CN101940937A - High-efficiency visible light catalyst silver phosphate and preparation method thereof - Google Patents
High-efficiency visible light catalyst silver phosphate and preparation method thereof Download PDFInfo
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- CN101940937A CN101940937A CN 201010516084 CN201010516084A CN101940937A CN 101940937 A CN101940937 A CN 101940937A CN 201010516084 CN201010516084 CN 201010516084 CN 201010516084 A CN201010516084 A CN 201010516084A CN 101940937 A CN101940937 A CN 101940937A
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Abstract
The invention provides a high-efficiency visible light catalyst silver phosphate and a preparation method thereof, and solves the problem of low photocatalytic performance of the visible light catalyst silver phosphate. A precipitation conversion method is applied to the preparation of the silver phosphate so as to prepare the silver phosphate with a simple cubic system; and Ag3PO4 powder with the grain diameter of 400 to 520nm is obtained, and the photocatalytic performance thereof is improved. By applying the precipitation conversion method, the preparation method comprises the following steps of: preparing silver carbonate precipitate from silver nitrate and sodium bicarbonate, and converting the silver carbonate precipitate into silver phosphate precipitate by using monopotassium phosphate; and washing and drying to prepare the powdery silver phosphate visible light catalyst with the simple cubic system. The preparation method has the advantages of simpleness, easy operation and contribution to wide application of production practice.
Description
Technical field
The present invention relates to photocatalysis field, more specifically relate to a kind of efficient visible light catalyst-silver phosphate and preparation method thereof.Relate to the improvement of silver orthophosphate photocatalysis performance.
Background technology
Water resource poor relatively, serious environmental problem all the more makes the research tool of the catalyst of can be effectively organic matter being degraded have very important significance.With the semiconductor is catalyst, utilizes sunlight catalytic oxidation toxic pollutant matter as a kind of effective contamination governing method, also becomes a focus of environmental protection science research simultaneously.
In recent years, increasing semi-conducting material is applied to fields such as environmental protection, water treatment, organic matter degradation, inefficacy degradation of pesticide, make visible light catalyst obtain increasing concern, the research of efficient visible light catalyst-silver phosphate also becomes new focus.
Summary of the invention
Purpose of the present invention aims to provide a kind of efficient visible light catalyst A g
3PO
4And preparation method thereof.The present invention will precipitate the preparation of transformation applications in Ag3PO4, improving its photocatalysis performance, and its preparation condition gentleness, cost is low, and is simple to operate, and the cycle is short, and visible light catalytic efficient height helps actual production.
Technical scheme of the present invention is:
A kind of efficient visible light catalyst-silver phosphate, it is Powdered simple cubic crystallographic system silver orthophosphate visible light catalyst, particle diameter is 400～520nm, using the precipitation transformation approach makes, the preparation method prepares the silver carbonate precipitation with silver nitrate and sodium acid carbonate earlier, with potassium dihydrogen phosphate silver carbonate precipitation is converted to the silver orthophosphate precipitation again, after washing, the drying promptly.
A kind of preparation method of efficient visible light catalyst-silver phosphate, it is characterized in that: use the precipitation transformation approach, prepare the silver carbonate precipitation with silver nitrate and sodium acid carbonate earlier, with potassium dihydrogen phosphate the silver carbonate precipitation is converted to the silver orthophosphate precipitation again, obtains Powdered simple cubic crystallographic system silver orthophosphate visible light catalyst after washing, the drying.
Preparation method's step of efficient visible light catalyst-silver phosphate of the present invention is as follows: the substep preparation,
1) preparation silver carbonate precipitation: take by weighing a certain amount of silver nitrate and sodium acid carbonate respectively, use deionized water dissolving respectively, be made into the liquor argenti nitratis ophthalmicus that concentration is 0.02M-0.2M, sodium bicarbonate solution with 0.015M-0.15M, under the condition of magnetic agitation, described sodium bicarbonate solution is added dropwise in the described liquor argenti nitratis ophthalmicus, dripping speed is 3-5s/d, obtains white opacity liquid, at room temperature continues magnetic agitation 2-3h after dropwising;
2) preparation photochemical catalyst silver orthophosphate: take by weighing a certain amount of potassium dihydrogen phosphate, use deionized water dissolving, be made into the potassium dihydrogen phosphate that concentration is 0.01M-0.1M, under the magnetic agitation condition, it is added dropwise in the white opacity liquid of step 1) gained, dripping speed is 3-5s/d, obtain yellow turbid solution, dropwise and continue reaction 5-6h under the room temperature of back, filter, use deionized water, absolute ethanol washing more than 3 times respectively sediment, in 60 ℃ of oven dry, obtain the Powdered photochemical catalyst of simple cubic crystallographic system silver orthophosphate, particle diameter is 400～520nm (about 500nm).
In the technical scheme of the present invention, in described silver carbonate precipitation preparation process, for guaranteeing the abundant conversion of silver nitrate, the mol ratio of silver nitrate and sodium acid carbonate content is 1: 0.75.
