CN 201711025034 A CN201711025034 A CN 201711025034A CN 107867712 A CN107867712 A CN 107867712A
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- C01G9/02—Oxides; Hydroxides
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Abstract
The invention provides a kind of active nano-ZnO, its preparation technology includes（1）Zinc sulfate is weighed, adds absolute ethyl alcohol, supersonic oscillations, as solution A；（2）Sodium Polyacrylate, calgon tune pH value are weighed to 9 10, as solution B；（3）Citric acid is weighed, regulation pH value of solution is to 3.5 4.5, as solution C；（4）Solution A, solution B, potassium carbonate are mixed, centrifuge to obtain white depositions D；(5) sediment D is poured into the beaker for the n-hexane solvent for being contained with methyl-silicone oil, obtained solution E（6）It is brought rapidly up to 280 320 DEG C, constant temperature, adds solution C；（7）It is brought rapidly up to 420 440 DEG C, constant temperature, adds AEO, VTES；（8）Cooling, centrifuge, wash, centrifuge, dry, produce.This method is simple, and reaction time is short, and yield is high, and activity is high, and diameter is small, and specific surface area is big, and size is homogeneous, good dispersion, improves the application performance of nano zine oxide.
Description
The present patent application is application number CN201610531154.2, the applying date 2016 year 07 month 07 day, denomination of invention " one
The divisional application of the preparation technology of kind active nano-ZnO ".
Technical field
The present invention relates to technical field of inorganic material, more particularly to a kind of active nano-ZnO and its preparation technology.
Background technology
Nano zine oxide is a kind of multi-functional new inorganic material, and its granular size is about at 1~100 nanometer.Due to
The granular of crystal grain, its Electronic Structure and crystal structure change, and generate the surface effect that macro object does not have
Should, bulk effect, quantum size effect and the features such as macroscopical tunnel-effect and the high grade of transparency, polymolecularity.Discovered in recent years
It shows many specific functions in catalysis, optics, magnetics, mechanics etc., makes it in ceramics, chemical industry, electronics, optics, life
There is important application value in many fields such as thing, medicine, have particularity and purposes that common zinc oxide can not compare.Nanometer
Zinc oxide can be used for ultraviolet light masking material, antiseptic, fluorescent material, catalysis material etc. in fields such as weaving, coating.Due to
The a series of superiority of nano zine oxide and very tempting application prospect, therefore research and development nano zine oxide turns into many science and technology
Personnel's focus of attention.
105 tons of the zinc oxide for industrial use is produced per annual meeting, production method mainly has three approach.
（1）Indirect method（France）
After pure metallic zinc melts in graphite crucible, higher than 907 DEG C（Generally at 1000 DEG C or so）At a temperature of evaporate shape
Into the steam of zinc, steam is oxidized by oxygen generation zinc oxide in atmosphere, and this oxidizing process can send glittering light companion simultaneously
With the reduction of temperature, subsequent Zinc oxide particles are collected in a dust storage chamber by a cooling dispatch tube.This synthesis
Method was popularized by Frenchman LeClaire in 1844 and opened, therefore the method is also referred to as method national law.What this method obtained
Product is usually the Zinc oxide particles of average-size 0.1 to several millimeters.By weight, in the world most zinc oxide be by
The manufacture of this method.
（2）Direct method（The U.S.）
Direct method using the accessory substance after impure zinc compound such as calamine or metal zinc refining as raw material, first use by raw material
Carbon（Such as anthracite）Heating reduction generates zinc fume, and then steam is oxidized to zinc oxide with indirect method.Because the purity of raw material
It is relatively low, so the final product that direct method obtains is lower compared to the product quality of indirect method.
（3）Wet chemical
The industrial products of sub-fraction are to produce zinc carbonate or hydroxide by raw material through chemical reaction of pure zinc salt solution
Zinc precipitates.By filtering, wash, after drying, roasting obtains product to precipitation at a temperature of 800 °C or so.
Have many dedicated for synthesis scientific research and the method for the zinc oxide of some special-purposes.Can be by these methods according to institute
Obtain the form of zinc oxide（Block zinc oxide, zinc-oxide film, zinc oxide nanowire）, synthesis temperature（Close to room temperature low temperature or
Temperature is close to 1000 °C of high temperature）, processing method（Vapour deposition or solution growth）Or other specification be divided into it is a variety of.
