CN103934007A - Oxidization synthesis method for network structure of surface plasma visible light catalyst Ag/AgCl - Google Patents
Oxidization synthesis method for network structure of surface plasma visible light catalyst Ag/AgCl Download PDFInfo
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- CN103934007A CN103934007A CN201410124633.3A CN201410124633A CN103934007A CN 103934007 A CN103934007 A CN 103934007A CN 201410124633 A CN201410124633 A CN 201410124633A CN 103934007 A CN103934007 A CN 103934007A
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Abstract
The invention relates to an oxidization synthesis method for a network structure of a surface plasma visible light catalyst Ag/AgCl. The oxidization synthesis method comprises the following two steps: 1, synthesizing a nano silver wire, namely preparing a silver salt and a surfactant solution, dropwise adding the silver salt and the surfactant solution into a three-necked flask containing an organic solvent heated to a certain temperature, and reacting for a period of time to generate the silver wire; and 2, oxidizing and carrying out ion exchange to form the Ag/AgCl network structure, namely weighing chlorate, preparing the chlorate into a solution, slowly dropwise adding the solution into the system, reacting for a period of time, cooling, centrifuging a sample, washing, drying, and collecting to obtain the product. The oxidization synthesis method is simple in process; the preparation conditions are universal, the shape of the product is stable and the purity of the product is high; the product is simple to treat and the oxidization synthesis method is suitable for middle-scale industrial production.
Description
Technical field
The invention belongs to technical field of inorganic nanometer material, relate in particular to the oxidation synthesis method of the network structure of a kind of surface plasma visible light catalyst Ag/AgCl.
Background technology
Nanoscale science and technology be produce late 1980s one just in the new technology of fast development.So-called nanometer technology refers to the unit with some molecules or atomic building---nanoparticle, the science and technology of manufactured materials or microdevice.Nanoparticle refers to metal or the semi-conductive fine particle of size between 1～100 nm.The special construction level that nanoparticle has, give its much special character and function, nano particle has large specific area, surface atom number, surface energy and surface tension sharply increase with the decline of particle diameter, skin effect, small-size effect, quantum size effect, macro quanta tunnel effect and Dielectric confinement effect etc. cause thermal and magnetic, light, sensitivity characteristic and the surface stability etc. of nano particle to be different from conventional particle, and this just makes it be with a wide range of applications.
Silver halide is widely used in manufacturing photo film, on hectograph and gummed paper. silver chlorate also has very important application in electrochemistry, silver monochlor(in)ate silver reference electrode is difficult for polarization, thereby can provide more accurate data. the photosensitivity of silver halide and unstability have limited its application aspect photocatalysis, if can make silver halide stable existence under irradiation just can be applied to aspect photocatalysis. and the argent of nanoscale has stronger absorption in black light district, by adjusting the size of argent, the residing environment of shape and nano particle can make its absorption spectrum generation red shift.In theory, can utilize silver nano-grain to strengthen the absorption of catalysis material to sunshine.In this experiment, silver and silver chlorate are carried out effectively compound, form the network structure of Ag/AgCl, first, due to the close contact of argent and silver chlorate, the electronic energy producing in system is more easily delivered in metallic silver particles, effectively promote separating and then having improved quantum efficiency of electronics and hole, ensured the stability of system; Secondly, the network structure of this novelty has larger specific area, and how light-catalysed avtive spot can be provided, and improves catalytic efficiency; Again, the network structure of Ag/AgCl has been expanded the response of system to visible ray effectively, makes it have very strong absorption at whole visible region, has greatly improved the utilization rate to sunshine.This method has been widened by metal surface plasma resonance body effect and has been strengthened the approach of catalysis material to visible absorption, and then has improved the performance of catalysis material.
Summary of the invention
The object of this invention is to provide the oxidation synthesis method of the network structure of a kind of surface plasma visible light catalyst Ag/AgCl.