In the technical scheme of the present invention, in described photochemical catalyst silver orthophosphate preparation process, for guaranteeing reacting completely of precipitation conversion, the mol ratio of silver carbonate content and biphosphate potassium content is 1: 1.
The visible light catalyst Ag3PO4 of the inventive method preparation is used for degradable organic pollutant under the visible light condition.
The invention has the advantages that:
1, the invention provides the preparation method of efficient visible light catalyst-silver phosphate, the product of preparation can carry out light-catalyzed reaction efficiently under visible light.
2, the present invention adopts the precipitation transformation approach to prepare the efficient visible light catalyst-silver phosphate, and the silver carbonate of preparation precipitation earlier is converted to silver carbonate the silver orthophosphate photochemical catalyst again, and its structure is improved, thereby reach the performance of silver orthophosphate is carried out improved purpose.
3, preparation method of the present invention is simple, and processing ease helps being extensive use of of production practices.
Room temperature described in the present invention means 10～30 ℃ of temperature.
Description of drawings
The SEM figure of the Ag3PO4 visible light catalyst of Fig. 1, the inventive method preparation.
The ultraviolet-visible absorption spectroscopy figure of the Ag3PO4 of Fig. 2, the inventive method preparation.
X-ray diffraction (XRD) figure of the Ag3PO4 of Fig. 3, the inventive method preparation.
The degradation curve of Ag3PO4 photochemical catalyst photocatalysis rhodamine B under the visible light condition of Fig. 4, the inventive method preparation.
Fig. 5, be the degradation curve of common Ag3PO4 photochemical catalyst photocatalysis rhodamine B under the visible light condition.
The Ag3PO4 visible light catalyst of Fig. 6, the inventive method preparation and In (Co/C)-T monobasic linearity curve comparison diagram of common Ag3PO4.
The specific embodiment
The substep preparation is adopted in the preparation of efficient visible light catalyst-silver phosphate of the present invention:
1, preparation silver carbonate precipitation: take by weighing a certain amount of silver nitrate and sodium acid carbonate respectively, place different beaker deionized water dissolvings respectively, be made into the liquor argenti nitratis ophthalmicus that concentration is 0.02M-0.2M, sodium bicarbonate solution with 0.015M-0.15M, under the condition of magnetic agitation, described sodium bicarbonate solution is slowly splashed in the described liquor argenti nitratis ophthalmicus, dripping speed is 3-5s/d, obtains white opacity liquid, at room temperature continues magnetic agitation 2-3h after dropwising;
2, preparation photochemical catalyst silver orthophosphate: take by weighing a certain amount of potassium dihydrogen phosphate, use deionized water dissolving, be made into the potassium dihydrogen phosphate that concentration is 0.01M-0.1M, under the magnetic agitation condition it slowly is added dropwise in the white opacity liquid of step 1 gained, dripping speed is 3-5s/d, obtains yellow turbid solution, dropwise and continue reaction 5-6h under the room temperature, filter, sediment is used deionized water, absolute ethanol washing 3 times respectively, obtain yellow powder in 60 ℃ of oven dry and be the photochemical catalyst silver orthophosphate.
For guaranteeing sufficient reacting, the ratio of silver nitrate, sodium acid carbonate, potassium dihydrogen phosphate three amount of substance is: 4: 3: 3.
Below in conjunction with embodiment silver orthophosphate photochemical catalyst and its application of the inventive method preparation are described further, but the present invention is not limited only to following embodiment.
Take by weighing AgNO respectively
3Solid 0.02mol and NaHCO
30.015mol, be dissolved in the deionized water of 100ml respectively, under the magnetic agitation condition with NaHCO
3Solution slowly splashes into AgNO
3In the solution, dripping speed is 3-5s/d, obtains white opacity liquid, at room temperature continues magnetic agitation 2-3h after dropwising.Take by weighing KH again
2PO
40.01mol be dissolved in the 100ml deionized water, dissolving back fully slowly drips it in above-mentioned white opacity liquid under the magnetic agitation condition, dripping speed is 3-5s/d, obtain yellow turbid solution, dropwise and at room temperature continue reaction 5-6h, filter, sediment is used deionized water, absolute ethanol washing 3 times respectively, in 60 ℃ of oven dry, obtain yellow silver orthophosphate powder.
The sem photograph of gained silver orthophosphate powder as shown in Figure 1.As seen from the figure, powder is that particle diameter is the silver orthophosphate of 500nm left and right sides simple cubic structure.Ultraviolet-visible absorption spectroscopy figure such as Fig. 2 of this silver orthophosphate, its ABSORPTION EDGE is near 500nm, and (400-600nm) has strong absorbability in the visible region.
XRD figure such as Fig. 3 of the silver orthophosphate of preparation.Fig. 3 show all peaks all with Ag
3PO
4(PDF CardNo.06-0505) is corresponding for standard card.Diffraction maximum is very narrow and sharp-pointed, and this silver orthophosphate that has reflected the present invention's preparation has very high degree of crystallinity, does not have other impurity to exist.The XRD figure spectrum shows that it is the simple cubic crystal.
