CN109850933A - A kind of preparation method of the zinc oxide nano-particle for bio-imaging - Google Patents
A kind of preparation method of the zinc oxide nano-particle for bio-imaging Download PDFInfo
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- CN109850933A CN109850933A CN201910016945.5A CN201910016945A CN109850933A CN 109850933 A CN109850933 A CN 109850933A CN 201910016945 A CN201910016945 A CN 201910016945A CN 109850933 A CN109850933 A CN 109850933A
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Abstract
The invention discloses a kind of preparation methods of zinc oxide nano-particle for bio-imaging, with NH3·H2O and NH4HCO3For precipitating reagent and ZnSO4It reacts, generates by ZnCO3The Zn (OH) of package2Precursor needs to be stirred during reaction, mixing speed 200-500r/min；Wherein, ZnSO4For Zinc sulphate, the Zinc sulphate that consumption proportion is 5-10g matches 25-35mlNH3·H2O and NH4HCO3；The presoma of generation is filtered out, is roasted after being washed, maturing temperature is 100 DEG C, calcining time 70-80min；After roasting, presoma is calcined；Calcination temperature is 300-400 DEG C, calcination time 2-4h.The state modulator that the present invention passes through this method is not in too big agglomeration, more balanced, the yield and quality improved, is suitable for bio-imaging.
Description
Technical field
The present invention relates to a kind of preparation methods of zinc oxide nano-particle for bio-imaging.
Background technique
Nano-ZnO is also known as activity ZnO, a kind of novel high function fine inorganic product geared to the 21st century.Because of its spy
Different size has special function, and granular size is about in 1-100nm.Show many special properties, as non-migratory,
Absorption, fluorescence, scatters ultraviolet ability and piezoelectricity etc., by apply light, electricity, in terms of performance, purple can be manufactured
Outside line masking material, rheostat, effective catalyst, gas sensor, plastic film, fluorophor, piezoelectric material, varistor,
Image recording material and magnetic material etc..
The preparation of nano-ZnO generally can be divided into physical method and chemical method.Physical method is called comminuting method, or mechanical
Method.The zinc oxide of common grade is crushed to by special crushing technology ultra-fine.Chemical method is called comminution granulation, is certain
Under conditions of, the particle with certain shapes and size is condensed by the nucleation of atom or molecule, growth or chemical combination.Chemistry side
Method can be divided into vapor phase method, solid phase method and liquid phase method again, and the prior art mainly adopts the precipitation method in liquid phase method to be prepared.Precipitating
Based on precipitation reaction, gained sediment all needs to obtain nano oxide powder by being filtered, washed, drying and calcine method.
The common ground of all precipitation method is produced using the liquid phase reactor of production precipitating, and entire reaction equation is indicated with following formula: nA++
nB+→[AB].During preparing nano-ZnO, easily there is agglomerated particle in the prior art, and quality is low and low yield, is unfavorable for
Bio-imaging.
Therefore, how to solve above-mentioned technical problem becomes those skilled in the art's technical problem urgently to be resolved.
Summary of the invention
It is an object of the invention to provide a kind of preparation methods of zinc oxide nano-particle for bio-imaging, can be completely
Solve above-mentioned the deficiencies in the prior art place.
The purpose of the present invention is realized by following technical proposals:
A kind of preparation method of the zinc oxide nano-particle for bio-imaging, with NH3·H2O and NH4HCO3For precipitating reagent
With ZnSO4It reacts, generates by ZnCO3The Zn (OH) of package2Precursor needs to be stirred during reaction, stirring speed
Degree is 200-500r/min, reaction equation are as follows: ZnSO4+2NH3·H2O=Zn (OH)2↓+(NH4)2SO4, ZnSO4+
NH4HCO3=ZnCO3↓+(NH4)2SO4；Wherein, ZnSO4For Zinc sulphate, the Zinc sulphate that consumption proportion is 5-10g matches 25-35mlNH3·
H2O and NH4HCO3, NH3·H2O and NH4HCO3Arbitrarily to match；
The presoma of generation is filtered out, is roasted after being washed, maturing temperature is 100 DEG C, calcining time 70-
80min；
After roasting, presoma is calcined, reaction equation are as follows: Zn (OH)2=ZnO+H2O；ZnCO3=ZnO+
CO2；Calcination temperature is 300-400 DEG C, calcination time 2-4h.
