CN103990477B - The preparation method of a kind of silver orthophosphate/silver vanadate composite photo-catalyst - Google Patents
The preparation method of a kind of silver orthophosphate/silver vanadate composite photo-catalyst Download PDFInfo
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- CN103990477B CN103990477B CN201410259044.6A CN201410259044A CN103990477B CN 103990477 B CN103990477 B CN 103990477B CN 201410259044 A CN201410259044 A CN 201410259044A CN 103990477 B CN103990477 B CN 103990477B
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Abstract
The invention discloses the preparation method of a kind of silver orthophosphate/silver vanadate composite photo-catalyst, in turn include the following steps: be under agitation that to be added drop-wise to 50 ~ 100mL concentration be in the sodium hydroxide solution of 0.1 ~ 0.2mol/L for the silver nitrate of 0.2 ~ 0.4mol/L by 50 ~ 100mL concentration, after separation of supernatant, obtain silver oxide particle; By 2 ~ 3mmol? V
2o
5powder dissolution is that in the ammonia spirit of 20% ~ 25%, wherein ammoniacal liquor is excessive in 20 ~ 30mL mass percentage concentration, obtained Ammonium Vanadate Solution; Silver oxide particle is joined in Ammonium Vanadate Solution and stir 2 ~ 3h, then add sodium dihydrogen phosphate 25 ~ 50mL that concentration is 0.2 ~ 0.4mol/L, precipitate and separate, with distilled water washing 3 ~ 4 times, dry and get final product for 105 DEG C.The present invention, by silver orthophosphate and silver vanadate compound, is conducive to the transition of light induced electron, avoids compound, is conducive to improving catalytic efficiency.
Description
Technical field
The invention belongs to water treatment field, relate to the preparation method of a kind of silver orthophosphate/silver vanadate composite photo-catalyst, particularly relate to a kind of catalysis material for the treatment of organic wastewater and preparation method thereof.
Background technology
Current, with the develop rapidly of industrial technology, the water resource that the mankind depend on for existence is all subject to pollution in various degree, and water resource pollution has become the problem demanding prompt solution that countries in the world face.The existence of the pollutant in water, particularly toxic organic pollutant, not only causes environmental pollution, ecological disruption, and serious harm human health.These organic pollutions comprise polycyclic aromatic hydrocarbon, Polychlorinated biphenyls, agricultural chemicals, environmental disturbances element, dyestuff etc.
Silver vanadate is that a class has visible light-responded novel photocatalyst, and its monoclinic phase energy gap, lower than 2.7eV, has higher visible light-responded, and stable in properties, become study hotspot in recent years.Silver vanadate has multiple preparation method, as solid-phase synthesis, coprecipitation, chemical deposition, metalorganic decomposition, hydro-thermal method, sonochemical method etc.In June, 2010, material research institution researcher finds that silver orthophosphate has the effect of photochemical catalyst, and photooxidation effect is more than the decades of times of current known various photochemical catalyst.But because silver orthophosphate self is unstable, in photocatalysis, easy self-reversal, causes catalyst degradation performance to reduce rapidly.
Composite catalyst is conducive to electron transition, form free radical at catalyst surface and improve catalytic efficiency, but, usually the semi-conducting material obtained is nano-powder, when it uses in liquid-phase system, less nanoparticle suspension not free settling in the solution, is difficult to separation and recovery, is unfavorable for that recirculation is reused.In addition, the poor stability of composite catalyst, crystal growth difficulty, particle diameter and load capacity wayward, be difficult to reach long catalysis requirement, affect and limit its practical application in industrial production.
Summary of the invention
The object of the invention is for overcoming the deficiencies in the prior art, the preparation method of a kind of silver orthophosphate/silver vanadate composite photo-catalyst is provided.