Embodiment 2
The Ag that the inventive method makes
3PO
4With common Ag
3PO
4Visible light catalytic performance evaluation
The visible light catalyst Ag that the inventive method makes
3PO
4The rhodamine B of under visible light, degrading, catalyst amounts 0.05g, rhodamine B concentration is 1 * 10-5mol/L, volume is 100ml, light source adopts the 500W halogen tungsten lamp, use optical filter to guarantee that incident light is visible light, 420nm＜λ＜800nm measures the absorbance of degradation process with the UV-2550 ultraviolet-visual spectrometer.Every 10min gets a sample, after the centrifugation, gets supernatant liquor and measures.Fig. 4 is the Ag of the inventive method preparation
3PO
4The degradation curve of photochemical catalyst photocatalysis rhodamine B under the visible light condition.Having under the catalyst action as seen from Figure 4, rhodamine B is degraded fully behind the 70min.
Common Ag
3PO
4Photocatalytic degradation rhodamine B under the visible light condition, the test method condition is the same.Fig. 5 is common Ag
3PO
4The degradation curve of photocatalysis rhodamine B under the visible light condition is having under the catalyst action as seen from Figure 5, and rhodamine B is degraded fully behind the 140min.
The Ag of the inventive method preparation
3PO
4Visible light catalyst and common Ag
3PO
4The In of 70min (Co/C)-T monobasic linearity curve comparison diagram such as Fig. 6, Co is 554nm among the figure, the absorption value of 0min, C is every interval 10min, 554nm place absorption value.From scheming as seen the Ag that the inventive method prepares
3PO
4Visible light catalyst has photocatalysis performance efficiently.
Claims (4)
1. efficient visible light catalyst-silver phosphate, it is characterized in that: it is Powdered simple cubic crystallographic system silver orthophosphate visible light catalyst, particle diameter is 400～520nm, using the precipitation transformation approach makes, the preparation method prepares the silver carbonate precipitation with silver nitrate and sodium acid carbonate earlier, with potassium dihydrogen phosphate silver carbonate precipitation is converted to the silver orthophosphate precipitation again, after washing, the drying promptly.
2. the preparation method of an efficient visible light catalyst-silver phosphate, it is characterized in that: preparation process is as follows:
1) silver carbonate precipitation preparation: take by weighing a certain amount of silver nitrate and sodium acid carbonate respectively, use deionized water dissolving respectively, be made into the liquor argenti nitratis ophthalmicus that concentration is 0.02M-0.2M, sodium bicarbonate solution with 0.015M-0.15M, under the condition of magnetic agitation, described sodium bicarbonate solution is added dropwise in the described liquor argenti nitratis ophthalmicus, dripping speed is 3-5s/d, obtains white opacity liquid, at room temperature continues magnetic agitation 2-3h after dropwising;
2) photochemical catalyst silver orthophosphate preparation: take by weighing a certain amount of potassium dihydrogen phosphate, use deionized water dissolving, be made into the potassium dihydrogen phosphate that concentration is 0.01M-0.1M, under the magnetic agitation condition, it is splashed in the white opacity liquid of step 1) gained, dripping speed is 3-5s/d, obtain yellow turbid solution, dropwise and continue reaction 5-6h under the room temperature of back, filter, use deionized water, absolute ethanol washing more than 3 times respectively sediment, in 60 ℃ of oven dry, obtain the Powdered photochemical catalyst of simple cubic crystallographic system silver orthophosphate, particle diameter is 400～520nm.
3. the preparation method of efficient visible light catalyst-silver phosphate according to claim 2 is characterized in that: in the described silver carbonate precipitation preparation process, for guaranteeing the abundant conversion of silver nitrate, the mol ratio of silver nitrate and sodium acid carbonate content is 1: 0.75.
4. the preparation method of efficient visible light catalyst-silver phosphate according to claim 2, it is characterized in that: in the described photochemical catalyst silver orthophosphate preparation process, for guaranteeing reacting completely of precipitation conversion, the mol ratio of silver carbonate content and biphosphate potassium content is 1: 1.
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| CN102151577A (en) * | 2011-01-28 | 2011-08-17 | 东华大学 | Ag3PO4/Mg-Al LDO (Layered Double Oxide) visible light composite photo catalyst, preparation and application thereof |
| CN102247874A (en) * | 2011-05-26 | 2011-11-23 | 上海电力学院 | Silver chloride-silver phosphate composite photocatalyst and preparation method thereof |
| CN102580714A (en) * | 2012-02-09 | 2012-07-18 | 江苏大学 | Graphene oxide/silver phosphate composite visible light catalyst and preparation method thereof |
| CN102600870A (en) * | 2012-03-13 | 2012-07-25 | 宜兴市氿润环保研究所有限公司 | Loaded type silver phosphate/polyphosphoric silver/silver chloride compound water treatment photo-catalyst and preparation method thereof |
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