CN101648139A - Novel visible catalyst-silver phosphate and preparation method thereof - Google Patents

Novel visible catalyst-silver phosphate and preparation method thereof Download PDF

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Publication number
CN101648139A
CN101648139A CN200910306562A CN200910306562A CN101648139A CN 101648139 A CN101648139 A CN 101648139A CN 200910306562 A CN200910306562 A CN 200910306562A CN 200910306562 A CN200910306562 A CN 200910306562A CN 101648139 A CN101648139 A CN 101648139A
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silver
preparation
concentration
solution
catalyst
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CN101648139B (en
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付贤智
苏文悦
刘长安
刘平
戴文新
李朝晖
陈旬
王绪绪
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Fuzhou University
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Fuzhou University
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Abstract

The present invention provides a novel visible catalyst-silver phosphate and a preparation method thereof, solving the problems of wide TiO2 forbidden band, no absorbability of visible weakness, and the like in the prior art and applying Ag3PO4 to the field of photocatalysis for the first time. In the invention, a silver ammonia solution for replacing a silver nitrate solution is used as a silversource, the reaction of silver ions and phosphate ions is slowed, and then the catalyst is obtained and has the effect of high-efficiency photocatalytic degradation. The preparing method of the invention is simple and is favorable to extensive popularization.

Description

Novel visible catalyst-silver phosphate and preparation method thereof
Technical field
The invention belongs to the photocatalysis technology in the environmental improvement, specifically is a kind of novel visible catalyst-silver phosphate and preparation method thereof.
Technical background
Utilizing photocatalysis elimination and degradation of contaminant is one of current most active research field, and people have researched and developed many semiconductor light-catalysts.Wherein, nano-TiO 2Inexpensive, nontoxic with it, stability is high, catalytic performance is good, can recycling etc. advantage, obtained extensive concern.But because Detitanium-ore-type TiO 2, the energy gap broad, need under the exciting of the ultraviolet light of λ＜387.5nm, could to show catalytic activity, and the energy in sunshine medium ultraviolet light district is less than 5% of gross energy, and the lower visible light of energy accounts for the major part of gross energy.Therefore, the development of new visible-light photocatalyst is expanded the wave-length coverage that sunshine absorbs, and improves solar energy utilization ratio, becomes the focus direction of present photocatalysis research.
Summary of the invention
The purpose of this invention is to provide a kind of novel visible catalyst Ag 3PO 4And preparation method thereof, the present invention solves TiO in the prior art 2Energy gap greatly, does not absorb the problems such as weakness of visible light, with Ag 3PO 4Be applied to photocatalysis field, and the preparation method is simple, do not need cost and complex equipment, the synthesis condition gentleness.
Novel visible catalyst Ag of the present invention 3PO 4, it is characterized in that: described catalyst is non-TiO2 catalyst, is a kind of novel visible light catalyst.
Novel visible catalyst Ag of the present invention 3PO 4The preparation method, it is characterized in that: described Preparation of catalysts step was divided into for two steps: step (1): the preparation of silver ammino solution; Step (2): in silver ammino solution, add NaH 2PO 4, make Ag 3PO 4Catalyst.
Remarkable advantage of the present invention is:
The present invention is first with Ag 3PO 4Be applied to photocatalysis field, its energy gap is less, can absorb visible light, is a kind of novel visible light catalyst, can carry out light-catalyzed reaction efficiently.
The present invention has replaced the silver-colored source of liquor argenti nitratis ophthalmicus as the preparation photochemical catalyst with silver ammino solution in preparation process, the speed of silver ion and the phosphate radical reaction of having slowed down can obtain the little Ag of particle 3PO 4, help Ag 3PO 4The raising of photocatalytic activity.
Preparation method of the present invention is simple, helps large-scale popularization.
Description of drawings:
Fig. 1 is Ag of the present invention 3PO 4X-ray diffraction (XRD) figure.
