CN103626146A - Preparation method of polyhedral silver phosphate - Google Patents
Preparation method of polyhedral silver phosphate Download PDFInfo
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- CN103626146A CN103626146A CN201310675938.9A CN201310675938A CN103626146A CN 103626146 A CN103626146 A CN 103626146A CN 201310675938 A CN201310675938 A CN 201310675938A CN 103626146 A CN103626146 A CN 103626146A
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Abstract
The invention relates to a preparation method of polyhedral silver phosphate and belongs to the technical field of photocatalysis. The preparation method comprises the following steps: firstly, mixing a silver nitrate aqueous solution and ammonia water to prepare an ammoniacal silver nitrate; uniformly mixing the ammoniacal silver nitrate and sodium dodecyl benzene sulfonate to form a first mixed solution; uniformly mixing a disodium hydrogen phosphate aqueous solution and sodium dodecyl benzene sulfonate to form a second mixed solution; under the stirring condition, dropwise adding the second mixed solution into the first mixed solution to obtain a yellow turbid solution; finally, after carrying out centrifugal washing on the yellow turbid solution, drying to obtain the polyhedral silver phosphate. The preparation method disclosed by the invention is simple; production can be carried out at room temperature; heating is not needed; the preparation method is energy-saving and environmental-friendly and is suitable for industrial production. The prepared silver phosphate is of a polyhedral shape, and has novel structure and high photocatalytic activity.
Description
Technical field
The invention belongs to photocatalysis technology field, be specifically related to the preparation method as the polyhedron Trisilver phosphate of photocatalyst.
Background technology
Environmental pollution is to affect one of focal issue of the mankind nowadays survival and development.Photocatalysis technology has the feature ， environmental pollution improvement aspects such as catalytic activity is high, good stability, environmental friendliness and has vast application prospect.It is than other technologies, and advantage is that reaction conditions is gentle, and photocatalytic degradation reaction is generally carried out at normal temperatures and pressures, and can thoroughly decompose the organic pollutant in air or in the aqueous solution, and making its mineralising is carbonic acid gas and water.
Titanium dioxide is the photocatalyst being most widely used at present, but due to its narrower photoresponse scope and lower quantum yield, causes it in industrial extensive popularization, to be subject to restriction.
2010 Nian Ye golden flower seminars report Ag on Nature Materials
3pO
4it is a kind of efficient novel photocatalysis material.Trisilver phosphate is yellow crystals, is cubic, and energy gap is 2.36eV, can absorbing wavelength be less than UV-light and the visible ray of 525nm.Under the irradiation of visible ray, show the ability of very strong oxidation and photocatalysis Decomposition organic dye.
The catalytic performance of photocatalyst largely depends on its physical properties, such as size, pattern, crystalline phase and degree of crystallinity etc.The particle radii of photocatalyst are less, and its specific surface area is just larger, thereby reaction area is just larger, and speed of reaction and efficiency are just higher; The particle radii of photocatalyst are less, and the recombination probability in electronics and hole is just less, and photocatalytic activity will be higher.The crystal formation of photocatalyst is different, and its catalytic activity is likely not identical yet; Crystal face difference can cause the exposure of catalyzing atom different, thereby causes the difference of its catalytic performance; Degree of crystallinity is higher, and its body phase defect is just fewer, and the probability of electronics and hole-recombination is just less, and photocatalytic activity is just higher.Therefore, the synthetic method of research Trisilver phosphate has important application value to the impact of crystal morphology, size.
Summary of the invention
The object of the invention is to provide that a kind of good stability, catalytic activity are high, the preparation method of the simple polyhedron Trisilver phosphate of method photocatalyst
The present invention includes following steps:
1) silver nitrate aqueous solution that is 0.1～1mol/L by concentration and ammoniacal liquor mix, and make silver ammino solution;
2) silver ammino solution and Sodium dodecylbenzene sulfonate are mixed, form the first mixed solution;
3) the Sodium phosphate dibasic aqueous solution and the Sodium dodecylbenzene sulfonate that by concentration, are 0.01～0.1mol/L mix, and form the second mixed solution;
4) under agitation condition, the second mixed solution is dripped in the first mixed solution, obtain yellow turbid solution;
5) by after yellow turbid solution centrifuge washing, at 40 ℃ of temperature, dry, obtain polyhedron Trisilver phosphate.
Preparation method of the present invention is simple, under room temperature, just can produce, and does not need heating, and energy-conserving and environment-protective, are suitable for suitability for industrialized production.The Trisilver phosphate light being prepared into, is polyhedral, novel structure, and photocatalytic activity is high.