To achieve these goals, technical scheme of the present invention is as follows:
An oxidation synthesis method for the network structure of surface plasma visible light catalyst Ag/AgCl, concrete steps are as follows:
(1) nano-silver thread is synthetic
Take silver salt and surfactant, it is dissolved in respectively in solvent, obtain silver salt solution and surfactant solution; Take a morsel solvent in three-neck flask, and magnetic agitation is also heated to 160 ~ 180 DEG C, after solvent temperature is stable, silver salt solution and surfactant solution is dropwise joined in described three-neck flask simultaneously, reacts after 70-80 minute, generates nano-silver thread; Wherein: the mol ratio of silver salt and surfactant is 1:1;
(2) oxidation and ion-exchange form Ag/AgCl network structure
Take chlorate, be dissolved in solvent, obtain solution of chlorate, solution is slowly joined in step (1) gained system, reaction 0-60 minute, cooling, sample is carried out centrifugal, washing, dry, obtain required product: wherein: the mol ratio of silver salt and chlorate is 1:1.
In the present invention, described in step (1) and step (2), solvent is ethylene glycol, and purity level is pure for analyzing.
In the present invention, described silver salt is silver nitrate, and its concentration is 0.12mol/L.
In the present invention, described surfactant is polyvinylpyrrolidone, and its average molecular mass is 1300000.
In the present invention, described chlorate is copper chloride, and its concentration is 0.12mol/L.
In the present invention, step adds thermal recovery oil bath pan described in (1), and whole heating process has condensation reflux unit.
In the present invention, the described washing of step (2) is by ethanol and deionized water washed product respectively.
In the present invention, dry described in step (2) is dry 10h in 60 DEG C of vacuum drying chambers.
Owing to adopting such scheme, the present invention has following beneficial effect:
1, to have realized and utilized common mantoquita and chlorate be presoma in the present invention, synthesized first the composite of Ag/AgCl network structure by adding hot reflux.
2, method of the present invention has very high control to the pattern of product.
3, the present invention adopts simple inorganic salts as reactant, has very strong versatility.
4, the product that prepared by the present invention has the good Photocatalytic Degradation Property to organic pollution, can be used as high-performance optical catalyst, has comparatively vast potential for future development and application space.
5, technique of the present invention is simple, and preparation condition is general, and product stable appearance, purity are high, and product processes convenient succinctly, is suitable for medium-scale industrial production.
6, method of the present invention has mild condition, homogeneous heating, efficient energy-saving, is easy to the features such as control.
Brief description of the drawings
Fig. 1 is the SEM photo of the intermediate product that obtains under the multiple of 200nm in embodiment 1.
Fig. 2 is the SEM photo of the product that obtains under the multiple of 600nm in embodiment 1.
Fig. 3 is the TEM photo of the product that obtains under the multiple of 200nm in embodiment 1.
Fig. 4 is the XRD collection of illustrative plates of embodiment 1 products therefrom.
Fig. 5 is the EDS collection of illustrative plates of embodiment 1 products therefrom.
Fig. 6 is the SEM photo of the product that obtains under the multiple of 200nm in embodiment 2.
Fig. 7 is the SEM photo of the product that obtains under the multiple of 200nm in embodiment 3.
Detailed description of the invention
Below in conjunction with accompanying drawing illustrated embodiment, the present invention is further detailed explanation.
Embodiment 1
The first step: take respectively 0.204g AgNO
3, 0.1332g polyvinylpyrrolidone (PVP), 0.204g CuCl
22H
2o is placed in three labels and is respectively A, and B, in the reaction bulb of the 20ml of C, adds respectively 10ml ethylene glycol ultrasonic to being dissolved as clear solution.
Second step: measure 10ml ethylene glycol in the three-neck flask of 50ml, add magneton, and be fixed on iron stand, be placed in oil bath pan, put up reflux condensate device, open recirculation water and oil bath pan switch, set temperature is 160 DEG C, and opens magnetic agitation.
The 3rd step: wait oil bath pan to reach set temperature stable, dropwise add AgNO simultaneously
3solution and PVP solution, time for adding continues ten minutes.
The 4th step: react 80 minutes, solution becomes milky, dropwise adds CuCl
2solution, time for adding continues ten minutes.
