CN102659171B - Preparation method of water-soluble zinc oxide nanoparticles - Google Patents
Preparation method of water-soluble zinc oxide nanoparticles Download PDFInfo
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- CN102659171B CN102659171B CN201210149761.4A CN201210149761A CN102659171B CN 102659171 B CN102659171 B CN 102659171B CN 201210149761 A CN201210149761 A CN 201210149761A CN 102659171 B CN102659171 B CN 102659171B
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Abstract
The invention discloses a preparation method of water-soluble zinc oxide nanoparticles, which comprises the following steps: (1) dissolving 0.44-1.2g of zinc salt and 0-1.2g of modifier in 25-35g of organic solvent, and stirring to obtain a clear solution; and (2) pouring the solution prepared in the step (1) into a three-neck flask, introducing nitrogen or argon as a shielding gas, heating to 200-320 DEG C, keeping the temperature for 0.5-2 hours, cooling, and carrying out centrifugal separation to obtain the zinc oxide. The zinc oxide is monodisperse granular nanoparticles of which the average particle size is 5-80nm, or nanoclusters (of which the average particle size is 30-200nm) formed by multiple granules gathering together; the organic solvent is polyethyleneglycol or triglycol; and the modifier is polyvinylpyrrolidone, polyethyleneimine or zinc stearate. The zinc oxide nanoparticles are prepared in the water-soluble biocompatible solvent, and thus, have favorable dispersion stability in the water solution; and the prepared zinc oxide nanoparticles have water solubility, and can be applied to the field of biomedicine.
Description
Technical field
The technical field of the invention is nano material, technical field of biological material, particularly is applied to the preparation method of a kind of water soluble oxidized zinc nanoparticle of biological field.
Background technology
Nano zine oxide stable chemical nature, low toxicity, there is good biocompatibility, biomolecules is had to very strong avidity, can enter viable cell, and there is fluorescent effect and photo-catalysis function, by can be used for the application such as oncotherapy, gene and pharmaceutical carrier, fluorescence imaging and cell marking after finishing and functionalization.
The preparation method of nano zine oxide is more, mainly contains the methods such as physical vapor deposition, chemical vapour deposition, magnetron sputtering, sol-gel, spray pyrolysis, hydro-thermal, microemulsion.Wherein sol-gel method is the main method of preparation biologic applications nano zine oxide, but low by the zinc oxide nano-particle degree of crystallinity of alcoholic solvent hydrolysis, in the aqueous solution, dispersion stabilization is poor, easily reunites.And some other zinc oxide nano-particle synthetic in oil-dissolving solvent can't be dispersed in the aqueous solution, thereby can't directly apply in organism.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of water soluble oxidized zinc nanoparticle.
Concrete steps are as follows:
(1) 0.44 ~ 1.2 gram zinc salt and 0 ~ 1.2 gram modifier are dissolved in 25 ~ 35 gram organic solvents, through stirring, are made into clear solution;
(2) solution step (1) made is poured there-necked flask into, passes into nitrogen or argon gas as protection gas, and gas flow is 100 ~ 500 ml/min, is heated to 200 ~ 320 ℃ of insulations cooling after 0.5 ~ 2 hour; Reaction soln is obtained to zinc oxide 5000 ~ 15000 rev/mins of centrifugations; Gained zinc oxide is monodisperse particles shape nanoparticle, and mean particle size is 5 ~ 80 nanometers, or the nanocluster flocked together for a plurality of small-particles, and mean particle size is 30 ~ 200 nanometers;
Described zinc salt is a kind of in zinc acetylacetonate, zinc acetate and Zinic stearas;
Described organic solvent is polyoxyethylene glycol or triglycol;
Described modifier is a kind of in polyvinylpyrrolidone, polymine and Zinic stearas.
The present invention prepares zinc oxide nano-particle in water-soluble and biocompatible solvent, and in the aqueous solution, dispersion stabilization is good, and prepared zinc oxide nano-particle has water-soluble, can be applicable to biomedical sector.
The accompanying drawing explanation
The transmission electron microscope photo that Fig. 1 is the zinc oxide that makes of the embodiment of the present invention 1.
The transmission electron microscope photo that Fig. 2 is the zinc oxide that makes of the embodiment of the present invention 2.
The transmission electron microscope photo that Fig. 3 is the zinc oxide that makes of the embodiment of the present invention 3.
The transmission electron microscope photo that Fig. 4 is the zinc oxide that makes of the embodiment of the present invention 4.
Embodiment
Embodiment 1:
(1) 0.44 gram zinc acetate and 1 gram polyvinylpyrrolidone are dissolved in 30 gram polyoxyethylene glycol, through stirring, are made into clear solution;
(2) solution step (1) made is poured there-necked flask into, passes into nitrogen as protection gas, and gas flow is 100 ml/min, is heated to 260 ℃ of insulations cooling after 0.5 hour; Reaction soln is obtained to zinc oxide 10000 rev/mins of centrifugations; Gained zinc oxide is monodisperse particles shape nanoparticle, and mean particle size is 28 nanometers.
