CN102659171A - Preparation method of water-soluble zinc oxide nanoparticles - Google Patents

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

A kind of water soluble oxidized zinc nanometer particle process method

Technical field

Technical field is nano material, technical field of biological material under the present invention, particularly is applied to a kind of water soluble oxidized zinc nanometer particle process method of biological field.

Background technology

The nano zine oxide chemical property is stable, low toxicity; Has excellent biological compatibility; Biomolecules there is very strong avidity; Can get into viable cell, and have fluorescent effect and photo-catalysis function, through can be used for application such as oncotherapy, gene and pharmaceutical carrier, fluorescence imaging and cell marking after finishing and the functionalization.

Nano-ZnO preparation is more, mainly contains 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 with alcoholic solvent hydrolysis synthetic zinc oxide nano-particle percent crystallinity, dispersion stabilization is poor in the aqueous solution, is prone to reunite.And some other synthetic zinc oxide nano-particle in oil-dissolving solvent can't be dispersed in the aqueous solution, thereby can't directly apply in the organism.

Summary of the invention

The object of the present invention is to provide a kind of water soluble oxidized zinc nanometer particle process method.

Concrete steps are following:

(1) 0.44 ~ 1.2 gram zinc salt and 0 ~ 1.2 gram modifier are dissolved in 25 ~ 35 gram organic solvents, are made into clear solution through stirring;

(2) solution that step (1) is made is poured there-necked flask into, feeds nitrogen or argon gas as protection gas, and gas flow is 100 ~ 500 ml/min, heat temperature raising to 200 ~ 320 ℃ 0.5 ~ 2 hour postcooling of insulation; Reaction soln is obtained zinc oxide 5000 ~ 15000 rev/mins of spinnings; Gained zinc oxide is monodisperse particles shape nanoparticle, and mean particle size is 5 ~ 80 nanometers, or the nanocluster that flocks together for a plurality of small-particles, and mean particle size is 30 ~ 200 nanometers;

Said zinc salt is a kind of in zinc acetylacetonate, zinc acetate and the Zinic stearas;

Said organic solvent is polyoxyethylene glycol or triglycol;

Said modifier is a kind of in Vinylpyrrolidone polymer, polymine and the Zinic stearas.

The present invention prepares zinc oxide nano-particle in water-soluble and biocompatible solvent, dispersion stabilization is good in the aqueous solution, and prepared zinc oxide nano-particle has water-soluble, can be applicable to biomedical sector.

Description of drawings

The transmission electron microscope photo of the zinc oxide that Fig. 1 makes for the embodiment of the invention 1.

The transmission electron microscope photo of the zinc oxide that Fig. 2 makes for the embodiment of the invention 2.

The transmission electron microscope photo of the zinc oxide that Fig. 3 makes for the embodiment of the invention 3.

The transmission electron microscope photo of the zinc oxide that Fig. 4 makes for the embodiment of the invention 4.

Embodiment

Embodiment 1:

(1) 0.44 gram zinc acetate and 1 gram Vinylpyrrolidone polymer are dissolved in the 30 gram polyoxyethylene glycol, are made into clear solution through stirring;

(2) solution that step (1) is made is poured there-necked flask into, feeds nitrogen as protection gas, and gas flow is 100 ml/min, heat temperature raising to 260 ℃ 0.5 hour postcooling of insulation; Reaction soln is obtained zinc oxide 10000 rev/mins of spinnings; 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 the 30 gram polyoxyethylene glycol, are made into clear solution through stirring;

(2) solution that step (1) is made is poured there-necked flask into, feeds nitrogen as protection gas, and gas flow is 200 ml/min, heat temperature raising to 280 ℃ 1 hour postcooling of insulation; Reaction soln is obtained zinc oxide 8000 rev/mins of spinnings; 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 is dissolved in the 30 gram triglycols, is made into clear solution through stirring;

(2) solution that step (1) is made is poured there-necked flask into, feeds nitrogen as protection gas, and gas flow is 300 ml/min, heat temperature raising to 200 ℃ 1.5 hours postcooling of insulation; Reaction soln is obtained zinc oxide 8000 rev/mins of spinnings; Gained zinc oxide is group's bunch average particle size 60 nanometers, is to be reunited by 20 nanometer left and right sides small-particles with forming, and sees Fig. 3.

Embodiment 4:

(1) 0.7 gram zinc acetylacetonate is dissolved in the 30 gram triglycols, is made into clear solution through stirring;

(2) solution that step (1) is made is poured there-necked flask into, feeds nitrogen as protection gas, and gas flow is 200 ml/min, heat temperature raising to 280 ℃ 1 hour postcooling of insulation; Reaction soln is obtained zinc oxide 8000 rev/mins of spinnings; Gained zinc oxide is group's bunch particle, and mean particle size 80 nanometers are to be reunited by 20 nanometer left and right sides small-particles with forming, and see Fig. 4.

Claims (1)

1. water soluble oxidized zinc nanometer particle process method is characterized in that concrete steps are following:

(1) 0.44 ~ 1.2 gram zinc salt and 0 ~ 1.2 gram modifier are dissolved in 25 ~ 35 gram organic solvents, are made into clear solution through stirring;

(2) solution that step (1) is made is poured there-necked flask into, feeds nitrogen or argon gas as protection gas, and gas flow is 100 ~ 500 ml/min, heat temperature raising to 200 ~ 320 ℃ 0.5 ~ 2 hour postcooling of insulation; Reaction soln is obtained zinc oxide 5000 ~ 15000 rev/mins of spinnings; Gained zinc oxide is monodisperse particles shape nanoparticle, and mean particle size is 5 ~ 80 nanometers, or the nanocluster that flocks together for a plurality of small-particles, and mean particle size is 30 ~ 200 nanometers;

Said zinc salt is a kind of in zinc acetylacetonate, zinc acetate and the Zinic stearas;

Said organic solvent is polyoxyethylene glycol or triglycol;

Said modifier is a kind of in Vinylpyrrolidone polymer, the polymine.

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