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 PDF

Info

Publication number
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
Authority
CN
China
Prior art keywords
hco
zinc oxide
calcination
znso
oxide nanoparticles
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201910016945.5A
Other languages
Chinese (zh)
Inventor
郑志勤
易发成
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Southwest University of Science and Technology
Original Assignee
Southwest University of Science and Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Southwest University of Science and Technology filed Critical Southwest University of Science and Technology
Priority to CN201910016945.5A priority Critical patent/CN109850933A/en
Publication of CN109850933A publication Critical patent/CN109850933A/en
Pending legal-status Critical Current

Links

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

A kind of preparation method of the zinc oxide nano-particle for bio-imaging
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)

1.一种用于生物成像的氧化锌纳米粒子的制备方法,其特征在于: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,其反应方程式为:ZnSO4+2NH3·H2O=Zn(OH)2↓+(NH4)2SO4,ZnSO4+NH4HCO3=ZnCO3↓+(NH4)2SO4;其中,ZnSO4为皓矾,用量配比为5-10g的皓矾配25-35mlNH3·H2O和NH4HCO3,NH3·H2O和NH4HCO3为任意配比;1. a preparation method of the zinc oxide nanoparticle for bioimaging , is characterized in that: take NH 3 H 2 O and NH 4 HCO 3 as precipitating agent and ZnSO 4 react with ZnSO , generate Zn( OH) 2 precursor, needs to be stirred during the reaction, the stirring speed is 200-500r/min, and its reaction equation is: ZnSO 4 +2NH 3 ·H 2 O=Zn(OH) 2 ↓+(NH 4 ) 2 SO 4 , ZnSO 4 +NH 4 HCO 3 =ZnCO 3 ↓+(NH 4 ) 2 SO 4 ; wherein, ZnSO 4 is alum, and the dosage ratio is 5-10g of alum with 25-35ml NH 3 ·H 2 O and NH 4 HCO 3 , NH 3 ·H 2 O and NH 4 HCO 3 are in any ratio; 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;The generated precursor is filtered out, washed and calcined, the calcination temperature is 100°C, and the calcination time is 70-80min; 焙烧后,对前驱体进行煅烧,其反应方程式为:Zn(OH)2=ZnO+H2O;ZnCO3=ZnO+CO2;煅烧温度为300-400℃,煅烧时间为2-4h。After calcination, the precursor is calcined, and the reaction equation is: Zn(OH) 2 =ZnO+H 2 O; ZnCO 3 =ZnO+CO 2 ; the calcination temperature is 300-400°C, and the calcination time is 2-4h. 2.根据权利要求1所述的用于生物成像的氧化锌纳米粒子的制备方法,其特征在于:所述NH3·H2O和NH4HCO3是纯的化学品,将其配置成0.5mol/L的水溶液。2 . The method for preparing zinc oxide nanoparticles for bioimaging according to claim 1 , wherein the NH 3 ·H 2 O and NH 4 HCO 3 are pure chemicals, which are configured to be 0.5 mol/L aqueous solution. 3.根据权利要求1所述的用于生物成像的氧化锌纳米粒子的制备方法,其特征在于:用量配比为5-8g的皓矾配28-35mlNH3·H2O和NH4HCO33. The method for preparing zinc oxide nanoparticles for bioimaging according to claim 1, characterized in that: the dosage ratio is that 5-8g of alum is mixed with 28-35ml NH 3 H 2 O and NH 4 HCO 3 . 4.根据权利要求3所述的用于生物成像的氧化锌纳米粒子的制备方法,其特征在于:用量配比为5-6g的皓矾配28-32mlNH3·H2O和NH4HCO34. The method for preparing zinc oxide nanoparticles for bioimaging according to claim 3, characterized in that: the dosage ratio is that 5-6g of alum is mixed with 28-32ml NH 3 H 2 O and NH 4 HCO 3 . 5.根据权利要求4所述的用于生物成像的氧化锌纳米粒子的制备方法,其特征在于:用量配比为5g的皓矾配30mlNH3·H2O和NH4HCO35 . The method for preparing zinc oxide nanoparticles for bioimaging according to claim 4 , wherein the dosage ratio is 5 g of alum with 30 ml of NH 3 ·H 2 O and NH 4 HCO 3 . 6 . 6.根据权利要求2所述的用于生物成像的氧化锌纳米粒子的制备方法,其特征在于:NH3·H2O和NH4HCO3的配比为质量比1:1。6 . The method for preparing zinc oxide nanoparticles for bioimaging according to claim 2 , wherein the ratio of NH 3 ·H 2 O to NH 4 HCO 3 is 1:1 by mass. 7 . 7.根据权利要求1所述的用于生物成像的氧化锌纳米粒子的制备方法,其特征在于:搅拌速度为200-400r/min。7 . The method for preparing zinc oxide nanoparticles for bioimaging according to claim 1 , wherein the stirring speed is 200-400 r/min. 8 . 8.根据权利要求1所述的用于生物成像的氧化锌纳米粒子的制备方法,其特征在于:焙烧时间为70-75min。8 . The method for preparing zinc oxide nanoparticles for bioimaging according to claim 1 , wherein the calcination time is 70-75 min. 9 . 9.根据权利要求1所述的用于生物成像的氧化锌纳米粒子的制备方法,其特征在于:煅烧温度为400℃,煅烧时间为2h。9 . The method for preparing zinc oxide nanoparticles for bioimaging according to claim 1 , wherein the calcination temperature is 400° C. and the calcination time is 2 hours. 10 .
CN201910016945.5A 2019-01-08 2019-01-08 A kind of preparation method of the zinc oxide nano-particle for bio-imaging Pending CN109850933A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201910016945.5A CN109850933A (en) 2019-01-08 2019-01-08 A kind of preparation method of the zinc oxide nano-particle for bio-imaging