Object of the present invention can be achieved through the following technical solutions:
The preparation method of a kind of silver orthophosphate/silver vanadate composite photo-catalyst adopts following methods to obtain:
1) be under agitation that to be added drop-wise to 50 ~ 100mL concentration be in the sodium hydroxide solution of 0.1 ~ 0.2mol/L for the silver nitrate of 0.2 ~ 0.4mol/L by 50 ~ 100mL concentration, after separation of supernatant, obtain silver oxide particle;
2) by 2 ~ 3mmolV
2o
5powder dissolution is that in the ammonia spirit of 20% ~ 25% (mass percentage concentration), wherein ammoniacal liquor is excessive in 20 ~ 30mL concentration, obtained Ammonium Vanadate Solution;
3) silver oxide particle is joined in Ammonium Vanadate Solution, stir 2 ~ 3h, then add sodium dihydrogen phosphate 25 ~ 50mL that concentration is 0.2 ~ 0.4mol/L, precipitate and separate, with distilled water washing 3 ~ 4 times, 105 DEG C of oven dry, i.e. obtained a kind of silver orthophosphate/silver vanadate composite photo-catalyst.
The invention has the beneficial effects as follows:
1, utilize ammonia solvent vanadic anhydride to form vanadate in building-up process, utilize ammoniacal liquor and silver oxide reaction to form complex silver simultaneously, then react with phosphate radical, form compound phosphoric acid silver/silver vanadate composite catalyst.
2, by silver orthophosphate and silver vanadate compound, be conducive to the transition of light induced electron, avoid compound, be conducive to improving catalytic efficiency.
Detailed description of the invention
Embodiment 1
Be under agitation that to be added drop-wise to 100mL concentration be in the sodium hydroxide solution of 0.1mol/L for the silver nitrate of 0.2mol/L by 100mL concentration, after separation of supernatant, obtain silver oxide particle; By 3mmolV
2o
5powder dissolution is that in the ammonia spirit of 25% (mass percentage concentration), wherein ammoniacal liquor is excessive in 30mL concentration, obtained Ammonium Vanadate Solution; Joined by silver oxide particle in Ammonium Vanadate Solution, stir 3h, then add the sodium dihydrogen phosphate 25mL that concentration is 0.4mol/L, precipitate and separate, washs 4 times with distilled water, 105 DEG C of oven dry, i.e. obtained a kind of silver orthophosphate/silver vanadate composite photo-catalyst.
Being joined by the silver orthophosphate obtained/silver vanadate composite photo-catalyst and 100mL concentration is housed is in the OrangeII waste water of 30mg/L, and under 300w iodine-tungsten lamp irradiates, react 40 minutes, percent of decolourization is 95.9%.The silver vanadate percent of decolourization at identical conditions of equal in quality is only 56.2%.
Embodiment 2
Be under agitation that to be added drop-wise to 50mL concentration be in the sodium hydroxide solution of 0.2mol/L for the silver nitrate of 0.4mol/L by 50mL concentration, after separation of supernatant, obtain silver oxide particle; By 2mmolV
2o
5powder dissolution is that in the ammonia spirit of 20% (mass percentage concentration), wherein ammoniacal liquor is excessive in 20mL concentration, obtained Ammonium Vanadate Solution; Joined by silver oxide particle in Ammonium Vanadate Solution, stir 2h, then add the sodium dihydrogen phosphate 50mL that concentration is 0.2mol/L, precipitate and separate, washs 3 times with distilled water, 105 DEG C of oven dry, i.e. obtained a kind of silver orthophosphate/silver vanadate composite photo-catalyst.
Being joined by the silver orthophosphate obtained/silver vanadate composite photo-catalyst and 100mL concentration is housed is in the OrangeII waste water of 30mg/L, and under 300w iodine-tungsten lamp irradiates, react 40 minutes, percent of decolourization is 94.7%.
Embodiment 3
Be under agitation that to be added drop-wise to 90mL concentration be in the sodium hydroxide solution of 0.1mol/L for the silver nitrate of 0.3mol/L by 60mL concentration, after separation of supernatant, obtain silver oxide particle; By 3mmolV
2o
5powder dissolution is that in the ammonia spirit of 25% (mass percentage concentration), wherein ammoniacal liquor is excessive in 20mL concentration, obtained Ammonium Vanadate Solution; Joined by silver oxide particle in Ammonium Vanadate Solution, stir 3h, then add the sodium dihydrogen phosphate 33mL that concentration is 0.3mol/L, precipitate and separate, washs 4 times with distilled water, 105 DEG C of oven dry, i.e. obtained a kind of silver orthophosphate/silver vanadate composite photo-catalyst.
