CN102698782B - Dendrite silver phosphate visible light catalyst and preparation method thereof - Google Patents
Dendrite silver phosphate visible light catalyst and preparation method thereof Download PDFInfo
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- CN102698782B CN102698782B CN201210209468.2A CN201210209468A CN102698782B CN 102698782 B CN102698782 B CN 102698782B CN 201210209468 A CN201210209468 A CN 201210209468A CN 102698782 B CN102698782 B CN 102698782B
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Abstract
The invention provides a dendritic silver phosphate visible light catalyst and a preparation method thereof. The appearance of silver phosphate is adjusted with sodium deoxycholate, so as to form the dendritic silver phosphate which has an efficient visible light catalytic performance and is suitable for degrading organic pollutants under visible light. The invention has the advantages that the preparation process is simple; the condition is mild; and the dendritic silver phosphate visible light catalyst is favorable for application to mass production practice.
Description
Technical field
The present invention relates to photocatalysis field, be specifically related to dendroid silver orthophosphate visible light catalyst and preparation method thereof.
Background technology
Ag
3pO
4be a kind of visible light catalyst of better performances, this is mainly by itself structures shape.Ag
3pO
4the strong oxidizing property in optical excitation hole in distinctive indirect band gap, valence band, its electron transfer rate is higher than hole migration speed simultaneously, thereby impels electron-hole separated.PO
4 3-inductive effect can impel electron-hole separated, this is conducive to improve visible light catalytic performance.While Ag vacancy defect can participate in photoelectron and catch, and more optical excitation hole is provided, and is also conducive to electron-hole separation.
But because of its pattern and performance easy-regulating not, make that its related manufacturing processes is less at present.
Summary of the invention
Object of the present invention aims to provide dendroid silver orthophosphate visible light catalyst and preparation method thereof.The dendroid silver orthophosphate that the present invention prepares, has efficient visible light photocatalytic degradation effect.
Technical scheme of the present invention is:
A silver orthophosphate visible light catalyst, is characterized in that: this catalyst is Powdered, and its microstructure is dendritic structure.
The preparation method of dendroid silver orthophosphate visible light catalyst of the present invention, its preparation process is as follows:
1), take AgAc deionized water dissolving, being configured to 30mL concentration is the AgAc solution of 0.03M-0.3M;
2), configuration 6mL concentration is 0.036M-0.36M deoxycholic acid sodium solution;
3), under the condition of magnetic agitation, by step 2) deoxycholic acid sodium solution slowly inject consoluet AgAc solution (AgAc solution is 30 milliliters), AgAc and NaTDC mol ratio=25:6, room temperature lower magnetic force stirs 2h;
4), in step 3) gained solution, add 4mL distilled water, adding 1-10 to drip concentration is 85wt% phosphoric acid, and magnetic agitation 1h, obtains sediment;
5), the centrifugation of step 4) gained sediment is collected, with deionized water and ethanol wash respectively 2 times above after, and dry under 60 ℃ of air atmospheres, obtain dendritic structure silver orthophosphate visible light catalyst Powdered.
In technical scheme of the present invention, utilize NaTDC to regulate and control silver orthophosphate pattern, thereby obtain dendritic structure.
In technical scheme of the present invention, for obtaining the silver orthophosphate of dendritic structure, silver-colored source used is silver acetate.
In technical scheme of the present invention, for forming the silver orthophosphate of dendritic structure, adopt phosphoric acid that phosphate anion is provided.
Dendroid silver orthophosphate visible light catalyst prepared by the present invention, is applicable to degradable organic pollutant under visible ray condition.
The invention has the advantages that:
1. the dendritic structure silver orthophosphate visible light catalyst that the present invention prepares, has excellent photocatalysis performance, can rapid degradable organic pollutant under visible ray condition.
2. the present invention utilizes NaTDC to regulate and control silver orthophosphate pattern.
4. process of the present invention is simple, and mild condition is conducive to the application of large-scale production practice.
Room temperature of the present invention means temperature 10-30 ℃.
