CN102701266B

CN102701266B - Preparation method for leaf-shaped silver chloride particle with micron structure

Info

Publication number: CN102701266B
Application number: CN201210169982.8A
Authority: CN
Inventors: 李美成; 余航; 姜永健; 李晓丹
Original assignee: North China Electric Power University
Current assignee: North China Electric Power University
Priority date: 2012-05-28
Filing date: 2012-05-28
Publication date: 2014-04-16
Anticipated expiration: 2032-05-28
Also published as: CN102701266A

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 has application potential very widely solving aspect the problem such as processing of the energy, environment and greenhouse gases, and photocatalyst material can be realized the functions such as photocatalytic hydrogen production by water decomposition, photodegradation organic pollutant and photoreduction carbonic acid gas.Traditional photocatalyst material is take titanium dioxide as representative, and its wider band gap makes it only can utilize the UV-light part that only accounts for sunlight 4%; In addition, the very easily compound quantum yield that also reduced in light induced electron and hole, therefore needs exploitation can utilize the new and effective photocatalyst material of larger wavelength region sunlight.Research is found, take silver chloride (AgCl) as substrate, the novel photocatalysis material of surface decoration Ag nanoparticle is due to the close contact between metal A g nanoparticle and semi-conductor AgCl, the electronic energy producing in system is more easily delivered in metallic silver particles, promoted the separation 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 sunlight 48%.

As everyone knows, micron or the nanostructure of material have remarkably influenced to its performance, and in order to improve the performance of catalysis, optics and electricity aspect of AgCl, the AgCl particle of the novel micron of research preparation or nanostructure is also more and more subject to people and pays close attention to.But, the AgCl grain pattern of having prepared at present is only confined to more dull cubes, chimb cubes, concave surface cubes and spherical, at the AgCl of these structures particle surface, decorate after Ag nanoparticle, all represented and be better than the absorbing wavelength responding range of traditional titanic oxide material to light.

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

Summary of the invention

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

A preparation method for leaf shape micrometer structure silver chloride particle, is characterized in that: the method concrete steps are as follows:

(1) weigh reactant and solution: use electronic balance weighing FeCl ₃solid and AgNO ₃solid is placed in respectively in two dry beakers, then weighs PVP solid and be placed in FeCl is housed ₃in the beaker of solid, wherein PVP solid and AgNO ₃the mass ratio of solid is PVP:AgNO ₃=(3:1) ~ (4:1), FeCl ₃solid and AgNO ₃the mass ratio of solid is FeCl ₃: AgNO ₃=1:10; Measure respectively 1 part of dense HCl solution and two parts of EG solution with graduated cylinder, two parts of EG solution are labeled as respectively EG1 and EG2, and wherein the volume ratio of dense HCl solution, EG1 solution and EG2 solution is HCl:EG1:EG2=3:7:10, the AgNO weighing ₃the volume of the dense HCl solution that solid is used during for 1 g is 147 ml ~ 206 ml;

(2) proportioning mixing solutions: to FeCl is housed ₃with in the beaker of PVP blended solid, add EG2 solution, after stirring with glass stick is rough, be placed in and on magnetic stirring apparatus, be stirred to FeCl ₃be dispersed in EG2 solution with PVP blended solid, now solution is yellow; EG1 solution is added AgNO is housed ₃in the beaker of solid, after stirring with glass stick is rough, be placed in and on magnetic stirring apparatus, be stirred to AgNO ₃be dispersed in EG1, now solution is colourless transparent liquid; Under magnetic agitation, by water white AgNO ₃eG1 solution evenly splash into yellow FeCl ₃in the EG2 mixing solutions of PVP, after stirring, add measured dense HCl solution, continue to stir this mixing solutions to mixing, now solution is 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 tetrafluoroethylene, put into loft drier, under the condition of 150 ℃ ~ 170 ℃, react 6 hours ~ 10 hours;

(4) abstraction reaction product A gCl: take out the hydrothermal reaction kettle in loft drier, be cooled at normal temperatures room temperature, opening reactor pours the solution in liner in beaker into, solution in beaker is poured in 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 chemical pure, Mw=30000.

Beneficial effect of the present invention is:

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

Accompanying drawing explanation

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

Fig. 2 contains leaf shape micrometer structure silver chloride, simple particulate state micrometer structure silver chloride and the Photocatalytic Degradation Property curve comparison figure of the methyl orange solution of chloride containing silver not.

Embodiment

The preparation method who the invention provides a kind of leaf shape micrometer structure silver chloride particle, below in conjunction with the drawings and specific embodiments, the present invention will be further described.

Embodiment 1

Weigh respectively 0.0016 g FeCl with electronic balance ₃, 0.0170 g AgNO ₃in two dry beakers, then weigh 0.0670 g PVP and be placed in FeCl is housed ₃beaker in; With graduated cylinder, measure the dense HCl of a 3 ml, two parts of EG solution respectively, be labeled as respectively EG1 and EG2, wherein the volume of EG1 solution is 7 ml, and the volume of EG2 solution is 10 ml.

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

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

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

A small amount of containing AgCl micron particle solution from drawing in centrifuge tube with dropper, drop on the conductive resin that is attached to sample table surface, by scanning electron microscope (SEM), observing its pattern after dry is leaf shape (as Fig. 1).The photocatalysis performance that detects micrometer structure AgCl by the experiment of illumination decomposition of methyl orange solution, show that through comparative analysis this leaf shape micrometer structure AgCl particle has good photocatalysis performance.

Claims

1. a preparation method for leaf shape micrometer structure silver chloride particle, is characterized in that: the method concrete steps are as follows:

(1) weigh reactant and solution: use electronic balance weighing FeCl ₃solid and AgNO ₃solid is placed in respectively in two dry beakers, then weighs PVP solid and be placed in FeCl is housed ₃in the beaker of solid, wherein PVP solid and AgNO ₃the mass ratio of solid is PVP:AgNO ₃=(3:1)～(4:1), FeCl ₃solid and AgNO ₃the mass ratio of solid is FeCl ₃: AgNO ₃=1:10; Measure respectively 1 part of dense HCl solution and two parts of EG solution with graduated cylinder, two parts of EG solution are labeled as respectively EG1 and EG2, and wherein the volume ratio of dense HCl solution, EG1 solution and EG2 solution is HCl:EG1:EG2=3:7:10, the AgNO weighing ₃the volume of the dense HCl solution that solid is used during for 1g is 147mL～206mL;

(2) proportioning mixing solutions: to FeCl is housed ₃with in the beaker of PVP blended solid, add EG2 solution, after stirring with glass stick is rough, be placed in and on magnetic stirring apparatus, be stirred to FeCl ₃be dispersed in EG2 solution with PVP blended solid, now solution is yellow; EG1 solution is added AgNO is housed ₃in the beaker of solid, after stirring with glass stick is rough, be placed in and on magnetic stirring apparatus, be stirred to AgNO ₃be dispersed in EG1 solution, now solution is colourless transparent liquid; Under magnetic agitation, by water white AgNO ₃eG1 solution evenly splash into yellow FeCl ₃in the EG2 mixing solutions of PVP, after stirring, add measured dense HCl solution, continue to stir this mixing solutions to mixing, now solution is 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 tetrafluoroethylene, put into loft drier, under the condition of 150 ℃～170 ℃, react 6 hours～10 hours;

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