The monocrystalline of large volume（Volume reaches several cubic centimetres）It is typically to use Vapor-phase transport method（Vapour deposition process）, hydro-thermal close
Prepared into method or melt growth method.But because the vapour pressure of zinc oxide is very high, melt growth method is not suitable for cultivating oxygen
Change zinc monocrystalline.The more difficult control of Vapor-phase transport method developing zinc oxide monocrystalline, this to tend to make when preparing the monocrystalline of zinc oxide
Use hydro-thermal method.The preparation method of zinc-oxide film includes chemical vapour deposition technique, Metalorganic chemical vapor deposition method, electrochemistry
Sedimentation（Electrophoretic deposition）, pulsed laser deposition, sputtering, sol-gal process, ald
Method, spray pyrolysis etc..But obtained zinc oxide nano rod material diameter is thicker, specific surface area is smaller, and size is not
Homogeneous, dispersiveness is also not good enough, have impact on the application performance of nano zine oxide.
The content of the invention
To overcome above-mentioned deficiency, the present invention provides a kind of preparation technology of active nano-ZnO.
The present invention takes following technical scheme to realize：A kind of active nano-ZnO, its preparation method include with
Lower step：
（1）Zinc sulfate is weighed to be put into 10mL test tubes, add absolute ethyl alcohol, through power be 80% supersonic oscillations 1.5-2.5h,
It is standby as solution A；
（2）Weigh Sodium Polyacrylate, calgon is put into 100mL test tubes, and add deionized water and adjust pH value to 9-10,
It is standby as solution B through the supersonic oscillations 1-3h that power is 80%；
（3）Citric acid is weighed, adds deionized water, regulation pH value of solution is standby as solution C to 3.5-4.5；
（4）Solution A, solution B are added to be contained with the 500mL beakers of potassium carbonate and mixed jointly, beaker is placed in magnetic agitation
On device, stir at room temperature to being completely dissolved, centrifuge to obtain white depositions D；
（5）By step（4）Gained sediment D is poured into the beaker for the n-hexane solvent for being contained with methyl-silicone oil, and beaker is placed in
On magnetic stirring apparatus, stir at room temperature to being completely dissolved, obtained solution E；
（6）By step（5）It is brought rapidly up to 280-320 DEG C, constant temperature, is slowly added to solution C, uniform stirring 25-35min；
（7）By step（6）It is brought rapidly up to 420-440 DEG C, constant temperature, is slowly added to AEO, the second of vinyl three
TMOS, uniform stirring 45-55min；
（8）By step（7）Solution naturally cools to room temperature, and absolute ethyl alcohol 60-70mL is added into obtained mixture, through centrifugation
Sediment is obtained, is washed again with absolute ethyl alcohol 80-100mL, is centrifuged, dries, obtains active nano-ZnO.
Wherein, step（1）In use absolute ethyl alcohol 10-15mL per 2g zinc sulfate.
Wherein, step（2）Middle Sodium Polyacrylate usage amount 2-4g, calgon usage amount 1-3g.
Wherein, step（3）Middle citric acid usage amount is 5-7mL.
Wherein, step（4）The usage amount of middle potassium carbonate is 0.5-0.7g.
Wherein, step（7）The usage amount of middle AEO is 1-5g, VTES use
Measure as 6-8g.
Wherein, the average grain diameter of the active nano-ZnO is 11nm or 12nm.
Wherein, the specific surface area of the active nano-ZnO is 82m2/ g or 83m2/g。
Wherein, the real density of the active nano-ZnO is 8.8g/cm3Or 8.9 g/cm3。
In summary the invention has the advantages that：Preparation method of the present invention is simple, and reaction time is short, and yield is high,
Obtained nano zine oxide activity is high, and diameter is small, and specific surface area is big, and size is homogeneous, good dispersion, improves nano oxidized
The application performance of zinc, it is adapted to large-scale production.
