CN103263937B - Method for preparing tetrahedral silver phosphate photocatalyst - Google Patents
Method for preparing tetrahedral silver phosphate photocatalyst Download PDFInfo
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- CN103263937B CN103263937B CN201310238378.0A CN201310238378A CN103263937B CN 103263937 B CN103263937 B CN 103263937B CN 201310238378 A CN201310238378 A CN 201310238378A CN 103263937 B CN103263937 B CN 103263937B
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- tetrahedral
- silver phosphate
- photocatalyst
- silver
- phosphoric acid
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Abstract
The invention discloses a novel method for preparing a tetrahedral silver phosphate photocatalyst. The silver phosphate photocatalyst is tetrahedral. The method is characterized by comprising the steps of taking separate water as a solvent, sequentially adding silver nitrate, urotropine and phosphoric acid while stirring, and carrying out centrifugal drying finally, thereby preparing the tetrahedral silver phosphate photocatalyst. The method disclosed by the invention is environment-friendly, simple, low in cost and easy to popularize; and the photocatalyst can be used for removing organic pollutants from water efficiently and has good application prospects.
Description
Technical field
The invention belongs to photocatalysis technology field, is a kind of preparation method of tetrahedral silver phosphate photocatalyst specifically.
Background technology
In order to utilize sunshine to a greater extent, people expect to develop more efficient visible-light-responsive photocatalyst.For this problem, Japanese material and Materials Research Institution photocatalyst material center researchers are conceived to the silver orthophosphate (Ag that nobody shows any interest in
3pO
4), according to experimental result such as investigation its water decomposition performance under visible light illumination and coating decomposability etc., find out that silver orthophosphate photooxidation performance is under visible light the decades of times of known photochemical catalyst at present.Relevant result is published in " nature " magazine material version with the article being entitled as " the phosphate semiconductor under excited by visible light with photooxidation performance ", this novel photochemical catalyst of reported first.This research center finds Ag
3pO
4absorbing wavelength can be less than the sunshine of 520 nm, quantum yield under visible light up to 90%, and shows powerful oxidability under visible light illumination.In the experiment of product oxygen, Ag under visible ray
3pO
4speed far above other visible-light response type catalyst, as BiVO
4, WO
3.Meanwhile, Ag
3pO
4in the Degrading experiment of methylene blue, show powerful oxidative degradation ability, the speed of equal number methylene blue of degrading under visible light is far ahead of TiO
2-xNx, BiVO
4deng photochemical catalyst.And Ag
3pO
4absorbing wavelength can be less than the sunshine of 520 nm, and quantum yield is under visible light up to 90%, it has huge potentiality in visible light catalytic.At present, the existing report of different structure silver orthophosphate, as nanometer granule, four forked types, regular hexahedron, granatohedron etc.Silver orthophosphate (Z. Yi, J. Ye, N. Kikugawa have prepared by solid phase method in leaf golden flower seminar, T. Kako, S. Ouyang, H.S. Williams, H. Yang, J. Cao, W. Luo, Z. Li, Y. Liu, R.L. Withers, Nature Materials 9 (2010) 559.), but the silver orthophosphate particle obtained does not have regular morphology and size is comparatively large, and in general the product particles radius decentralization of solid phase reaction acquisition is large, and random pattern.Compared with traditional solid reaction process, liquid-phase precipitation method is easy and simple to handle, have controllability, can avoid introducing the disadvantageous objectionable impurities of material, the product of generation has that higher chemical uniformity, granularity are comparatively thin, particle size distribution is narrower and has certain pattern simultaneously.Therefore seek effective silver orthophosphate preparation method and have very important effect to its photocatalytic Quality Research.
Summary of the invention
The object of the invention is there is no regular morphology and larger-size deficiency for preparing the silver orthophosphate particle drawn in above-mentioned prior art, a kind of preparation method utilizing liquid-phase precipitation method to prepare tetrahedral silver phosphate photocatalyst is at ambient temperature provided.