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201910016945.5A CN109850933A (en) 2019-01-08 2019-01-08 A kind of preparation method of the zinc oxide nano-particle for bio-imaging

Publications (1)

Publication Number Publication Date
CN109850933A true CN109850933A (en) 2019-06-07

Family

ID=66894183

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201910016945.5A Pending CN109850933A (en) 2019-01-08 2019-01-08 A kind of preparation method of the zinc oxide nano-particle for bio-imaging

Country Status (1)

Country Link
CN (1) CN109850933A (en)

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN106064827A (en) * 2016-07-29 2016-11-02 柳州豪祥特科技有限公司 A kind of preparation method of nanometer Zinc oxide powder

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1415545A (en) * 2001-11-01 2003-05-07 北京化工大学 A kind of preparation method of nano-sized 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
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
CN106064827A (en) * 2016-07-29 2016-11-02 柳州豪祥特科技有限公司 A kind of preparation method of nanometer Zinc oxide powder

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
王润申 等: "分步沉淀法制备氧化锌超细粉体的工艺研究", 《四川有色金属》 *
赵燕禹 等: "碳铵法制备纳米氧化锌的研究", 《无机盐工业》 *

Similar Documents

Publication Publication Date Title
CN102515252B (en) Film-coating production technology for nano zinc oxide
JP2002255515A (en) Method for producing metal oxide fine particles
CN101372353A (en) Method for preparing nano CeO2 power by ultrasonic atomization process
WO2016065950A1 (en) Method for preparing basic zinc chloride
CN100494069C (en) A kind of preparation method of nano zinc oxide
CN103553116A (en) Nanometer zinc oxide particle preparation method
CN114308073B (en) Preparation method and application of composite catalyst
CN104209126B (en) A kind of preparation method of pencil prism cobaltosic oxide
CN101070192A (en) Method for synthesizing spinel structure magnesium frrite nano particles
CN103191783B (en) Zinc sulfide-benzoic acid nano composite photocatalytic material and preparation method thereof
CN103641147B (en) A kind of preparation method of micron-order ellipsoidal cerium oxide
CN103193472A (en) Method for synthesizing subsphaeroidal barium ferrite superfine powder by using ultrasound-assisted coprecipitation method
CN113184908B (en) Rapid synthesis method of molybdenum oxide nanowire
KR101108691B1 (en) Method for preparing nano zinc oxide powder by hydrothermal synthesis
CN101905870B (en) A method for continuously preparing nanoscale anionic layered materials
CN109850933A (en) A kind of preparation method of the zinc oxide nano-particle for bio-imaging
CN106995218B (en) Brick-shaped monoclinic phase WO3Preparation method of (1)
CN1192991A (en) A new method for preparing nanoscale zinc oxide
CN103910377B (en) A kind of improvement plant film S type nano zine oxide production technique
CN113735172A (en) Method for preparing fine-particle chromium hydroxide from chromium-containing sludge
CN104528814A (en) A kind of preparation method and product of layered structure CaTi2O4(OH)4rhombic nanosheets
CN106986371A (en) A kind of method for preparing nanometer Zinc oxide powder
Balamurugan et al. Comparison of the synthesis of s, p, d, and f block simple oxides of MgO, SnO2, NiO, and CeO2 nanostructured materials
CN104986799A (en) A kind of co-precipitation method for synthesizing Gd2Hf2O7 nanopowder
CN101570478B (en) Spherical cobalt oxalate powder and production method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20190607