Embodiment 2:
(1) 0.7 gram zinc acetylacetonate and 0.8 gram polymine are dissolved in 30 gram polyoxyethylene glycol, through stirring, are made into clear solution;
(2) solution step (1) made is poured there-necked flask into, passes into nitrogen as protection gas, and gas flow is 200 ml/min, is heated to 280 ℃ of insulations cooling after 1 hour; Reaction soln is obtained to zinc oxide 8000 rev/mins of centrifugations; Gained zinc oxide is monodisperse particles shape nanoparticle, and mean particle size is 35 nanometers, sees Fig. 2.
Embodiment 3:
(1) 1.2 gram Zinic stearass are dissolved in 30 gram triglycols, through stirring, are made into clear solution;
(2) solution step (1) made is poured there-necked flask into, passes into nitrogen as protection gas, and gas flow is 300 ml/min, is heated to 200 ℃ of insulations cooling after 1.5 hours; Reaction soln is obtained to zinc oxide 8000 rev/mins of centrifugations; Gained zinc oxide is cluster average particle size 60 nanometers, is to be reunited and formed by 20 nanometer left and right small-particles, sees Fig. 3.
Embodiment 4:
(1) 0.7 gram zinc acetylacetonate is dissolved in 30 gram triglycols, through stirring, is made into clear solution;
(2) solution step (1) made is poured there-necked flask into, passes into nitrogen as protection gas, and gas flow is 200 ml/min, is heated to 280 ℃ of insulations cooling after 1 hour; Reaction soln is obtained to zinc oxide 8000 rev/mins of centrifugations; Gained zinc oxide is the cluster particle, and mean particle size 80 nanometers are to be reunited and formed by 20 nanometer left and right small-particles, see Fig. 4.
Claims (1)
1. the preparation method of a water soluble oxidized zinc nanoparticle is characterized in that concrete steps are as follows:
(1), by 0.44 ~ 1.2 gram zinc salt be greater than 0 and be less than or equal to 1.2 gram modifiers and be dissolved in 25 ~ 35 gram organic solvents, through stirring, being made into clear solution;
(2) solution step (1) made is poured there-necked flask into, passes into nitrogen or argon gas as protection gas, and gas flow is 100 ~ 500 ml/min, is heated to 200 ~ 320 ℃ of insulations cooling after 0.5 ~ 2 hour; Reaction soln is obtained to zinc oxide 5000 ~ 15000 rev/mins of centrifugations; Gained zinc oxide is monodisperse particles shape nanoparticle, and mean particle size is 5 ~ 80 nanometers;
Described zinc salt is a kind of in zinc acetylacetonate, zinc acetate and Zinic stearas;
Described organic solvent is polyoxyethylene glycol or triglycol;
Described modifier is a kind of in polyvinylpyrrolidone, polymine.
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| CN201210149761.4A CN102659171B (en) | 2012-05-15 | 2012-05-15 | Preparation method of water-soluble zinc oxide nanoparticles |
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| CN102659171B true CN102659171B (en) | 2014-01-08 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106006711A (en) * | 2016-07-07 | 2016-10-12 | 安徽省含山县锦华氧化锌厂 | Preparing method for nanometer zinc oxide |
| CN106986374B (en) * | 2017-05-08 | 2018-11-16 | 济南大学 | A kind of high specific surface area and mesoporous zinc-oxide nano cluster and preparation method thereof |
| CN108184898B (en) * | 2018-01-05 | 2019-06-21 | 烟台鲁量新材料科技有限公司 | A kind of preparation method of inorganic complex antimicrobials |
| CN112779073B (en) * | 2021-01-05 | 2022-01-11 | 中国科学院兰州化学物理研究所 | Prefabricated thickening agent containing nano zinc oxide and lubricating grease composition obtained by prefabricated thickening agent |
| CN112777626B (en) * | 2021-01-11 | 2022-04-12 | 大连理工大学 | Highly uniform zinc oxide submicron spheres with controllable particle size and preparation method thereof |
| CN115960367A (en) * | 2022-12-26 | 2023-04-14 | 浙江科曼奇生物科技股份有限公司 | Preparation method and application of quaternized polyethyleneimine zinc oxide or cuprous oxide particles |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1562762A (en) * | 2004-04-22 | 2005-01-12 | 上海交通大学 | Method for preparing nano zinc oxide in monodisperse, with no agglomeration and strong ultraviolet absorption |
| CN1935664A (en) * | 2006-09-30 | 2007-03-28 | 南京大学 | Method for preparing laminated structure submicron and micron ZnO particles |
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| JP2011148186A (en) * | 2010-01-21 | 2011-08-04 | Mitsubishi Plastics Inc | Laminated polyester film |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1562762A (en) * | 2004-04-22 | 2005-01-12 | 上海交通大学 | Method for preparing nano zinc oxide in monodisperse, with no agglomeration and strong ultraviolet absorption |
| CN1935664A (en) * | 2006-09-30 | 2007-03-28 | 南京大学 | Method for preparing laminated structure submicron and micron ZnO particles |
Non-Patent Citations (3)
| Title |
|---|
| JP特开2011-148186A 2011.08.04 |
| 室温下纳米氧化锌新相的合成及表征;杨青林等;《高等学校化学学报》;20030131;第82-85页 * |
| 杨青林等.室温下纳米氧化锌新相的合成及表征.《高等学校化学学报》.2003,第82-85页. |
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