CN102701266A - Preparation method for leaf-shaped silver chloride particle with micron structure - Google Patents

Abstract

The invention relates to the technical field of hydrothermal synthesis of photocatalytic materials, in particular to a preparation method for a leaf-shaped silver chloride particle with a micron structure. The preparation method for the leaf-shaped silver chloride particle with the micron structure comprises the following steps: through hydrothermal reduction, mixing EG solutions of AgNO3, FeCl3 and PVP, which contain concentrated HCl; performing reaction for a certain time, and then cooling the solution; extracting a sample through centrifugation, and finally obtaining the high-content and axially-symmetrical leaf-shaped AgCl particle with the micron structure. The preparation method for the leaf-shaped silver chloride particle with the micron structure is simple in step and easy and convenient to operate; a larger proportion of concentrated HCl is added, the product is in a form of AgCl crystals and people usually use an Ag elementary substance obtained from the reaction composition and the preparation method; the scanning electron microscopy shows that the structure of the AgCl crystal particle with the micron structure has an unified axially-symmetrical triangular leaf shape; and a performance test shows that the leaf-shaped silver chloride particle with the micron structure has a good performance for photocatalytically degrading organic contaminants.

Description

A kind of preparation method of leaf shape micrometer structure silver chloride particle

Technical field

The invention belongs to the method and technology field of the synthetic photocatalyst material of hydrothermal method, particularly a kind of preparation method of leaf shape micrometer structure silver chloride particle.

Background technology

Photochemical catalysis is having application potential very widely aspect the problems such as processing that solve the energy, environment and greenhouse gases, photocatalyst material can be realized functions such as photocatalytic hydrogen production by water decomposition, photodegradation organic pollutant and photoreduction carbonic acid gas.Traditional photocatalyst material is representative with titanium oxide, and the band gap of its broad makes it only can utilize the UV-light part that only accounts for sunshine 4%; In addition, therefore the very easily compound quantum yield that also reduced in light induced electron and hole needs exploitation can utilize the new and effective photocatalyst material of big wavelength region sunshine.Discover; With Silver monochloride (AgCl) is substrate, and the novel photocatalysis material of surface decoration Ag nanoparticle is because the tight contact between metal A g nanoparticle and the semi-conductor AgCl makes the electronic energy that is produced in the system be delivered on the metallic silver particles more easily; Promoted separating of light induced electron and hole; Guaranteed the stability of system, in addition, this novel photocatalysis material can also absorb the visible light part that occupies sunshine 48%.

As everyone knows, the micron or the nanostructure of material have remarkably influenced to its performance, and for the performance of catalysis, optics and the electricity aspect of improving AgCl, the AgCl particle of novel micron of research preparation or nanostructure also more and more receives people's concern.Yet; The AgCl grain pattern of having prepared at present only is confined to comparison dull cubes, chimb cubes, concave surface cubes and sphere; After the AgCl of these structures particle surface is decorated the Ag nanoparticle, all represented and be superior to the absorbing wavelength responding range of traditional titanic oxide material light.

Except the application in photocatalysis field, AgCl and other silver halide have been widely used in photographic material and the color-changing lens because of its photosensitivity, and its bacterinertness makes AgCl can be used for the preparation of sterilization conduit, bone cement and fabric web material again.The limitation of existing AgCl grain pattern also makes the preparation of high performance AgCl material receive restriction.

Summary of the invention

The present invention is directed to the deficiency of prior art, a kind of preparation method of leaf shape micrometer structure silver chloride particle is provided.