Accompanying drawing explanation
Fig. 1. X-ray diffraction (XRD) figure of dendroid silver orthophosphate visible light catalyst prepared by the inventive method
Fig. 2. the SEM figure of dendroid silver orthophosphate visible light catalyst prepared by the inventive method
Fig. 3. the ultraviolet-visible absorption spectroscopy figure of dendroid silver orthophosphate visible light catalyst prepared by the inventive method
Fig. 4. dendroid silver orthophosphate visible light catalyst prepared by the inventive method is in visible light photocatalytic degradation rhodamine B performance
Fig. 5. dendroid silver orthophosphate visible light catalyst prepared by the inventive method is in visible light photocatalytic degradation MO (methyl orange) performance.
The specific embodiment
Preparation method's step of dendroid silver orthophosphate visible light catalyst of the present invention is as follows:
Take respectively a certain amount of AgAc, be placed in beaker and dissolve respectively by deionized water, configuration obtains the AgAc solution that concentration is 0.03M-0.3M.Configuration 6mL concentration 0.036M-0.36M NaTDC, under the condition of magnetic agitation, NaTDC is injected to consoluet AgAc solution (30 milliliters of the AgAc solution that concentration is 0.3M add 6 milliliters of the NaTDCs of 0.36M concentration) room temperature lower magnetic force slowly and stir 2h.In above-mentioned solution, add 4mL distilled water, add 1-10 to drip the phosphoric acid of 85wt%, magnetic agitation 1h, obtains sediment.Sediment is collected by centrifugation, then washs 3 times respectively with deionized water and ethanol, then in 60 ℃ of oven dry.Obtain dendroid silver orthophosphate visible light catalyst product.Utilize NaTDC to regulate and control silver orthophosphate pattern, thereby obtain dendritic structure.
For obtaining the silver orthophosphate of dendritic structure, silver-colored source used is silver acetate.
For forming the silver orthophosphate of dendritic structure, adopt phosphoric acid that phosphate anion is provided.
The dendroid silver orthophosphate visible light catalyst of below in conjunction with example case being prepared by the inventive method and its application are described further, but the present invention is not limited only to following embodiment.
Take AgAc, be placed in beaker and dissolve respectively by deionized water, being made into 30mL concentration is the AgAc solution of 0.03M.Configuration 6mL 0.036M NaTDC slowly injects it consoluet AgAc solution under the condition of magnetic agitation, and room temperature lower magnetic force stirs 2h.In above-mentioned solution, add 4mL distilled water, add the phosphoric acid of 1 85wt%, magnetic agitation 1h.Sediment is collected by centrifugation, then washs several times with deionized water, alcohol, dries de for 60 ℃ and obtains sample.
Fig. 1 is the X ray diffracting spectrum of gained sample, the diffraction maximum of all samples and simple cubic crystal Ag
3pO
4standard diagram (JCPDS No. 06-0505) is completely corresponding.And in diffracting spectrum, do not have the diffraction maximum of other crystal to occur, illustrate that the material of preparation is pure Ag
3pO
4crystal.
Fig. 2 is the SEM picture of gained sample, and as seen from the figure, sample is dendroid silver orthophosphate visible light catalyst.It is 500nm left and right dendroid Ag
3pO
4, on branch, there are some stem tubers, so branch surface is also rough, between branch, angle is uncertain, the length of each branch top set is also uncertain simultaneously.
Figure 3 shows that dendroid silver orthophosphate visible light catalyst sample UV-Vis DRS spectrogram.Known in figure, sample has obvious absworption peak in visible region, and sample can absorb the visible ray that is less than 530nm.
The visible light catalytic performance evaluation of the dendroid silver orthophosphate that the inventive method makes.