The object of the invention is to be achieved through the following technical solutions:
The preparation method of tetrahedral silver phosphate photocatalyst of the present invention is, at room temperature, be that solvent adds silver nitrate, methenamine, phosphoric acid under agitation with water, the concrete steps of preparation method comprise:
1) add in deionized water by by silver nitrate, stir, the liquor argenti nitratis ophthalmicus of preparation 0.0075g/ml-0.01 g/ml concentration;
2) in step 1) gained liquor argenti nitratis ophthalmicus, add methenamine, stir; Wherein every milliliter of described liquor argenti nitratis ophthalmicus adds 0.005-0.01g methenamine;
3) continue to step 2) add phosphoric acid in gained solution, stir 5 minutes, obtain turbid solution, dry under turbid solution being carried out centrifugation, washing, 40-60 DEG C temperature, obtain tetrahedral silver phosphate; Wherein described in often liter of step 1), liquor argenti nitratis ophthalmicus adds 2.5-3.25ml phosphoric acid;
Water level pure water used in above-mentioned steps, in step 3), the concentration of phosphoric acid is mass percent 85%.
Methenamine used in the present invention, also referred to as hexa, hexamethylenetetramine, be a multi-ring heterocyclic compound similar with adamantane structure, molecular formula is C
6h
12n
4, be a kind of widely used chemical materials.
The tetrahedral silver phosphate photocatalyst that the inventive method obtains is tetrahedral silver phosphate, and crystal particle diameter, at about 2 μm, can exceed about 5 times than dodecahedron silver orthophosphate activity.
the present invention has following outstanding beneficial effect:
Method preparation condition of the present invention is simple, be easy to control, synthesis cycle is short, and cost is lower, without the need to heating, obtained tetrahedral silver phosphate crystal particle diameter is at about 2 μm, and be less than the illumination of 520nm at wavelength under, its degraded Luo Dan Ming B activity is compared common commercial type TiO
2have and significantly improve, be applicable to large-scale promotion.
Accompanying drawing explanation
Fig. 1 is tetrahedral silver phosphate photocatalyst scanning electron microscope (SEM) photograph (SEM) of the present invention;
Fig. 2 is the scanning electron microscope (SEM) photograph (SEM) that tetrahedral silver phosphate photocatalyst of the present invention is amplified;
Fig. 3 is that the obtained tetrahedral silver phosphate of embodiment 1 and dodecahedron silver orthophosphate are as photocatalyst for degrading rhodamine B experimental result comparison diagram;
In Fig. 3: curve A be dodecahedron silver orthophosphate as rhodamine B light degradation situation during photochemical catalyst, curve B is that tetrahedral silver phosphate is as rhodamine B light degradation situation during photochemical catalyst.C
0for the initial concentration of Luo Dan Ming B, C is the Luo Dan Ming B concentration value measured after visible ray (>420 nm) irradiates a period of time, and t is that Luo Dan Ming B concentration drops to certain concentration time used.
Detailed description of the invention
Below in conjunction with drawings and Examples, the invention will be further described:
case study on implementation one:
Under room temperature, get the pure water (deionized water) of 40mL, pour in beaker, add the silver nitrate of 0.318g under agitation, then add 0.315g methenamine, fully stir, the last phosphoric acid adding 123 μ L again, stir five minutes, centrifuge washing precipitates, and dries and can obtain tetrahedral silver phosphate at 60 DEG C of temperature.Fig. 1, Fig. 2 are the scanning electron microscope (SEM) photographs (SEM) of the product that the present embodiment obtains, and as can be seen from the figure it is tetrahedral.
The tetrahedral silver phosphate obtained and dodecahedron silver orthophosphate are used as catalyst degradation rhodamine B, take 100mg sample and add 200mL rhodamine B solution (10-50mg/L), lucifuge stirs 30 min, makes rhodamine B solution reach absorption/desorption equilibrium at catalyst surface.Then open light source and carry out light-catalyzed reaction, get 15mL reactant liquor every 3 min, after centrifugation, supernatant spectrophotometer detects.Rhodamine B change in concentration in degradation process is determined per sample at 550 nm place absorbances.What adopt in the present embodiment is 300W xenon lamp, uses optical filter to ensure that incident light is for visible ray (>420nm).The light degradation situation now obtained as shown in Figure 3, tetrahedral silver phosphate activity (light degradation situation is curve B) will exceed about 5 times than dodecahedron silver orthophosphate activity (light degradation situation is curve A) as seen from Figure 3, and therefore tetrahedral silver phosphate has efficient photocatalysis performance.