Further, the NH3·H2O and NH4HCO3It is pure chemicals, is configured to the aqueous solution of 0.5mol/L.
Further, the Zinc sulphate that consumption proportion is 5-8g matches 28-35mlNH3·H2O and NH4HCO3。
Further, the Zinc sulphate that consumption proportion is 5-6g matches 28-32mlNH3·H2O and NH4HCO3。
Further, the Zinc sulphate that consumption proportion is 5g matches 30mlNH3·H2O and NH4HCO3。
Further, NH3·H2O and NH4HCO3Proportion be mass ratio 1:1.
Further, mixing speed 200-400r/min.
Further, calcining time 70-75min.
Further, calcination temperature is 400 DEG C, calcination time 2h.
It compared with prior art, is not in too big the beneficial effects of the present invention are: the state modulator by this method
Agglomeration, more balanced, the yield and quality improved, be suitable for bio-imaging.
Detailed description of the invention
Fig. 1 is flow chart of the invention；
Fig. 2 is that ZnSO is added in the present invention4·7H2The amount of O (Zinc sulphate) is in the relational graph of sediment yield；
Fig. 3 is the relational graph between reaction temperature of the present invention and the sediment of generation；
Fig. 4 is the relational graph between calcining time of the present invention and sediment；
Fig. 5 is the relational graph between calcination time of the present invention and calcining surplus.
Specific embodiment
The present invention is further illustrated with attached drawing combined with specific embodiments below.
As shown in Figure 1, a kind of preparation method of the zinc oxide nano-particle for bio-imaging, with NH3·H2O and
NH4HCO3For precipitating reagent and ZnSO4It reacts, generates by ZnCO3The Zn (OH) of package2Precursor needs during reaction
It is stirred, mixing speed 200-500r/min, preferably 200-400r/min.Its reaction equation are as follows: ZnSO4+2NH3·
H2O=Zn (OH)2↓+(NH4)2SO4, ZnSO4+NH4HCO3=ZnCO3↓+(NH4)2SO4；Wherein, ZnSO4For Zinc sulphate, consumption proportion
Match 25-35mlNH for the Zinc sulphate of 5-10g3·H2O and NH4HCO3, the Zinc sulphate that preferable amount proportion is 5-8g is with 28-35mlNH3·
H2O and NH4HCO3Or the Zinc sulphate that consumption proportion is 5-6g matches 28-32mlNH3·H2O and NH4HCO3Or consumption proportion is 5g's
Zinc sulphate matches 30mlNH3·H2O and NH4HCO3。NH3·H2O and NH4HCO3Arbitrarily to match, preferred mass ratio is 1:1.By generation
Presoma filters out, and roasts after being washed, and maturing temperature is 100 DEG C, calcining time 70-80min, preferably 70-75min.
After roasting, presoma is calcined, reaction equation are as follows: Zn (OH)2=ZnO+H2O；ZnCO3=ZnO+CO2.Calcining temperature
Degree is 300-400 DEG C, preferably 400 DEG C.Calcination time is 2-4h, preferably 3h.NH3·H2O and NH4HCO3It is pure chemicals, it will
Its aqueous solution for being configured to 0.5mol/L.