Fig. 2 is Ag of the present invention 3PO 4Ultraviolet-visible diffuse reflection figure.
Fig. 3 is Ag of the present invention 3PO 4As the photocatalytic degradation rhodamine B, curve a is the rhodamine B light degradation situation when not having catalyst, curve b is the light degradation situation of rhodamine B when photochemical catalyst is arranged.
The specific embodiment
Preparation process of the present invention is as follows:
(1) preparation process of silver ammino solution is: 0.05-0.50mol silver nitrate solid is dissolved in the 200mL deionized water, stirred 10 minutes, obtain the liquor argenti nitratis ophthalmicus that 200mL concentration is 0.25-2.5mol/L; Other gets the concentrated ammonia liquor that 1～10mL concentration is 25.0w%, add deionized water and be diluted to 50mL, the ammonia spirit that makes is slowly splashed in the above-mentioned liquor argenti nitratis ophthalmicus, when the color of solution just becomes colorless, stop to drip, continue to stir 10 minutes, obtain the silver ammino solution that water white concentration is 0.2～2.0mol/L;
(2) 0.02～0.2mol sodium dihydrogen phosphate solid is dissolved in the 100mL deionized water, stirred 10 minutes, obtain sodium dihydrogen phosphate that 100ml concentration is 0.2～2.0mol/L and it is transferred in the dropping funel, the 250mL concentration that splashes into above-mentioned gained slowly is in the silver ammino solution of 0.2～2.0mol/L, obtain yellow turbid solution, dropwise the back and continue to stir 56 hours, turbid solution is centrifugal, washing, 60 ℃ of oven dry, grind the silver orthophosphate powder that obtains yellow.
In above-mentioned course of reaction, the mol ratio of the biphosphate sodium content in the sodium dihydrogen phosphate and the silver-colored ammonia content of silver ammino solution is 3.
Below be several embodiments of the present invention, further specify the present invention, but the present invention is not limited only to this.
Embodiment 1
The preparation of novel visible catalyst
Take by weighing 0.15mol AgNO 3Solid is dissolved in the deionized water of 200mL, stirs 10 minutes, obtains AgNO 3Solution; Measure 3mL concentrated ammonia liquor (25%) with pipette in addition and add the dilution of 47ml deionized water, splash into above-mentioned AgNO after stirring slowly 3Solution dropwises the back and continues to stir 10 minutes, obtains water white silver ammino solution.Other takes by weighing 0.05mol NaH 2PO 4Solid is dissolved in the 100mL deionized water, stirs 10 minutes, obtains NaH 2PO 4Solution is also transferred to it in dropping funel, and control rate of addition (2-3 second one) is added drop-wise to above-mentioned silver ammino solution slowly, dropwises and continues to stir 5-6 hour, the yellow turbid solution of gained is centrifugal, washing, 60 ℃ of oven dry, grinds the Ag that obtains yellow 3PO 4Powder.Fig. 1 has showed novel visible catalyst Ag of the present invention 3PO 4X-ray diffraction (XRD) figure, from figure, can find the Ag for preparing 3PO 4Be pure phase.Fig. 2 has showed novel visible catalyst Ag of the present invention 3PO 4UV, visible light diffuse reflection figure, Ag as can be seen from FIG. 3PO 4The absorption band edge be 506nm, being open to the custom and calculating energy gap is 2.45eV, is that yellow is consistent with the color of sample, can effectively absorb visible light.Therefore, Ag 3PO 4Can regard a kind of novel visible light catalyst.
Embodiment 2
Novel visible catalyst Ag 3PO 4The degraded rhodamine B
With the Ag that obtains 3PO 4Powder takes by weighing the 80mg sample and adds 80mL RhB solution (10-5mol/L) as the photocatalyst for degrading rhodamine B, and lucifuge stirs 1h, makes RhB solution reach absorption/desorption balance at catalyst surface.Open light source then and carry out light-catalyzed reaction, get the 3mL reactant liquor every 5min, after centrifugation, supernatant detects with Cary-500 type spectrophotometer.554nm place light absorption value is determined RhB change in concentration in the degradation process per sample.The radiance of reaction is for placing the 500W halogen tungsten lamp of two glass jacket (logical condensed water), uses optical filter to be visible light (420nm＜λ＜800nm) to guarantee incident light.The degraded situation of RhB as shown in Figure 3, as can be seen when not adding catalyst, rhodamine B is not degraded (curve a), and when catalyst was arranged, rhodamine B is degraded (curve b) substantially fully behind illumination 15min substantially from the figure.Therefore, Ag 3PO 4Has photocatalysis performance efficiently.

