CN102600870B - Loaded type silver phosphate/polyphosphoric silver/silver chloride compound water treatment photo-catalyst and preparation method thereof - Google Patents
Loaded type silver phosphate/polyphosphoric silver/silver chloride compound water treatment photo-catalyst and preparation method thereof Download PDFInfo
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- CN102600870B CN102600870B CN201210065515.0A CN201210065515A CN102600870B CN 102600870 B CN102600870 B CN 102600870B CN 201210065515 A CN201210065515 A CN 201210065515A CN 102600870 B CN102600870 B CN 102600870B
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Abstract
The invention discloses a loaded type silver phosphate/polyphosphoric silver/silver chloride compound water treatment photo-catalyst and a preparation method thereof. The preparation method comprises the following steps of: 1) weighting NaCl, grinding and then adding H3PO4 solution while severely stirring, and continuously stirring; 2) dropwise adding AgNO3 solution into the solution prepared in the step 1, continuously stirring while dropwise adding, stirring again after finishing dropwise adding, and then depositing and ageing; and 3) washing the obtained precipitate with deionized water, and drying, thereby obtaining the loaded type silver phosphate/polyphosphoric silver/silver chloride photo-catalyst. According to the preparation method provided by the invention, the strong complexing action of polyphosphates on metal is utilized to efficiently avoid the self-etching of silver phosphate; the visible photo-catalytic characteristic of the catalyst is efficiently utilized to prolong the service life of the catalyst and accelerate the decomposition on organic matters; and the silver phosphate, the silver chloride and the polyphosphoric silver are compounded together, thereby being beneficial to the synergistic effect and promoting the photo-degrading efficiency.
Description
Technical field
The present invention relates to a kind of support type silver orthophosphate/polyphosphoric acids silver/silver chlorate water treatment photochemical catalyst and preparation method thereof, belong to technical field of sewage in environmental protection.
Background technology
Traditional method for treating water efficiency is low, cost is high, have secondary pollution problems, the solution that waste water control can not get always.The development of nanometer technology and application probably thoroughly solve this difficult problem.1972, A.Fujishima and K.Honda were at N-shaped semiconductor TiO
2on electrode, found the photoelectrocatalysis decomposition of water, TiO
2oxidation activity is higher, and chemical stability is good, and to human body nonhazardous, cost is low, pollution-free, applied range, thereby paid attention to most, be current most widely used nano-photocatalyst material, be also the environmental type catalyst with exploitation future.But TiO
2large (the anatase TiO for example of energy gap
2energy gap Eg=3.2eV), only can absorb the light of ultraviolet region (wavelength is less than 387nm), lower to the utilization ratio of solar energy.
In June, 2010, the researcher of material research institution finds that silver orthophosphate has the effect of photochemical catalyst, and photooxidation effect is more than the decades of times of known various photochemical catalysts at present.But because silver orthophosphate self is unstable, easily self-reversal in photocatalysis.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, provide a kind of support type silver orthophosphate/polyphosphoric acids silver/silver chlorate Compound Water to process photochemical catalyst.The method is that silver orthophosphate/polyphosphoric acids silver/silver chlorate is combined with each other, and has extended the service life of silver orthophosphate, has accelerated contaminant degradation.
Another object of the present invention is to provide a kind of support type silver orthophosphate/polyphosphoric acids silver/silver chlorate Compound Water to process the preparation method of photochemical catalyst.