The 5th step: react ten minutes, close oil bath pan and condensed water, and oil bath pan is shifted out to liquid level, be cooled to room temperature, with absolute ethyl alcohol and deionized water washing several, be placed in vacuum drying chamber dry.
Fig. 1 is the SEM photo of the intermediate product silver line product that obtains under the multiple of 200nm in embodiment 1; Fig. 2 is the SEM photo of the product that obtains under the multiple of 200nm in embodiment 1; Fig. 3 is the TEM picture of embodiment 1 products therefrom; Fig. 4 is the XRD collection of illustrative plates of embodiment 1 products therefrom, and the existing AgCl in compound is described, has again Ag to exist.Fig. 5 is the EDS collection of illustrative plates of embodiment 1 products therefrom, and the atomicity of Ag is more than the atomicity of Cl, and further having proved product is Ag/AgCl compound.
Embodiment 2
The first step: take respectively 0.204g AgNO3,0.1332g polyvinylpyrrolidone (PVP), 0.102g CuCl
22H
2o is placed in three labels and is respectively A, and B, in the reaction bulb of the 20ml of C, adds respectively 10ml ethylene glycol ultrasonic to being dissolved as clear solution.
Second step: measure 10ml ethylene glycol in the three-neck flask of 50ml, add magneton, and be fixed on iron stand, be placed in oil bath pan, put up reflux condensate device, open recirculation water and oil bath pan switch, set temperature is 160 DEG C, and opens magnetic agitation.
The 3rd step: wait oil bath pan to reach set temperature stable, dropwise add AgNO3 solution and PVP solution simultaneously, time for adding continues ten minutes.
The 4th step: react 80 minutes, solution becomes milky, dropwise adds CuCl
2solution, time for adding continues ten minutes.
The 5th step: react 40 minutes, close oil bath pan and condensed water, and oil bath pan is shifted out to liquid level, be cooled to room temperature, with absolute ethyl alcohol and deionized water washing several, be placed in vacuum drying chamber dry.
Fig. 5 is the SEM photo of the product that obtains under the multiple of 200nm in embodiment 2.Can be found out by picture, still can form with this understanding the network structure of Ag/AgCl, just net is thicker, and the surface area that compares is less.
Embodiment 3
The first step: take respectively 0.204g AgNO
3, 0.1332g polyvinylpyrrolidone (PVP), 0.204g CuCl
22H
2o is placed in three labels and is respectively A, and B, in the reaction bulb of the 20ml of C, adds respectively 10ml ethylene glycol ultrasonic to being dissolved as clear solution.
Second step: measure 10ml ethylene glycol in the three-neck flask of 50ml, add magneton, and be fixed on iron stand, be placed in oil bath pan, put up reflux condensate device, open recirculation water and oil bath pan switch, set temperature is 180 DEG C, and opens magnetic agitation.
The 3rd step: wait oil bath pan to reach set temperature stable, dropwise add AgNO3 solution and PVP solution simultaneously, time for adding continues ten minutes.
The 4th step: react 80 minutes, solution becomes milky, dropwise adds CuCl2 solution, time for adding continues ten minutes.
The 5th step: react 40 minutes, close oil bath pan and condensed water, and oil bath pan is shifted out to liquid level, be cooled to room temperature, with absolute ethyl alcohol and deionized water washing several, be placed in vacuum drying chamber dry.
Fig. 6 is the SEM photo of the product that obtains under the multiple of 200nm in embodiment 2.Can be found out by picture, still can form with this understanding the network structure of Ag/AgCl, net spacing is larger, comparatively loose.
The above-mentioned description to embodiment is can understand and apply the invention for ease of those skilled in the art.Person skilled in the art obviously can easily make various amendments to these embodiment, and General Principle described herein is applied in other embodiment and needn't passes through performing creative labour.Therefore, the invention is not restricted to the embodiment here, the amendment of making in the situation that not departing from category of the present invention is all within protection scope of the present invention.