A kind of preparation method of leaf shape micrometer structure silver chloride particle is characterized in that: these method concrete steps are following:

(1) weighing reactant and solution: use electronic balance weighing FeCl ₃Solid and AgNO ₃Solid places respectively in two exsiccant beakers, and weighing PVP solid places FeCl is housed again ₃In the solid beaker, wherein PVP solid and AgNO ₃The solid mass ratio is PVP:AgNO ₃=(3:1) ~ (4:1), FeCl ₃Solid and AgNO ₃The solid mass ratio is FeCl ₃: AgNO ₃=1:10; Measure 1 part of dense HCl solution and two parts of EG solution respectively with graduated cylinder, two parts of EG solution are labeled as EG1 and EG2 respectively, and the volume ratio of wherein dense HCl solution, EG1 solution and EG2 solution is HCl:EG1:EG2=3:7:10, the AgNO of institute's weighing ₃The volume of employed dense HCl solution was 147 ml ~ 206 ml when solid was 1 g;

(2) proportioning mixing solutions: to FeCl is housed ₃With add EG2 solution in the beaker of PVP blended solid, after stirring with glass stick is rough, place and be stirred to FeCl on the magnetic stirring apparatus ₃Be dispersed in the EG2 solution with the PVP blended solid, this moment, solution was yellow; AgNO is equipped with in the adding of EG1 solution ₃In the solid beaker, after the rough stirring of glass stick, place and be stirred to AgNO on the magnetic stirring apparatus ₃Be dispersed among the EG1, this moment, solution was colourless transparent liquid; Under magnetic agitation, with water white AgNO ₃EG1 solution evenly splash into xanchromatic FeCl ₃In the EG2 mixing solutions of PVP, after stirring, add measured dense HCl solution, continue to stir this mixing solutions to mixing, this moment, solution was faint yellow;

(3) carry out hydrothermal synthesis reaction: the faint yellow mixing solutions of gained is poured in the hydrothermal reaction kettle that liner is a tetrafluoroethylene, put into loft drier, reaction 6 h ~ are 10 hours under 150 ℃ ~ 170 ℃ condition;

(4) abstraction reaction product A gCl: take out the hydrothermal reaction kettle in the loft drier; Be cooled to room temperature at normal temperatures; Open reaction kettle the solution in the liner is poured in the beaker, the solution in the beaker is poured in the centrifuge tube, put into whizzer; With ethanol centrifuge washing three times, finally obtain leaf shape micrometer structure silver chloride particle.

FeCl ₃, AgNO ₃, EG, dense HCl be analytical pure, PVP is a CP, Mw=30000.

Beneficial effect of the present invention is:

Step of the present invention is simple, and is easy and simple to handle, adopted stablizer PVP, strengthened AgCl micron particle stability of structure greatly, adds the Cl that dense HCl provides big concentration ^-, make that reaction product is the AgCl micron particle, rather than Ag micron or nanoparticle.The prepared leaf shape micrometer structure silver chloride particle that goes out has good photocatalysis performance.

Description of drawings

Fig. 1 is ESEM (SEM) figure of leaf shape micrometer structure silver chloride particle.

Fig. 2 contains leaf shape micrometer structure Silver monochloride, simple particulate state micrometer structure Silver monochloride and the photocatalytic degradation performance curve comparison diagram that does not contain the methyl orange solution of Silver monochloride.

Embodiment

The invention provides a kind of preparation method of leaf shape micrometer structure silver chloride particle, the present invention is further specified below in conjunction with accompanying drawing and embodiment.

Embodiment 1

With electronic balance difference weighing 0.0016 g FeCl ₃, 0.0170 g AgNO ₃In two exsiccant beakers, weighing 0.0670 g PVP places FeCl is housed again ₃Beaker in; Measure the dense HCl of a 3 ml, two parts of EG solution with graduated cylinder respectively, be labeled as EG1 and EG2 respectively, wherein the volume of EG1 solution is 7 ml, and the volume of EG2 solution is 10 ml.

To FeCl is housed ₃With pour EG2 solution in the beaker of PVP, with glass stick rough stir to be placed on be stirred to FeCl on the magnetic stirring apparatus ₃Be dispersed among the EG with PVP, this moment, solution was yellow.EG1 solution poured into AgNO is housed ₃Beaker in, with glass stick rough stir to be placed on be stirred to AgNO on the magnetic stirring apparatus ₃Be dispersed among the EG, this moment, solution was colourless transparent liquid.Under magnetic agitation, with water white AgNO ₃Solution evenly is added drop-wise to xanchromatic FeCl ₃In the mixing solutions of PVP, stir 1 min after, add the dense HCl solution of load weighted 3 ml, continue to stir this mixing solutions to stirring, this moment, solution was faint yellow.