The technical scheme that object of the present invention adopts realizes:
Support type silver orthophosphate/polyphosphoric acids silver/silver chlorate Compound Water is processed a photochemical catalyst, and it is to obtain by following steps: 1) take NaCl, join the H that concentration is 1～2mol/L after grinding under vigorous stirring
3pO
4in solution, continue to stir 30～40min, described NaCl and H
3pO
4the molal volume of solution is 1～2: 3～4 than mol: L; 2) to step 1) prepare and in solution, drip the AgNO that concentration is 1～2mol/L
3solution, continues during dropping to stir, and is added dropwise to complete and stirs 60～70min again, then precipitation aging 20～30h; Step 1) H in
3pO
4solution and step 2) in AgNO
3the volume ratio of solution is 3～4: 2～4; 3) by the sediment obtaining with after washed with de-ionized water, dry, obtain support type silver orthophosphate/polyphosphoric acids silver/silver chlorate Compound Water and process photochemical catalyst.Mixing speed during vigorous stirring is 320～400 revs/min; In other situations, mixing speed remains on 100～300 revs/min.
Above-mentioned support type silver orthophosphate/polyphosphoric acids silver/silver chlorate Compound Water is processed photochemical catalyst, and it is that it is 100～300 μ m that described NaCl is ground to particle diameter.
Above-mentioned support type silver orthophosphate/polyphosphoric acids silver/silver chlorate Compound Water is processed photochemical catalyst, and it is step 2) also the aging time is 24h to middle precipitation; Step 3) in by washed with de-ionized water 4～5 times for the sediment that obtains.
Support type silver orthophosphate/polyphosphoric acids silver/silver chlorate Compound Water is processed a preparation method for photochemical catalyst, and it is to comprise the following steps: 1) take NaCl, join the H that concentration is 1～2mol/L after grinding under vigorous stirring
3pO
4in solution, continue to stir 30～40min, described NaCl and H
3pO
4the molal volume of solution is than (mol: be L) 1～2: 3～4; 2) to step 1) prepare and in solution, drip the AgNO that concentration is 1～2mol/L
3solution, continues during dropping to stir, and is added dropwise to complete and stirs 60～70min again, then precipitation aging 20～30h; Step 1) H in
3pO
4solution and step 2) in AgNO
3the volume ratio of solution (L: be L) 3～4: 2～4; 3) by the sediment obtaining with after washed with de-ionized water, dry, obtain support type silver orthophosphate/polyphosphoric acids silver/silver chlorate Compound Water and process photochemical catalyst.Mixing speed during vigorous stirring is 320～400 revs/min; In other situations, mixing speed remains on 100～300 revs/min.
Above-mentioned support type silver orthophosphate/polyphosphoric acids silver/silver chlorate Compound Water is processed the preparation method of photochemical catalyst, and it is that it is 100～300 μ m that described NaCl is ground to particle diameter.
Above-mentioned support type silver orthophosphate/polyphosphoric acids silver/silver chlorate Compound Water is processed the preparation method of photochemical catalyst, and it is step 2) also the aging time is 24h to middle precipitation; Step 3) in by washed with de-ionized water 4～5 times for the sediment that obtains.
The present invention utilizes the strong complexing of Quadrafos to metal, can effectively avoid the self-reversal of silver orthophosphate, can effectively utilize its visible light catalytic characteristic again, accelerates organic decomposition.
The invention has the beneficial effects as follows:
(1) NaCl adds in phosphoric acid solution after grinding, and can impel phosphoric acid that party reaction occurs, but this reaction is not thorough, so can there is polyphosphoric acid (P in solution
2o
7 4-, P
3o
9 3-) also there is orthophosphoric acid (PO
4 3-), then add silver nitrate, can obtain compound phosphoric acid silver/polyphosphoric acids silver/silver chlorate photochemical catalyst.(2) silver orthophosphate, silver chlorate and polyphosphoric acids silver are combined with each other and are conducive to synergy, promote the disposal efficiency.(3) polyphosphoric acids silver and silver orthophosphate are combined with each other and can utilize the strong complexing of polyphosphoric acids silver, reduce silver-coloredly in degree of corrosion, have extended the life-span of catalyst.