Claims (8)
1. an oxidation synthesis method for the network structure of surface plasma visible light catalyst Ag/AgCl, is characterized in that concrete steps are as follows:
(1) nano-silver thread is synthetic
Take silver salt and surfactant, it is dissolved in respectively in solvent, obtain silver salt solution and surfactant solution; Take a morsel solvent in three-neck flask, and magnetic agitation is also heated to 160 ~ 180 DEG C, after solvent temperature is stable, silver salt solution and surfactant solution is dropwise joined in described three-neck flask simultaneously, reacts after 70-80 minute, generates nano-silver thread; Wherein: the mol ratio of silver salt and surfactant is 1:1;
(2) oxidation and ion-exchange form Ag/AgCl network structure
Take chlorate, be dissolved in solvent, obtain solution of chlorate, solution is slowly joined in step (1) gained system, reaction 0-60 minute, cooling, sample is carried out centrifugal, washing, dry, obtain required product: wherein: the mol ratio of silver salt and chlorate is 1:1.
2. the oxidation synthesis method of the network structure of a kind of surface plasma visible light catalyst Ag/AgCl according to claim 1, it is characterized in that: described in step (1) and step (2), solvent is ethylene glycol, purity level is pure for analyzing.
3. the oxidation synthesis method of the network structure of a kind of surface plasma visible light catalyst Ag/AgCl according to claim 1, is characterized in that: described silver salt is silver nitrate, and its concentration is 0.12mol/L.
4. the oxidation synthesis method of the network structure of a kind of surface plasma visible light catalyst Ag/AgCl according to claim 1, is characterized in that: described surfactant is polyvinylpyrrolidone, and its average molecular mass is 1300000.
5. the oxidation synthesis method of the network structure of a kind of surface plasma visible light catalyst Ag/AgCl according to claim 1, is characterized in that: described chlorate is copper chloride, and its concentration is 0.12mol/L.
6. the oxidation synthesis method of the network structure of a kind of surface plasma visible light catalyst Ag/AgCl according to claim 1, is characterized in that: step adds thermal recovery oil bath pan described in (1), and whole heating process has condensation reflux unit.
7. the oxidation synthesis method of the network structure of a kind of surface plasma visible light catalyst Ag/AgCl according to claim 1, is characterized in that: the described washing of step (2) is by ethanol and deionized water washed product respectively.
8. the oxidation synthesis method of the network structure of a kind of surface plasma visible light catalyst Ag/AgCl according to claim 1, is characterized in that: dry described in step (2) is dry 10h in 60 DEG C of vacuum drying chambers.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104190449A (en) * | 2014-08-20 | 2014-12-10 | 江苏大学 | Preparation method for hollow Ag/AgCl nano-structure photocatalysis material |
| CN104400001A (en) * | 2014-11-14 | 2015-03-11 | 东北林业大学 | Method for preparing Ag/AgCl nanocomposite by utilizing trichoderma hamatum extracellular fluid |
| CN104841947A (en) * | 2015-04-30 | 2015-08-19 | 同济大学 | Synthesis method of cable type silver chloride coated copper nano-structure |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102441376A (en) * | 2011-10-25 | 2012-05-09 | 通化师范学院 | Photoactivation preparation method of AgCl/Ag nano visible light catalyst |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102441376A (en) * | 2011-10-25 | 2012-05-09 | 通化师范学院 | Photoactivation preparation method of AgCl/Ag nano visible light catalyst |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104190449A (en) * | 2014-08-20 | 2014-12-10 | 江苏大学 | Preparation method for hollow Ag/AgCl nano-structure photocatalysis material |
| CN104400001A (en) * | 2014-11-14 | 2015-03-11 | 东北林业大学 | Method for preparing Ag/AgCl nanocomposite by utilizing trichoderma hamatum extracellular fluid |
| CN104400001B (en) * | 2014-11-14 | 2016-03-16 | 东北林业大学 | A kind of method utilizing the mould extracellular fluid of hook-shaped wood to prepare Ag/AgCl nano composite material |
| CN104841947A (en) * | 2015-04-30 | 2015-08-19 | 同济大学 | Synthesis method of cable type silver chloride coated copper nano-structure |
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