As shown in Fig. 2, Zinc sulphate is divided into the several groups of 5g, 10g, 15g, 20g, zinc oxide is prepared as variable using precipitating reagent
Nanoparticle.First group by 5g Zinc sulphate respectively slowly be added 10ml and 20ml the 0.5mol/L being configured to precipitating reagent water
It in solution and is stirred, gained sediment is filtered, roast, is calcined, zinc oxide nano-powder is finally obtained；Second group
10g Zinc sulphate is slowly added respectively in the aqueous solution for the 0.5mol/L of 20ml, 40ml and 60ml being configured to precipitating reagent simultaneously
It is stirred, gained sediment is filtered, roast, is calcined, zinc oxide nano-powder is finally obtained；Third group is white by 15g
Alum is slowly added in the aqueous solution for the 0.5mol/L of 40ml, 80ml and 100ml being configured to precipitating reagent respectively and is stirred
It mixes, gained sediment is filtered, roast, is calcined, zinc oxide nano-powder is finally obtained；4th group is distinguished 20g Zinc sulphate
It is slowly added in the aqueous solution for the 0.5mol/L of 80ml, 100ml and 120ml being configured to precipitating reagent and is stirred, it will
Gained sediment is filtered, roasts, calcines, and finally obtains zinc oxide nano-powder.
As shown in figure 3, changing reaction temperature to above-mentioned group, first group of reaction temperature is room temperature；Second group is placed in constant temperature
In water-bath, temperature is 50 DEG C；Third group is placed in thermostat water bath, and temperature is 60 DEG C；4th group is placed in thermostat water bath,
Temperature is 70 DEG C；Reaction time is 15min.Band is filtered after completion of the reaction, roasts, is calcined, and weighing obtains:
| Reaction temperature (DEG C) | Sediment granularity |
| Room temperature | It is larger |
| 50 | It is smaller |
| 60 | It is smaller |
| 70 | It is smaller |
Change mixing speed, each group acted on 0r/min, 200r/min, 400r/min respectively, is obtained:
| Mixing speed (r/min) | Reaction rate | Granularity |
| 0 | Generally | It is larger |
| 200 | It is larger | It is smaller |
| 400 | It is larger | It is smaller |
Change calcining time, each group is acted on 30min, 50min, 70min, 90min respectively, sediment is with roasting
The variation of time and change, obtain shortest calcining time, as shown in Figure 4.
Change calcination time, calcination temperature remains 400 DEG C, acts on each group respectively with 1h, 2h, 3h, 4h, obtain
Best calcination time, as shown in Figure 5.
The state modulator that the present invention passes through this method is not in too big agglomeration, more balanced, the production improved
Rate and quality.It is easier to reunite because the probability of particle encounter increases, therefore the Zinc sulphate that consumption proportion is 5g is matched
30mlNH3·H2O and NH4HCO3It for optimal components ratio, i.e., less will appear reunion, and can ensure yield.It is anti-as the temperature increases
Rate is answered to accelerate, the chance of molecular collision increases, and reunion probability increases.Since ammonium hydroxide is in aqueous solution with NH4 +And OH-Form
In the presence of simultaneously because NH4 +Hydrolysis be the endothermic reaction, as the temperature increases, NH4 +And OH-Ion is reduced, so leading to Zn
(OH)2It reduces, ZnCO3Increase, breaks their equilibrium, so that ZnCO3It is easy to happen reunion, so preferably reaction temperature is
Room temperature.With the increase of mixing speed, the appearance of reunion will be reduced, and mixing speed is excessive is easy for vortex occur, be easy
It splashes out, it is unfavorable to reacting, so the preferable speed of stirring is 200r/min.Roasting is to evaporate the hydrone in sediment all
Out, there is certain relationship with temperature to this time, be 70min with 100 DEG C of preferable calcining time.Calcining is to make presoma point
For solution close to completely, calcination temperature has certain relationship with the time, is 3h with 400 DEG C of preferable calcination time.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (9)
1. a kind of preparation method of the zinc oxide nano-particle for bio-imaging, it is characterised in that: with NH3·H2O and NH4HCO3
For precipitating reagent and ZnSO4It reacts, generates by ZnCO3The Zn (OH) of package2Precursor needs to be stirred during reaction
It mixes, mixing speed 200-500r/min, reaction equation are as follows: ZnSO4+2NH3·H2O=Zn (OH)2↓+(NH4)2SO4,
ZnSO4+NH4HCO3=ZnCO3↓+(NH4)2SO4；Wherein, ZnSO4For Zinc sulphate, the Zinc sulphate that consumption proportion is 5-10g matches 25-
35mlNH3·H2O and NH4HCO3, NH3·H2O and NH4HCO3Arbitrarily to match；
The presoma of generation is filtered out, is roasted after being washed, maturing temperature is 100 DEG C, calcining time 70-80min；
After roasting, presoma is calcined, reaction equation are as follows: Zn (OH)2=ZnO+H2O；ZnCO3=ZnO+CO2；Calcining
Temperature is 300-400 DEG C, calcination time 2-4h.