For complete reaction, generate Trisilver phosphate, the molar ratio of Silver Nitrate of the present invention and SODIUM PHOSPHATE, MONOBASIC is 3:1.
The volume ratio that feeds intake of described silver ammino solution and biphosphate sodium water solution is 4:3.Under this ratio, could guarantee that the Trisilver phosphate pattern of making is polyhedron completely.
Constant in order to guarantee the concentration of the Sodium dodecylbenzene sulfonate in preparation process system, make more homogeneous of pattern, in step 4) of the present invention, the concentration of the Sodium dodecylbenzene sulfonate in the first mixed solution is identical with the concentration of Sodium dodecylbenzene sulfonate in described the second mixed solution.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope sem figure of the polyhedral structure Trisilver phosphate light made of the present invention.
Fig. 2 is the enlarged view of Fig. 1.
Fig. 3 is the X-ray diffraction XRD figure of the polyhedral structure Trisilver phosphate light made of the present invention.
Fig. 4 is polyhedron Trisilver phosphate and the business type N-TiO that the present invention makes
2as photocatalyst for degrading methylene blue experiment effect comparison diagram.
In Fig. 4: curve A is the methylene blue photodegradation situation of polyhedron Trisilver phosphate during as photocatalyst, and curve B is business type N-TiO
2methylene blue photodegradation situation during as photocatalyst, C
0for the starting point concentration of methylene blue, C
tfor the concentration of the methylene blue measured after visible ray (> 420nm) irradiation time t, t is the time of methylene blue solution illumination.
Embodiment
One, the preparation of Trisilver phosphate photocatalyst:
1, in ionized water, add Silver Nitrate, be mixed with the silver nitrate aqueous solution that concentration is 0.1～1mol/L.
2, get silver nitrate aqueous solution 100mL, dropwise add ammoniacal liquor, the vibration while dripping, until the initial precipitation generating is just dissolved, is mixed with silver ammino solution.Get 40mL silver ammino solution, add 0.01～1g Sodium dodecylbenzene sulfonate, stir, form the first mixed solution.Sodium dodecylbenzene sulfonate concentration in the first mixed solution is: 0.3～30g/L.
3, in ionized water, add Sodium phosphate dibasic, being mixed with concentration is the Sodium phosphate dibasic aqueous solution of 0.01～0.1mol/L.
4, get Sodium phosphate dibasic aqueous solution 30mL, add 0.01～1g Sodium dodecylbenzene sulfonate, stir, form the second mixed solution.Sodium dodecylbenzene sulfonate concentration in the second mixed solution is: 0.3～30g/L.
5, under agitation, the second mixed solution is dripped in the first mixed solution, obtain yellow turbid solution.Attention is got: the concentration of the Sodium dodecylbenzene sulfonate in the second mixed solution is identical with the concentration of Sodium dodecylbenzene sulfonate in the first mixed solution.
6, after yellow turbid solution is centrifugal, get solid phase, then use after deionized water and washing with alcohol 3 times, at 40 ℃ of temperature, dry, obtain polyhedron Trisilver phosphate.
Fig. 1 and Fig. 2 have shown the scanning electron microscope (SEM) photograph (SEM) of Trisilver phosphate prepared by the present invention, and as can be seen from the figure Trisilver phosphate is polyhedral, and size is between 1～2 μ m.
Fig. 3 has shown the X-ray diffractogram (XRD) of Trisilver phosphate prepared by the present invention, and as can be seen from the figure the Trisilver phosphate of preparation is pure phase.
Two, application---Trisilver phosphate photocatalytic degradation methylene blue:
Take aqueous solution of methylene blue as simulating pollution thing carries out photocatalytic activity evaluation, 0.05g catalyzer is added to 200mL methylene blue solution (1 * 10 is housed
-5mol/L) in glass reactor, dark adsorption 30min makes catalyst surface reach adsorption-desorption balance, take xenon lamp as light source 250W, use spectral filter to guarantee that incident light is visible ray, logical water of condensation guarantees that temperature of reaction is 20 ℃, after reaction starts, interval certain hour sampling, sample is through 10000r/min high speed centrifugation 2min, and the absorbancy of employing spectrophotometric determination wavelength 664nm place methylene blue detects the change in concentration of methylene blue.
As shown in Figure 4, the photocatalytic activity of polyhedron Trisilver phosphate (curve A) is than business type N-TiO
2photocatalytic activity (curve B) much higher.Adopt polyhedron Trisilver phosphate to make catalyzer, methylene blue solution is substantially degradable at 50min, and adopts business type N-TiO
2make catalyzer and only degraded 20%.Therefore, polyhedron Trisilver phosphate has efficient photocatalysis performance.