Claims (8)

1. novel visible catalyst-silver phosphate, it is characterized in that: described silver orthophosphate photochemical catalyst is non-TiO 2Catalyst.
2. the preparation method of a photochemical catalyst silver orthophosphate as claimed in claim 1, it is characterized in that: being prepared as of described silver orthophosphate adds sodium dihydrogen phosphate in silver ammino solution, make the silver orthophosphate catalyst.
3. the preparation method of photochemical catalyst silver orthophosphate according to claim 2 is characterized in that: described preparation method's step is as follows:
(1) preparation process of silver ammino solution is: the silver nitrate solid is dissolved in the deionized water, stirred 10 minutes, obtaining concentration is the 0.025-0.25mol/L liquor argenti nitratis ophthalmicus; The dilute ammonia solution of getting concentration and be 0.5-5.0wt% slowly splashes in the above-mentioned liquor argenti nitratis ophthalmicus, when the color of solution just becomes colorless, stops to drip, and continues to stir 10 minutes, obtains the silver ammino solution that water white concentration is 0.2～2.0mol/L; Dropwise 5 0ml dilute ammonia solution in described every 200ml liquor argenti nitratis ophthalmicus;
(2) the sodium dihydrogen phosphate solid is dissolved in the deionized water, stirred 10 minutes, obtain sodium dihydrogen phosphate that concentration is 0.2～2.0mol/L and it is transferred in the dropping funel, the concentration that splashes into step (1) gained slowly is in the silver ammino solution of 0.2～2.0mol/L, obtain yellow turbid solution, dropwise the back and continue to stir 5-6 hour, turbid solution is centrifugal, washing, 60 ℃ of oven dry, grindings obtain the described silver orthophosphate of yellow powder; Drip the described silver ammino solution of 250mL in the sodium dihydrogen phosphate of described every 100ml.
4. the preparation method of photochemical catalyst silver orthophosphate according to claim 3, it is characterized in that: being prepared as of described liquor argenti nitratis ophthalmicus: 0.05-0.50mol silver nitrate solid is dissolved in the 200mL deionized water, stirred 10 minutes, and obtained the liquor argenti nitratis ophthalmicus that 200mL concentration is 0.25-2.5mol/L.
5. the preparation method of photochemical catalyst silver orthophosphate according to claim 3 is characterized in that: being prepared as of the dilute ammonia solution of described 0.5-5.0wt%: get the concentrated ammonia liquor that 1～10mL concentration is 25.0wt%, add deionized water and be diluted to 50mL.
6. the preparation method of photochemical catalyst silver orthophosphate according to claim 3, it is characterized in that: the sodium dihydrogen phosphate of described concentration 0.2～2.0mol/L is prepared as: 0.02～0.2mol sodium dihydrogen phosphate solid is dissolved in the 100mL deionized water, stirred 10 minutes, and obtained the sodium dihydrogen phosphate that 100ml concentration is 0.2～2.0mol/L.
7. the preparation method of photochemical catalyst silver orthophosphate according to claim 3 is characterized in that: described sodium dihydrogen phosphate the speed in the silver ammino solution of splashing into slowly is 2-3 second/drip.
8. the purposes of the photochemical catalyst silver orthophosphate of the purposes of a silver orthophosphate as claimed in claim 1 or claim 2,3,4,5,6 or 7 described method preparations is characterized in that: described silver orthophosphate photocatalyst.
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