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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- hco
- zinc oxide
- calcination
- znso
- oxide nanoparticles
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 28
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 238000003384 imaging method Methods 0.000 title description 8
- 238000001354 calcination Methods 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- 239000011701 zinc Substances 0.000 claims abstract description 11
- 229940037003 alum Drugs 0.000 claims abstract description 8
- 239000002243 precursor Substances 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 230000001376 precipitating effect Effects 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 238000005054 agglomeration Methods 0.000 abstract description 3
- 230000002776 aggregation Effects 0.000 abstract description 3
- 238000012984 biological imaging Methods 0.000 abstract 2
- 238000005406 washing Methods 0.000 abstract 1
- 239000011686 zinc sulphate Substances 0.000 description 24
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 20
- 235000009529 zinc sulphate Nutrition 0.000 description 16
- 239000013049 sediment Substances 0.000 description 11
- 239000011667 zinc carbonate Substances 0.000 description 8
- 229910000010 zinc carbonate Inorganic materials 0.000 description 8
- 229910000368 zinc sulfate Inorganic materials 0.000 description 8
- 239000003153 chemical reaction reagent Substances 0.000 description 7
- 238000002156 mixing Methods 0.000 description 6
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 4
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 4
- ONIOAEVPMYCHKX-UHFFFAOYSA-N carbonic acid;zinc Chemical compound [Zn].OC(O)=O ONIOAEVPMYCHKX-UHFFFAOYSA-N 0.000 description 4
- 239000007791 liquid phase Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000000053 physical method Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 230000000873 masking effect Effects 0.000 description 1
- 238000010297 mechanical methods and process Methods 0.000 description 1
- 230000001617 migratory effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 239000002985 plastic film Substances 0.000 description 1
- 229920006255 plastic film Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
本发明公开了一种用于生物成像的氧化锌纳米粒子的制备方法，以NH3·H2O和NH4HCO3为沉淀剂与ZnSO4发生反应，生成由ZnCO3包裹的Zn(OH)2前躯体，在反应的过程中需进行搅拌，搅拌速度为200‑500r/min；其中，ZnSO4为皓矾，用量配比为5‑10g的皓矾配25‑35mlNH3·H2O和NH4HCO3；将生成的前驱体过滤出，进行洗涤后焙烧，焙烧温度为100℃，焙烧时间为70‑80min；焙烧后，对前驱体进行煅烧；煅烧温度为300‑400℃，煅烧时间为2‑4h。本发明通过本方法的参数控制不会出现太大的团聚现象，比较均衡，提升了的产率和品质，适用于生物成像。
The invention discloses a preparation method of zinc oxide nanoparticles for biological imaging. NH 3 ·H 2 O and NH 4 HCO 3 are used as precipitants to react with ZnSO 4 to generate Zn(OH) wrapped by ZnCO 3 2 precursors need to be stirred in the process of reaction, and the stirring speed is 200-500r /min; Wherein, ZnSO is alum, and the consumption ratio is that the alum of 5-10g is equipped with 25-35mlNH 3 ·H 2 O and NH 4 HCO 3 ; filter out the generated precursor, and calcine after washing, the calcination temperature is 100°C, and the calcination time is 70-80min; after calcination, the precursor is calcined; the calcination temperature is 300-400°C, and the calcination time is 300-400°C is 2‑4h. Through the parameter control of the method, the present invention does not appear too large agglomeration phenomenon, is relatively balanced, improves the yield and quality, and is suitable for biological 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)
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| 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 |
| CN1415545A (en) * | 2001-11-01 | 2003-05-07 | 北京化工大学 | A kind of preparation method of nano-sized 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 |
| CN1927722A (en) * | 2006-06-21 | 2007-03-14 | 兰州理工大学 | Preparation method for nanometer zinc oxide |
| 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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2019
- 2019-01-08 CN CN201910016945.5A patent/CN109850933A/en active Pending
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|---|---|---|---|---|
| CN1415545A (en) * | 2001-11-01 | 2003-05-07 | 北京化工大学 | A kind of preparation method of nano-sized zinc oxide |
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Application publication date: 20190607 |