CN103894191B - A kind of layering Ag@TiO 2the preparation method of Core-shell Structure Nanoparticles - Google Patents

Abstract

The invention discloses a kind of layering Ag@TiO ₂the preparation method of Core-shell Structure Nanoparticles, layering Ag@TiO of the present invention ₂core-shell Structure Nanoparticles structure is unique, specific area is high, the fields such as medicament slow release, photocatalysis, sterilization processing or cell marking can be widely used in, and it is higher at water treatment field effect, its photocatalytic activity is high, load metallic atom, enhances the hydrophobicity on surface, makes the catabolite of attachment be easy to cleaning.

Description

A kind of layering Ag@TiO 2the preparation method of Core-shell Structure Nanoparticles

Technical field

The present invention relates generally to field of nano material preparation, particularly relates to a kind of layering Ag@TiO ₂the preparation method of Core-shell Structure Nanoparticles.

Background technology

Photocatalysis technology can utilize solar energy degradation of organic substances, non-secondary pollution, and reaction condition is gentle, has " energy " and " environmental protection " dual significance.TiO ₂as a kind of semiconductor light-catalyst, because it has oxidability by force, the advantages such as physicochemical properties are stablized, nontoxic, cheap, are in the core status of research always in depollution of environment field.But TiO ₂because it can only utilize ultraviolet light, this is on the low side in Solar use aspect efficiency to cause material, and the easy compound of photo-generate electron-hole, be its key in actual applications of restriction, how make photochemical catalyst effectively utilize solar energy and improve electron-hole separative efficiency to improve the emphasis that photocatalytic activity is research always.

Summary of the invention

The object of the invention is just to provide a kind of layering Ag TiO ₂the preparation method of Core-shell Structure Nanoparticles.

The present invention is achieved by the following technical solutions:

A kind of Ag@TiO ₂the preparation method of Core-shell Structure Nanoparticles, is characterized in that comprising the following steps:

(1) synthesis of Ag nano particle:

1, join in the ethylene glycol of 10ml by the PVP of 0.050g, stir, until PVP dissolves completely, solution is transparent;

2, by the AgNO of 0.0255g ₃be dissolved in the ethylene glycol of 5ml, stir, until solution mixes;

3, kind of the solution mixing of two after above-mentioned process is proceeded in the polytetrafluoroethylene (PTFE) autoclave inner bag of 50ml, stir 50-70 minute, autoclave is put into air dry oven and be incubated 180 DEG C, time 2 h;

4, product through clean centrifugal after, obtain Ag nano particle, be made into the water dispersion solution of 0.01M Ag, ultrasonic, make it be uniformly dispersed, for subsequent use;

(2) layering nucleocapsid structure preparation:

1,0.05ml butyl titanate is added in the ethylene glycol of 10ml, magnetic agitation 8h, be labeled as solution A;

2, the aqueous dispersions of the above-mentioned 0.01M Ag of 3ml is added in 10ml acetone, stir 5min, be labeled as solution B;

3,0.5ml solution A is joined solution B, leave standstill 1h, occur after brown color sediment through collected by centrifugation;

4, brown color sediment obtained above is distributed in the mixed solvent of 30ml butylamine and ethanol, described butylamine and the concentration ratio of ethanol are 1:1, stir 10min, add 0.1ml butyl titanate, magnetic agitation 1 hour, proceed in 50ml polytetrafluoroethylene (PTFE) autoclave inner bag, 180 DEG C are incubated 12 hours;

5, product is through cleaning collected by centrifugation, at 60 DEG C of drying one nights, obtains described Ag@TiO ₂core-shell Structure Nanoparticles.

Advantage of the present invention is:

Ag@TiO of the present invention ₂core-shell Structure Nanoparticles structure is unique, specific area is high, the fields such as medicament slow release, photocatalysis, sterilization processing or cell marking can be widely used in, and it is higher at water treatment field effect, its photocatalytic activity is high, load metallic atom, enhances the hydrophobicity on surface, makes the catabolite of attachment be easy to cleaning.

Accompanying drawing explanation

Fig. 1 is layering Ag@TiO of the present invention ₂the SEM figure of Core-shell Structure Nanoparticles;

Fig. 2 is layering Ag@TiO of the present invention ₂the TEM figure of Core-shell Structure Nanoparticles;

Fig. 3 is layering Ag@TiO of the present invention ₂the XPS spectrum figure of Core-shell Structure Nanoparticles, abscissa combines energy, and ordinate is relative intensity;

Fig. 4 is layering Ag@TiO of the present invention ₂core-shell Structure Nanoparticles and titanium dioxide P25 are under visible light to the degradation effect comparison diagram of methyl orange.