（1）The two end number mixing dispersant that the present invention is formed using Sodium Polyacrylate, calgon, collective effect, point
Dissipate property to improve, be adsorbed in nano zine oxide crystalline substance nucleating surface, cladding nano zinc oxide particles surface, be advantageous to limit its nucleation chi
The very little and direction of growth, promote the dispersion effect of nano zine oxide；
（2）From citric acid to the hydroxyl of surface of nanometer zinc oxide bonding reaction occurs for the present invention, make nano granular of zinc oxide it
Between be not easy to reunite, improve the dispersiveness of nano zine oxide, increase the specific surface area of nano zine oxide；
（3）The present invention selects the n-hexane solvent dissolved with methyl-silicone oil, and siliceous deposits modification is carried out on the surface of nano zine oxide,
The dissolution of nano zine oxide is inhibited, further increasing the dispersiveness of nano zine oxide；
（4）Particle Size of Nanometer ZnO 10-15nm prepared by the present invention, specific surface area is big, good dispersion, chemism height etc..
Embodiment
To be easy to understand the technical means, the inventive features, the objects and the advantages of the present invention, with reference to
Embodiment, the present invention is expanded on further.
A kind of preparation technology of active nano-ZnO, comprises the following steps：（1）Weigh zinc sulfate 2g and be put into 10mL test tubes
In, 10-15mL absolute ethyl alcohols are added, it is standby as solution A through the supersonic oscillations 1.5-2.5h that power is 80%；
（2）Weigh Sodium Polyacrylate 2-4g, calgon 1-3g is put into 100mL test tubes, and add deionized water regulation pH
Value is standby as solution B through power is 80% supersonic oscillations 1-3h to 9-10；
（3）Citric acid 5-7mL is weighed, adds deionized water, regulation pH value of solution is standby as solution C to 3.5-4.5；
（4）Solution A, solution B are added to be contained with the 500mL beakers of 0.5-0.7g potassium carbonate and mixed jointly, beaker is placed in
On magnetic stirring apparatus, stir at room temperature to being completely dissolved, centrifuge to obtain white depositions D；
(5) by step（4）Gained sediment D is poured into the beaker for the n-hexane solvent for being contained with methyl-silicone oil, and beaker is placed in
On magnetic stirring apparatus, stir at room temperature to being completely dissolved, obtained solution E；
（6）By step（5）It is brought rapidly up to 280-320 DEG C, constant temperature, is slowly added to solution C, uniform stirring 25-35min；
（7）By step（6）It is brought rapidly up to 420-440 DEG C, constant temperature, is slowly added to AEO 1-5g, vinyl
Triethoxysilane 6-8g, uniform stirring 45-55min；
（8）By step（7）Solution naturally cools to room temperature, and absolute ethyl alcohol 60-70mL is added into obtained mixture, through centrifugation
Sediment is obtained, is washed again with absolute ethyl alcohol 80-100mL, is centrifuged, dries, obtains active nano-ZnO.
A kind of preparation technology of 1 active nano-ZnO of embodiment
A kind of preparation technology of active nano-ZnO, comprises the following steps：（1）Zinc sulfate 2g is weighed to be put into 10mL test tubes,
10mL absolute ethyl alcohols are added, it is standby as solution A through the supersonic oscillations 1.5h that power is 80%；
（4）Weigh Sodium Polyacrylate 2g, calgon 1g is put into 100mL test tubes, and add deionized water adjust pH value to
9, it is standby as solution B through the supersonic oscillations 1h that power is 80%；
（5）Citric acid 5mL is weighed, adds deionized water, regulation pH value of solution is standby as solution C to 3.5；
（4）Solution A, solution B are added to be contained with the 500mL beakers of 0.5g potassium carbonate and mixed jointly, beaker is placed in magnetic force
On agitator, stir at room temperature to being completely dissolved, centrifuge to obtain white depositions D；
(5) by step（4）Gained sediment D is poured into the beaker for the n-hexane solvent for being contained with methyl-silicone oil, and beaker is placed in
On magnetic stirring apparatus, stir at room temperature to being completely dissolved, obtained solution E；
（6）By step（5）It is brought rapidly up to 280 DEG C, constant temperature, is slowly added to solution C, uniform stirring 25min；
（7）By step（6）It is brought rapidly up to 420 DEG C, constant temperature, is slowly added to AEO 1g, the ethoxy of vinyl three
Base silane 6g, uniform stirring 45min；
（8）By step（7）Solution naturally cools to room temperature, absolute ethyl alcohol 60mL is added into obtained mixture, through centrifuging
Sediment, washed, centrifuged with absolute ethyl alcohol 80mL again, dried, obtain active nano-ZnO.