The specific embodiment
Embodiment 1
Take 1mol NaCl, be ground to particle diameter 100 μ m, under vigorous stirring (350 revs/min), joining volume is 3L, the H that concentration is 1mol/L
3pO
4in solution, continue to stir (200 revs/min) 30min; In above-mentioned solution, drip the AgNO that concentration is 1mol/L
32L, continues during dropping to stir altogether, is added dropwise to complete and stirs 60min again, precipitation aging 24h; By the sediment obtaining washed with de-ionized water 4 times, dry, obtain support type silver orthophosphate/polyphosphoric acids silver/silver chlorate Compound Water and process photochemical catalyst.
The silver orthophosphate obtaining/polyphosphoric acids silver/silver chlorate photochemical catalyst 0.1g is joined in the Orange II waste water that 500mL concentration is 30mg/L, under 500w Metal halogen lamp irradiates, reaction 20min, percent of decolourization is 98.8%, reusing after 6 times, is 90.5% to the percent of decolourization of Orange II.
Embodiment 2
Take 2mol NaCl, be ground to particle diameter 300 μ m, under vigorous stirring (350 revs/min), joining volume is 4L, the H that concentration is 2mol/L
3pO
4in solution, continue to stir (200 revs/min) 40min; In above-mentioned solution, drip the AgNO that concentration is 2mol/L
34L, continues during dropping to stir altogether, is added dropwise to complete and stirs 70min again, precipitation aging 24h; By the sediment obtaining washed with de-ionized water 5 times, dry, obtain support type silver orthophosphate/polyphosphoric acids silver/silver chlorate Compound Water and process photochemical catalyst.
The silver orthophosphate obtaining/polyphosphoric acids silver/silver chlorate photochemical catalyst 0.1g is joined in the Methyl Orange in Wastewater that 500mL concentration is 20mg/L, under 500w Metal halogen lamp irradiates, reaction 20min, percent of decolourization is 97.6%, reusing after 6 times, is 91.5% to the percent of decolourization of methyl orange.
Embodiment 3
Take 2molNaCl, be ground to particle diameter 300 μ m, under vigorous stirring (350 revs/min), joining volume is 3L, the H that concentration is 2mol/L
3pO
4in solution, continue to stir (200 revs/min) 40min; In above-mentioned solution, drip the AgNO that concentration is 2mol/L
33L, continues during dropping to stir altogether, is added dropwise to complete and stirs 70min again, precipitation aging 24h; By the sediment obtaining washed with de-ionized water 5 times, dry, obtain support type silver orthophosphate/polyphosphoric acids silver/silver chlorate Compound Water and process photochemical catalyst.
The silver orthophosphate obtaining/polyphosphoric acids silver/silver chlorate photochemical catalyst 0.1g is joined in the acid scarlet waste water that 500mL concentration is 20mg/L, under 500w Metal halogen lamp irradiates, reaction 20min, percent of decolourization is 99.8%, reusing after 6 times, is 91.9% to the percent of decolourization of acid scarlet.
Claims (6)
1. silver orthophosphate/polyphosphoric acids silver/silver chlorate Compound Water is processed a photochemical catalyst, it is characterized in that obtaining by following steps:
1) take NaCl, after grinding, under vigorous stirring, join the H that concentration is 1 ~ 2 mol/L
3pO
4in solution, continue to stir 30 ~ 40 min, described NaCl and H
3pO
4the molal volume of solution is 1 ~ 2:3 ~ 4 than mol:L;
2) to step 1), prepare and in solution, drip the AgNO that concentration is 1 ~ 2 mol/L
3solution, continues during dropping to stir, and is added dropwise to complete and stirs 60 ~ 70 min again, then precipitation aging 20 ~ 30h; H in step 1)
3pO
4solution and step 2) in AgNO
3the volume ratio of solution is 3 ~ 4:2 ~ 4;
3) by the sediment obtaining with after washed with de-ionized water, dry, obtain silver orthophosphate/polyphosphoric acids silver/silver chlorate Compound Water and process photochemical catalyst.
2. silver orthophosphate according to claim 1/polyphosphoric acids silver/silver chlorate Compound Water is processed photochemical catalyst, it is characterized in that it is 100 ~ 300 μ m that described NaCl is ground to particle diameter.