case study on implementation two:
Under room temperature, get the pure water (deionized water) of 40mL, pour in beaker, add the silver nitrate of 0.3g under agitation, then add 0.2g methenamine, fully stir, the last phosphoric acid adding 100 μ L again, stir five minutes, centrifuge washing precipitates, and dries and can obtain tetrahedral silver phosphate at 40 DEG C of temperature.
case study on implementation three:
Under room temperature, get the pure water (deionized water) of 40mL, pour in beaker, add the silver nitrate of 0.4g under agitation, then add 0.4g methenamine, fully stir, the last phosphoric acid adding 130 μ L again, stir five minutes, centrifuge washing precipitates, and dries and can obtain tetrahedral silver phosphate at 50 DEG C of temperature.
Be more than preferred embodiment of the present invention, all changes done according to technical solution of the present invention, when the function produced does not exceed the scope of technical solution of the present invention, all belong to protection scope of the present invention.
Claims (1)
1. a preparation method for tetrahedral silver phosphate photocatalyst, concrete steps comprise:
1) silver nitrate is added in deionized water, stir, be mixed with the liquor argenti nitratis ophthalmicus that concentration is 0.0075-0.01g/ml;
2) in step 1) gained liquor argenti nitratis ophthalmicus, add methenamine, stir; Wherein every milliliter of described liquor argenti nitratis ophthalmicus adds 0.005-0.01g methenamine;
3) continue to step 2) add phosphoric acid in gained solution, stir 5 minutes, obtain turbid solution, dry under turbid solution being carried out centrifugation, washing, 40-60 DEG C temperature, obtain tetrahedral silver phosphate; Wherein described in often liter of step 1), liquor argenti nitratis ophthalmicus adds 2.5-3.25ml phosphoric acid, and the concentration of described phosphoric acid is mass percent 85%.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103466584A (en) * | 2013-09-26 | 2013-12-25 | 新疆大学 | Method for preparing silver phosphate nanometer material by solid phase chemical reaction |
| CN104495777B (en) * | 2014-12-25 | 2018-05-18 | 盐城工学院 | Polyhedral silver phosphate nano material and preparation method thereof |
| CN105435823B (en) * | 2015-12-11 | 2017-08-25 | 华南理工大学 | A kind of granatohedron silver phosphate photocatalyst and preparation and application |
| CN107486225B (en) * | 2017-08-14 | 2020-02-21 | 北京化工大学 | Tetrahedral silver phosphate/graphene oxide composite material and preparation method thereof |
| CN109046406A (en) * | 2018-07-20 | 2018-12-21 | 长春工业大学 | A kind of preparation method of silver bromide compound phosphoric acid silver photochemical catalyst |
| CN113546657B (en) * | 2021-08-27 | 2023-05-23 | 陕西科技大学 | Ag (silver) alloy 3 PO 4 MXene composite photocatalyst and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009078211A (en) * | 2007-09-26 | 2009-04-16 | National Institute For Materials Science | Photocatalyst |
| CN101648139A (en) * | 2009-09-03 | 2010-02-17 | 福州大学 | Novel visible catalyst-silver phosphate and preparation method thereof |
| CN102698782A (en) * | 2012-06-25 | 2012-10-03 | 武汉理工大学 | Dendrite silver phosphate visible light catalyst and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009078211A (en) * | 2007-09-26 | 2009-04-16 | National Institute For Materials Science | Photocatalyst |
| CN101648139A (en) * | 2009-09-03 | 2010-02-17 | 福州大学 | Novel visible catalyst-silver phosphate and preparation method thereof |
| CN102698782A (en) * | 2012-06-25 | 2012-10-03 | 武汉理工大学 | Dendrite silver phosphate visible light catalyst and preparation method thereof |
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