Pouring the faint yellow mixing solutions of 20 ml of gained into 25 ml liners is in the hydrothermal reaction kettle of tetrafluoroethylene, puts into the loft drier that has set temperature (160 ℃) in advance, reacts 7 hours.

Take out reaction kettle, be cooled to room temperature at normal temperatures after, open reaction kettle, the solution in the liner is poured in the beaker.Solution in the beaker is poured in the centrifuge tube, put into whizzer, be 6000 rpm, time to be at rotating speed under the 10 min conditions with ethanol centrifugal for three times, finally obtains the AgCl micron particle.

In centrifuge tube, draw a spot of AgCl micron particle solution that contains with dropper, drop on the conductive resin that is attached to the sample table surface, it is leaf shape (like Fig. 1) that its pattern is observed with ESEM (SEM) in dry back.Detect the photocatalysis performance of micrometer structure AgCl through the experiment of illumination decomposition of methyl orange solution, draw this leaf shape micrometer structure AgCl particle through comparative analysis and have good photocatalysis performance.

Claims (2)

1. the preparation method of a leaf shape micrometer structure silver chloride particle, it is characterized in that: these method concrete steps are following:

(1) weighing reactant and solution: use electronic balance weighing FeCl ₃Solid and AgNO ₃Solid places respectively in two exsiccant beakers, and weighing PVP solid places FeCl is housed again ₃In the solid beaker, wherein PVP solid and AgNO ₃The solid mass ratio is PVP:AgNO ₃=(3:1) ~ (4:1), FeCl ₃Solid and AgNO ₃The solid mass ratio is FeCl ₃: AgNO ₃=1:10; Measure 1 part of dense HCl solution and two parts of EG solution respectively with graduated cylinder, two parts of EG solution are labeled as EG1 and EG2 respectively, and the volume ratio of wherein dense HCl solution, EG1 solution and EG2 solution is HCl:EG1:EG2=3:7:10, the AgNO of institute's weighing ₃The volume of employed dense HCl solution was 147 ml ~ 206 ml when solid was 1 g;

(2) proportioning mixing solutions: to FeCl is housed ₃With add EG2 solution in the beaker of PVP blended solid, after stirring with glass stick is rough, place and be stirred to FeCl on the magnetic stirring apparatus ₃Be dispersed in the EG2 solution with the PVP blended solid, this moment, solution was yellow; AgNO is equipped with in the adding of EG1 solution ₃In the solid beaker, after the rough stirring of glass stick, place and be stirred to AgNO on the magnetic stirring apparatus ₃Be dispersed among the EG1, this moment, solution was colourless transparent liquid; Under magnetic agitation, with water white AgNO ₃EG1 solution evenly splash into xanchromatic FeCl ₃In the EG2 mixing solutions of PVP, after stirring, add measured dense HCl solution, continue to stir this mixing solutions to mixing, this moment, solution was faint yellow;

(3) carry out hydrothermal synthesis reaction: the faint yellow mixing solutions of gained is poured in the hydrothermal reaction kettle that liner is a tetrafluoroethylene, put into loft drier, reaction 6 h ~ are 10 hours under 150 ℃ ~ 170 ℃ condition;

(4) abstraction reaction product A gCl: take out the hydrothermal reaction kettle in the loft drier; Be cooled to room temperature at normal temperatures; Open reaction kettle the solution in the liner is poured in the beaker, the solution in the beaker is poured in the centrifuge tube, put into whizzer; With ethanol centrifuge washing three times, finally obtain leaf shape micrometer structure silver chloride particle.

2. the preparation method of a kind of leaf shape micrometer structure silver chloride particle according to claim 1 is characterized in that: said FeCl ₃, AgNO ₃, EG, dense HCl be analytical pure, PVP is a CP, Mw=30000.

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