3. silver orthophosphate according to claim 1/polyphosphoric acids silver/silver chlorate Compound Water is processed photochemical catalyst, it is characterized in that step 2) also the aging time is 24h to middle precipitation; In step 3) by washed with de-ionized water 4 ~ 5 times for the sediment that obtains.
4. silver orthophosphate/polyphosphoric acids silver/silver chlorate Compound Water is processed a preparation method for photochemical catalyst, it is characterized in that comprising the following steps:
1) take NaCl, after grinding, under vigorous stirring, join the H that concentration is 1 ~ 2 mol/L
3pO
4in solution, continue to stir 30 ~ 40 min, described NaCl and H
3pO
4the molal volume of solution is 1 ~ 2:3 ~ 4 than mol:L;
2) to step 1), prepare and in solution, drip the AgNO that concentration is 1 ~ 2 mol/L
3solution, continues during dropping to stir, and is added dropwise to complete and stirs 60 ~ 70 min again, then precipitation aging 20 ~ 30h; H in step 1)
3pO
4solution and step 2) in AgNO
3the volume ratio of solution is 3 ~ 4:2 ~ 4;
3) by the sediment obtaining with after washed with de-ionized water, dry, obtain silver orthophosphate/polyphosphoric acids silver/silver chlorate Compound Water and process photochemical catalyst.
5. silver orthophosphate according to claim 4/polyphosphoric acids silver/silver chlorate Compound Water is processed the preparation method of photochemical catalyst, it is characterized in that it is 100 ~ 300 μ m that described NaCl is ground to particle diameter.
6. silver orthophosphate according to claim 4/polyphosphoric acids silver/silver chlorate Compound Water is processed the preparation method of photochemical catalyst, it is characterized in that step 2) also the aging time is 24h to middle precipitation; In step 3) by washed with de-ionized water 4 ~ 5 times for the sediment that obtains.
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| CN103028428B (en) * | 2013-01-16 | 2014-09-10 | 华东理工大学 | Method for preparing composite visual light catalytic material Ag3PO4 and g-C3N4 |
| CN104549387A (en) * | 2015-02-03 | 2015-04-29 | 苏州德捷膜材料科技有限公司 | Preparation method and application of catalyst of novel light degradation phosphate organic dye |
| CN106807414A (en) * | 2017-01-06 | 2017-06-09 | 华南理工大学 | A kind of silver orthophosphate/bromination silver/carbon nanotube composite photo-catalyst and preparation and application |
| US11207435B2 (en) * | 2018-01-31 | 2021-12-28 | Sensor Electronic Technology, Inc. | Humidifier disinfection using ultraviolet light |
| CN108325542B (en) * | 2018-02-02 | 2020-12-08 | 华北理工大学 | Net-shaped Ag/Ag3PO4Synthetic method of/AgCl composite photocatalytic material |
| CN115069302B (en) * | 2022-07-20 | 2023-05-09 | 江苏农林职业技术学院 | Efficient visible light catalytic material and preparation method and application thereof |
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| CN102247874A (en) * | 2011-05-26 | 2011-11-23 | 上海电力学院 | Silver chloride-silver phosphate composite photocatalyst and preparation method thereof |
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| CN102247874A (en) * | 2011-05-26 | 2011-11-23 | 上海电力学院 | Silver chloride-silver phosphate composite photocatalyst and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| Doan Pham Minh et al.,.One-step synthesis of sodium trimetaphosphate(Na3P3O9) from sodium chloride and orthophosphoric acid.《Industrial Engineering chemistry research》.2012,第51卷3851-3854. * |
| One-step synthesis of sodium trimetaphosphate(Na3P3O9) from sodium chloride and orthophosphoric acid;Doan Pham Minh et al.,;《Industrial Engineering chemistry research》;20120212;第51卷;3851-3854 * |
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