Detailed description of the invention

Embodiment 1

A kind of Ag@TiO ₂the preparation method of Core-shell Structure Nanoparticles, is characterized in that comprising the following steps:

(1) synthesis of Ag nano particle:

1, join in the ethylene glycol of 10ml by the PVP of 0.050g, stir, until PVP dissolves completely, solution is transparent;

2, by the AgNO of 0.0255g ₃be dissolved in the ethylene glycol of 5ml, stir, until solution mixes;

3, kind of the solution mixing of two after above-mentioned process is proceeded in the polytetrafluoroethylene (PTFE) autoclave inner bag of 50ml, stir 60 minutes, autoclave is put into air dry oven and be incubated 180 DEG C, time 2 h;

4, product through clean centrifugal after, obtain Ag nano particle, be made into the water dispersion solution of 0.01M Ag, ultrasonic, make it be uniformly dispersed, for subsequent use;

(2) layering nucleocapsid structure preparation:

1,0.05ml butyl titanate is added in the ethylene glycol of 10ml, magnetic agitation 8h, be labeled as solution A;

2, the aqueous dispersions of the above-mentioned 0.01M Ag of 3ml is added in 10ml acetone, stir 5min, be labeled as solution B;

3,0.5ml solution A is joined solution B, leave standstill 1h, occur after brown color sediment through collected by centrifugation;

4, brown color sediment obtained above is distributed in the mixed solvent of 30ml butylamine and ethanol, described butylamine and the concentration ratio of ethanol are 1:1, stir 10min, add 0.1ml butyl titanate, magnetic agitation 1 hour, proceed in 50ml polytetrafluoroethylene (PTFE) autoclave inner bag, 180 DEG C are incubated 12 hours;

5, product is through cleaning collected by centrifugation, at 60 DEG C of drying one nights, obtains described layering Ag@TiO ₂core-shell Structure Nanoparticles.

Experiment material and method:

By contrasting titanium dioxide P25 and Ag@TiO respectively ₂the degradation rate of Core-shell Structure Nanoparticles to Methyl Orange in Wastewater studies Ag@TiO ₂core-shell Structure Nanoparticles is to TiO ₂the impact of photocatalysis performance.

Reaction uses 350W high-pressure sodium lamp as light source, apart from liquid level 10cm, the methyl orange solution that 50ml concentration is 15mg/L put into by 0.04g photocatalysis sample, mixed liquor constantly stirs, 3ml solution is got every 20min, with the catalyst in 5000 revs/min of centrifuge removing solution, clear liquid ultraviolet-visual spectrometer test absorption maximum light rate judges its residual concentration.

Experimental result

Experimental result as shown in Figure 4, can be found out, compared to titanium dioxide P25, and layering Ag@TiO ₂core-shell Structure Nanoparticles significantly promotes for the degradation capability of methyl orange, confirms that it has good Photocatalytic Degradation Property.

Claims (1)

1. a layering Ag TiO ₂the preparation method of Core-shell Structure Nanoparticles, is characterized in that comprising the following steps:

(1) synthesis of Ag nano particle:

1, join in the ethylene glycol of 10ml by the PVP of 0.050g, stir, until PVP dissolves completely, solution is transparent;

2, by the AgNO of 0.0255g ₃be dissolved in the ethylene glycol of 5ml, stir, until solution mixes;

3, kind of the solution mixing of two after above-mentioned process is proceeded in the polytetrafluoroethylene (PTFE) autoclave of 50ml, stir 50-70 minute, autoclave is heated and is incubated at 180 DEG C, time 2 h;

4, product through clean centrifugal after, obtain Ag nano particle, be made into the water dispersion solution of 0.01M Ag, ultrasonic, make it be uniformly dispersed, for subsequent use;

(2) layering nucleocapsid structure preparation:

1,0.05ml butyl titanate is added in the ethylene glycol of 10ml, magnetic agitation 8h, be labeled as solution A;

2, the aqueous dispersions of the above-mentioned 0.01M Ag of 3ml is added in 10ml acetone, stir 5min, be labeled as solution B;

3,0.5ml solution A is joined solution B, leave standstill 1h, occur after brown color sediment through collected by centrifugation;

4, be distributed in the mixed solvent of 30ml butylamine and ethanol by brown color sediment obtained above, described butylamine and the concentration ratio of ethanol are 1:1, stir 10min, add 0.1ml butyl titanate, magnetic agitation 1 hour, proceeds in 50ml still, and 180 DEG C are incubated 12 hours;

5, product is through cleaning collected by centrifugation, at 60 DEG C of drying one nights, obtains described layering Ag@TiO ₂core-shell Structure Nanoparticles.