Claims (4)
1. a preparation method for polyhedron Trisilver phosphate, is characterized in that comprising the following steps:
1) silver nitrate aqueous solution that is 0.1～1mol/L by concentration and ammoniacal liquor mix, and make silver ammino solution;
2) silver ammino solution and Sodium dodecylbenzene sulfonate are mixed, form the first mixed solution;
3) the Sodium phosphate dibasic aqueous solution and the Sodium dodecylbenzene sulfonate that by concentration, are 0.01～0.1mol/L mix, and form the second mixed solution;
4) under agitation condition, the second mixed solution is dripped in the first mixed solution, obtain yellow turbid solution;
5) by after yellow turbid solution centrifuge washing, at 40 ℃ of temperature, dry, obtain polyhedron Trisilver phosphate.
2. the preparation method of polyhedron Trisilver phosphate according to claim 1, the molar ratio that it is characterized in that described Silver Nitrate and SODIUM PHOSPHATE, MONOBASIC is 3:1.
3. the preparation method of polyhedron Trisilver phosphate according to claim 1, is characterized in that the volume ratio that feeds intake of described silver ammino solution and biphosphate sodium water solution is 4:3.
4. the preparation method of polyhedron Trisilver phosphate according to claim 1, is characterized in that in described step 4), and the concentration of the Sodium dodecylbenzene sulfonate in the first mixed solution is identical with the concentration of Sodium dodecylbenzene sulfonate in described the second mixed solution.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103934009A (en) * | 2014-04-14 | 2014-07-23 | 扬州大学 | Preparation method of magnetic silver phosphate |
| CN107311135A (en) * | 2017-07-14 | 2017-11-03 | 华南师范大学 | A kind of preparation method of polypody shape phosphoric acid ag material |
| CN109806895A (en) * | 2019-03-01 | 2019-05-28 | 东华大学 | A kind of quadrangle claw-like silver phosphate photocatalyst and preparation method thereof |
| CN115090307A (en) * | 2022-08-08 | 2022-09-23 | 国能南京电力试验研究有限公司 | Silver phosphate composite photocatalyst and preparation method thereof |
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| 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 |
| CN102698781A (en) * | 2012-06-15 | 2012-10-03 | 桂林理工大学 | Method for preparing Ag/Ag3PO4 composite photo-catalyst |
| CN102826531A (en) * | 2012-09-14 | 2012-12-19 | 华东理工大学 | Preparation method of nano silver phosphate catalyst driven by visible light |
| CN102921438A (en) * | 2012-11-06 | 2013-02-13 | 武汉理工大学 | Preparation for silver phosphate nano ball-graphene composite material and photocatalysis application |
| CN102974374A (en) * | 2012-10-10 | 2013-03-20 | 江苏大学 | Silver phosphate/P25 bi-functional composite material, preparation method and application thereof |
| CN103272623A (en) * | 2013-06-20 | 2013-09-04 | 南京信息工程大学 | Preparation method of cubic silver phosphate photocatalyst |
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2013
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Patent Citations (7)
| 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 |
| CN102698781A (en) * | 2012-06-15 | 2012-10-03 | 桂林理工大学 | Method for preparing Ag/Ag3PO4 composite photo-catalyst |
| CN102826531A (en) * | 2012-09-14 | 2012-12-19 | 华东理工大学 | Preparation method of nano silver phosphate catalyst driven by visible light |
| CN102974374A (en) * | 2012-10-10 | 2013-03-20 | 江苏大学 | Silver phosphate/P25 bi-functional composite material, preparation method and application thereof |
| CN102921438A (en) * | 2012-11-06 | 2013-02-13 | 武汉理工大学 | Preparation for silver phosphate nano ball-graphene composite material and photocatalysis application |
| CN103272623A (en) * | 2013-06-20 | 2013-09-04 | 南京信息工程大学 | Preparation method of cubic silver phosphate photocatalyst |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103934009A (en) * | 2014-04-14 | 2014-07-23 | 扬州大学 | Preparation method of magnetic silver phosphate |
| CN103934009B (en) * | 2014-04-14 | 2016-04-13 | 扬州大学 | A kind of preparation method of magnetic silver orthophosphate |
| CN107311135A (en) * | 2017-07-14 | 2017-11-03 | 华南师范大学 | A kind of preparation method of polypody shape phosphoric acid ag material |
| 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 |
| CN109806895A (en) * | 2019-03-01 | 2019-05-28 | 东华大学 | A kind of quadrangle claw-like silver phosphate photocatalyst and preparation method thereof |
| CN115090307A (en) * | 2022-08-08 | 2022-09-23 | 国能南京电力试验研究有限公司 | Silver phosphate composite photocatalyst and preparation method thereof |
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Application publication date: 20140312 |