The visible light catalytic performance of the dendroid silver orthophosphate that the inventive method makes is by under simulation visible ray, adopts the situation of sample degradation of organic substances to evaluate.Photocatalysis experiment is carried out in photochemical reactor (comprising Xe lamp 350W, optical filter, magnetic stirring apparatus).Take 0.05g and prepare sample, add liquid dyes solution (10
-5m RhB(rhodamine B), 30mg/L MO (methyl orange)), lucifuge condition lower magnetic force stirs 30min, reaches and adsorbs-desorb balance.350W Xe lamp adds optical filter (λ > 420nm) and, as analog light source, gets at regular intervals 3ml suspension, after centrifugation (6000rpm, 5min), gets supernatant.Use UV-2550 ultraviolet-visual spectrometer to measure the absorbance of dye solution.Fig. 4 and Fig. 5 are the visible light catalytic performance of the dendroid silver orthophosphate visible light catalyst prepared of the present invention, and dendroid silver orthophosphate can be degradable by MO in 7min, in 4min by RhB degraded completely.
Claims (3)
1. a silver orthophosphate visible light catalyst, is characterized in that: this catalyst is Powdered, and its microstructure is dendritic structure, and preparation method is:
1), take AgAc deionized water dissolving, being configured to 30mL concentration is the AgAc solution of 0.03M-0.3M;
2), configuration 6mL concentration is 0.036M-0.36M deoxycholic acid sodium solution;
3), under the condition of magnetic agitation, by step 2) the deoxycholic acid sodium solution implantation step 1 that blows slowly) 30 milliliters of AgAc solution in, AgAc and NaTDC mol ratio=25:6, room temperature lower magnetic force stirs 2h;
4), in step 3) gained solution, add 4mL distilled water, adding 1-10 to drip concentration is 85wt% phosphoric acid, and magnetic agitation 1h, obtains sediment;
5), the centrifugation of step 4) gained sediment is collected, with deionized water and ethanol wash respectively 2 times above after, and dry under 60 ℃ of air atmospheres, obtain dendritic structure silver orthophosphate visible light catalyst powder.
2. the preparation method of silver orthophosphate visible light catalyst as claimed in claim 1, is characterized in that:
1), take AgAc deionized water dissolving, being configured to 30mL concentration is the AgAc solution of 0.03M-0.3M;
2), configuration 6mL concentration is 0.036M-0.36M deoxycholic acid sodium solution;
3), under the condition of magnetic agitation, by step 2) the deoxycholic acid sodium solution implantation step 1 that blows slowly) 30 milliliters of AgAc solution in, AgAc and NaTDC mol ratio=25:6, room temperature lower magnetic force stirs 2h;
4), in step 3) gained solution, add 4mL distilled water, adding 1-10 to drip concentration is 85wt% phosphoric acid, and magnetic agitation 1h, obtains sediment;
5), the centrifugation of step 4) gained sediment is collected, with deionized water and ethanol wash respectively 2 times above after, and dry under 60 ℃ of air atmospheres, obtain dendritic structure silver orthophosphate visible light catalyst powder.
3. the application of silver orthophosphate visible light catalyst as claimed in claim 1, is characterized in that: be applicable to degradable organic pollutant under visible ray condition.
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| CN103263937B (en) * | 2013-06-17 | 2015-03-25 | 南京信息工程大学 | Method for preparing tetrahedral silver phosphate photocatalyst |
| CN103272622B (en) * | 2013-06-20 | 2015-03-11 | 南京信息工程大学 | Preparation method of silver phosphate photocatalyst |
| CN107311135B (en) * | 2017-07-14 | 2019-04-05 | 华南师范大学 | A kind of preparation method of polypody shape phosphoric acid ag material |
| CN110227510A (en) * | 2019-06-26 | 2019-09-13 | 成都理工大学 | A kind of preparation method of low temperature liquid phase precipitation method silver orthophosphate visible-light photocatalyst |
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| CN101648139B (en) * | 2009-09-03 | 2011-05-04 | 福州大学 | Preparation method of novel visible catalyst-silver phosphate |
| CN101940937B (en) * | 2010-10-21 | 2012-04-25 | 武汉理工大学 | High-efficiency visible light catalyst silver phosphate and preparation method thereof |
| CN102000594B (en) * | 2010-11-26 | 2012-05-16 | 大连理工大学 | Preparation method of visible light photo catalyst silver and silver phosphate and application thereof |
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