A kind of preparation technology of 2 active nano-ZnO of embodiment
A kind of preparation technology of active nano-ZnO, comprises the following steps：（1）Zinc sulfate 2g is weighed to be put into 10mL test tubes,
13mL absolute ethyl alcohols are added, it is standby as solution A through the supersonic oscillations 2h that power is 80%；
（4）Weigh Sodium Polyacrylate 3g, calgon 2g is put into 100mL test tubes, and add deionized water adjust pH value to
9.5, it is standby as solution B through the supersonic oscillations 2h that power is 80%；
（5）Citric acid 6mL is weighed, adds deionized water, regulation pH value of solution is standby as solution C to 4；
（4）Solution A, solution B are added to be contained with the 500mL beakers of 0.6g potassium carbonate and mixed jointly, beaker is placed in magnetic force
On agitator, stir at room temperature to being completely dissolved, centrifuge to obtain white depositions D；
(5) by step（4）Gained sediment D is poured into the beaker for the n-hexane solvent for being contained with methyl-silicone oil, and beaker is placed in
On magnetic stirring apparatus, stir at room temperature to being completely dissolved, obtained solution E；
（6）By step（5）It is brought rapidly up to 300 DEG C, constant temperature, is slowly added to solution C, uniform stirring 30min；
（7）By step（6）It is brought rapidly up to 430 DEG C, constant temperature, is slowly added to AEO 3g, the ethoxy of vinyl three
Base silane 7g, uniform stirring 50min；
（8）By step（7）Solution naturally cools to room temperature, absolute ethyl alcohol 65mL is added into obtained mixture, through centrifuging
Sediment, washed, centrifuged with absolute ethyl alcohol 90mL again, dried, obtain active nano-ZnO.
A kind of preparation technology of 3 active nano-ZnO of embodiment
A kind of preparation technology of active nano-ZnO, comprises the following steps：（1）Zinc sulfate 2g is weighed to be put into 10mL test tubes,
15mL absolute ethyl alcohols are added, it is standby as solution A through the supersonic oscillations 2.5h that power is 80%；
（6）Weigh Sodium Polyacrylate 4g, calgon 3g is put into 100mL test tubes, and add deionized water adjust pH value to
10, it is standby as solution B through the supersonic oscillations 3h that power is 80%；
（7）Citric acid 7mL is weighed, adds deionized water, regulation pH value of solution is standby as solution C to 4.5；
（4）Solution A, solution B are added to be contained with the 500mL beakers of 0.7g potassium carbonate and mixed jointly, beaker is placed in magnetic force
On agitator, stir at room temperature to being completely dissolved, centrifuge to obtain white depositions D；
(5) by step（4）Gained sediment D is poured into the beaker for the n-hexane solvent for being contained with methyl-silicone oil, and beaker is placed in
On magnetic stirring apparatus, stir at room temperature to being completely dissolved, obtained solution E；
（6）By step（5）It is brought rapidly up to 320 DEG C, constant temperature, is slowly added to solution C, uniform stirring 35min；
（7）By step（6）It is brought rapidly up to 440 DEG C, constant temperature, is slowly added to AEO 1-5g, the second of vinyl three
TMOS 6-8g, uniform stirring 55min；
（8）By step（7）Solution naturally cools to room temperature, absolute ethyl alcohol 70mL is added into obtained mixture, through centrifuging
Sediment, washed, centrifuged with absolute ethyl alcohol 100mL again, dried, obtain active nano-ZnO.
Active nano-ZnO obtained by embodiment 1-3 is detected with the nano zine oxide of in the market, compared with, such as table
Shown in 1：
The technical indicator of active nano-ZnO obtained by the embodiment 1-3 of table 1
Average grain diameter of the superfine zinc oxide obtained by 1-3 of the embodiment of the present invention than the zinc oxide of in the market as can be found from Table 1
Small, bigger than surface, density is high.