Being joined by the silver orthophosphate obtained/silver vanadate composite photo-catalyst and 100mL concentration is housed is in the methylene blue waste water of 30mg/L, and under 300w iodine-tungsten lamp irradiates, react 40 minutes, percent of decolourization is 94.9%.
Claims (1)
1. a preparation method for silver orthophosphate/silver vanadate composite photo-catalyst, is characterized in that in turn including the following steps:
1) be under agitation that to be added drop-wise to 50 ~ 100mL concentration be in the sodium hydroxide solution of 0.1 ~ 0.2mol/L for the silver nitrate of 0.2 ~ 0.4mol/L by 50 ~ 100mL concentration, after separation of supernatant, obtain silver oxide particle;
2) by 2 ~ 3mmolV
2o
5powder dissolution is that in the ammonia spirit of 20% ~ 25% (mass percentage concentration), wherein ammoniacal liquor is excessive in 20 ~ 30mL concentration, obtained Ammonium Vanadate Solution;
3) silver oxide particle is joined in Ammonium Vanadate Solution, stir 2 ~ 3h, then add sodium dihydrogen phosphate 25 ~ 50mL that concentration is 0.2 ~ 0.4mol/L, precipitate and separate, with distilled water washing 3 ~ 4 times, 105 DEG C of oven dry, i.e. obtained a kind of silver orthophosphate/silver vanadate composite photo-catalyst.
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| CN103990477B true CN103990477B (en) | 2015-12-30 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103990457B (en) * | 2014-06-11 | 2015-12-09 | 常州大学 | The preparation method of a kind of silver/silver vanadate composite photo-catalyst |
| CN105478749B (en) * | 2015-12-17 | 2018-03-02 | 中南大学 | A kind of Ag/ α AgVO3Overlong nanowire composite and preparation method thereof |
| CN114917903B (en) * | 2022-05-27 | 2023-03-17 | 福州大学 | Preparation and application of silver metavanadate thin-film photocatalyst |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4137259A (en) * | 1976-07-09 | 1979-01-30 | Stamicarbon, B.V. | Catalytic gas phase oxidation of toluene to benzaldehyde and/or benzoic acid |
| CN102500371A (en) * | 2011-10-18 | 2012-06-20 | 山东大学 | Visible light response photocatalysis material Ag@Ag3VO4 and preparation method thereof |
| CN102600869A (en) * | 2012-02-23 | 2012-07-25 | 常州水木环保科技有限公司 | Synthetic method of supported silver phosphate photocatalyst |
| CN103990457A (en) * | 2014-06-11 | 2014-08-20 | 常州大学 | Preparation method of silver/silver vanadate composite photocatalyst |
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2014
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4137259A (en) * | 1976-07-09 | 1979-01-30 | Stamicarbon, B.V. | Catalytic gas phase oxidation of toluene to benzaldehyde and/or benzoic acid |
| CN102500371A (en) * | 2011-10-18 | 2012-06-20 | 山东大学 | Visible light response photocatalysis material Ag@Ag3VO4 and preparation method thereof |
| CN102600869A (en) * | 2012-02-23 | 2012-07-25 | 常州水木环保科技有限公司 | Synthetic method of supported silver phosphate photocatalyst |
| CN103990457A (en) * | 2014-06-11 | 2014-08-20 | 常州大学 | Preparation method of silver/silver vanadate composite photocatalyst |
Non-Patent Citations (1)
| Title |
|---|
| Interaction of Ag ion with a vanadium pentoxide hydrate-Formation of silver vanadate at low temperature;S.Kittaka等;《Journal of Material Science》;20001231;第2000卷(第35期);2185-2192 * |
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