2. the preparation method of the zinc oxide nano-particle according to claim 1 for bio-imaging, it is characterised in that: institute
State NH3·H2O and NH4HCO3It is pure chemicals, is configured to the aqueous solution of 0.5mol/L.
3. the preparation method of the zinc oxide nano-particle according to claim 1 for bio-imaging, it is characterised in that: use
The Zinc sulphate that amount proportion is 5-8g matches 28-35mlNH3·H2O and NH4HCO3。
4. the preparation method of the zinc oxide nano-particle according to claim 3 for bio-imaging, it is characterised in that: use
The Zinc sulphate that amount proportion is 5-6g matches 28-32mlNH3·H2O and NH4HCO3。
5. the preparation method of the zinc oxide nano-particle according to claim 4 for bio-imaging, it is characterised in that: use
The Zinc sulphate that amount proportion is 5g matches 30mlNH3·H2O and NH4HCO3。
6. the preparation method of the zinc oxide nano-particle according to claim 2 for bio-imaging, it is characterised in that:
NH3·H2O and NH4HCO3Proportion be mass ratio 1:1.
7. the preparation method of the zinc oxide nano-particle according to claim 1 for bio-imaging, it is characterised in that: stir
Mixing speed is 200-400r/min.
8. the preparation method of the zinc oxide nano-particle according to claim 1 for bio-imaging, it is characterised in that: roasting
The burning time is 70-75min.
9. the preparation method of the zinc oxide nano-particle according to claim 1 for bio-imaging, it is characterised in that: forge
Burning temperature is 400 DEG C, calcination time 2h.
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| CN1415545A (en) * | 2001-11-01 | 2003-05-07 | 北京化工大学 | Method for preparing nano zinc oxide |
| WO2004028972A1 (en) * | 2002-09-25 | 2004-04-08 | Societe Industrielle Liegeoise Des Oxydes Sa | Zinc oxide in the form of an improved flow powder, method for the production and use thereof in polymers |
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| CN102627313A (en) * | 2012-04-12 | 2012-08-08 | 广汉隆达饲料有限公司 | Wet production process for feed-grade active zinc oxide |
| US20150246822A1 (en) * | 2012-09-25 | 2015-09-03 | Sichuan Xinhong Technology Co., Ltd. | Method for Producing a High-purity Nanometer Zinc Oxide from Electrolytic Zinc Acid Leaching Residues by Ammonia Decarburization |
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| CN1415545A (en) * | 2001-11-01 | 2003-05-07 | 北京化工大学 | Method for preparing nano zinc oxide |
| CN1396117A (en) * | 2002-06-13 | 2003-02-12 | 山东小鸭集团有限责任公司 | Process for preparing nano zinc oxide |
| WO2004028972A1 (en) * | 2002-09-25 | 2004-04-08 | Societe Industrielle Liegeoise Des Oxydes Sa | Zinc oxide in the form of an improved flow powder, method for the production and use thereof in polymers |
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| US20150246822A1 (en) * | 2012-09-25 | 2015-09-03 | Sichuan Xinhong Technology Co., Ltd. | Method for Producing a High-purity Nanometer Zinc Oxide from Electrolytic Zinc Acid Leaching Residues by Ammonia Decarburization |
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