Described above is embodiments of the invention, therefore all construction, feature and principle institutes according to described in the present patent application scope
The equivalent change or modification done, is included in the range of present patent application.
Claims (9)
- A kind of 1. active nano-ZnO, it is characterised in that：Preparation method comprises the following steps,（1）Zinc sulfate is weighed to be put into 10mL test tubes, add absolute ethyl alcohol, through power be 80% supersonic oscillations 1.5-2.5h, It is standby as solution A；（2）Weigh Sodium Polyacrylate, calgon is put into 100mL test tubes, and add deionized water and adjust pH value to 9-10, It is standby as solution B through the supersonic oscillations 1-3h that power is 80%；（3）Citric acid is weighed, adds deionized water, regulation pH value of solution is standby as solution C to 3.5-4.5；（4）Solution A, solution B are added to be contained with the 500mL beakers of potassium carbonate and mixed jointly, beaker is placed in magnetic agitation On device, stir at room temperature to being completely dissolved, centrifuge to obtain white depositions D；（5）By step（4）Gained sediment D is poured into the beaker for the n-hexane solvent for being contained with methyl-silicone oil, and beaker is placed in On magnetic stirring apparatus, stir at room temperature to being completely dissolved, obtained solution E；（6）By step（5）It is brought rapidly up to 280-320 DEG C, constant temperature, is slowly added to solution C, uniform stirring 25-35min；（7）By step（6）It is brought rapidly up to 420-440 DEG C, constant temperature, is slowly added to AEO, the second of vinyl three TMOS, uniform stirring 45-55min；（8）By step（7）Solution naturally cools to room temperature, and absolute ethyl alcohol 60-70mL is added into obtained mixture, through centrifugation Sediment is obtained, is washed again with absolute ethyl alcohol 80-100mL, is centrifuged, dries, obtains active nano-ZnO.
- 2. active nano-ZnO as claimed in claim 1, it is characterised in that：Step（1）In use anhydrous second per 2g zinc sulfate Alcohol 10-15mL.
- 3. active nano-ZnO as claimed in claim 1 or 2, it is characterised in that：Step（2）Middle Sodium Polyacrylate usage amount 2- 4g, calgon usage amount 1-3g.
- 4. active nano-ZnO as claimed in claim 1 or 2, it is characterised in that：Step（3）Middle citric acid usage amount is 5- 7mL。
- 5. active nano-ZnO as claimed in claim 1 or 2, it is characterised in that：Step（4）The usage amount of middle potassium carbonate is 0.5-0.7g。
- 6. active nano-ZnO as claimed in claim 1 or 2, it is characterised in that：Step（7）Middle AEO Usage amount is 1-5g, the usage amount of VTES is 6-8g.
- 7. active nano-ZnO as claimed in claim 1 or 2, it is characterised in that：The average grain of the active nano-ZnO Footpath is 11nm or 12nm.
- 8. active nano-ZnO as claimed in claim 1 or 2, it is characterised in that：The ratio surface of the active nano-ZnO Product is 82m2/ g or 83m2/g。
- 9. active nano-ZnO as claimed in claim 1 or 2, it is characterised in that：The active nano-ZnO it is true close Spend for 8.8g/cm3Or 8.9 g/cm3。
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| CN1533985A (en) * | 2003-03-31 | 2004-10-06 | 上海大学 | Preparation method of nano-grade zinc oxide powder |
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| US9376319B2 (en) * | 2011-06-10 | 2016-06-28 | Sakai Chemical Industry Co., Ltd. | Rounded zinc peroxide particles, rounded zinc oxide particles, method for production thereof, cosmetic and heat releasing filler |
| CN104386735A (en) * | 2014-11-03 | 2015-03-04 | 苏州市泽镁新材料科技有限公司 | Preparation method of zinc oxide |
| CN105036178B (en) * | 2015-07-20 | 2016-06-29 | 苏州宇希新材料科技有限公司 | A kind of preparation method of modified nano zinc oxide |
| CN105152200A (en) * | 2015-07-20 | 2015-12-16 | 苏州宇希新材料科技有限公司 | Silicon deposition modified nano zinc oxide inorganic powder material |
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