CN102247874A - Silver chloride-silver phosphate composite photocatalyst and preparation method thereof - Google Patents

Silver chloride-silver phosphate composite photocatalyst and preparation method thereof Download PDF

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CN102247874A
CN102247874A CN2011101379399A CN201110137939A CN102247874A CN 102247874 A CN102247874 A CN 102247874A CN 2011101379399 A CN2011101379399 A CN 2011101379399A CN 201110137939 A CN201110137939 A CN 201110137939A CN 102247874 A CN102247874 A CN 102247874A
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silver
catalyst
composite photo
chlorate
orthophosphate
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姚伟峰
宋秀兰
吴一平
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Shanghai University of Electric Power
University of Shanghai for Science and Technology
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Shanghai University of Electric Power
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Abstract

The invention discloses a silver chloride-silver phosphate composite photocatalyst and a preparation method thereof. In the composite photocatalyst, the mole percent ratio of silver chloride and silver phosphate, i.e. silver chloride: silver phosphate, ranges from 1:0-0.3. The preparation method comprises the steps of: preparing a mixed solution of chloride ions and phosphate ions first, and then adding Ag+ ions to the mixed solution, thus obtaining the silver chloride-silver phosphate composite photocatalyst. Application of the silver chloride-silver phosphate composite photocatalyst provided in the invention to photocatalytic degradation of the organic pollutant methylene blue can greatly improve the reaction activity of a silver chloride photocatalyst. In addition, the preparation method of the silver chloride-silver phosphate composite photocatalyst in the invention is simple and practicable, thus benefiting large-scale popularization.

Description

Silver chlorate-silver orthophosphate composite photo-catalyst and preparation method
Technical field
The invention belongs to the photocatalysis technology in the environmental pollution improvement, be specifically related to silver chlorate-silver orthophosphate composite photo-catalyst and preparation method thereof.
Background technology
Photocatalysis technology is easy to operate, pollution-free with it, can directly utilize advantage such as sunshine to become one of research focus that current solar energy utilizes.Tradition photochemical catalyst TiO 2Advantage such as inexpensive, nontoxic, stable with it, that catalytic activity is good obtains extensive concern.But because TiO 2The energy gap broad, need wavelength could display light under less than the exciting of the ultraviolet light of 400nm catalytic activity, its utilizable solar energy only accounts for about 4% of solar energy.It should be noted that (400～750nm) occupy 43% of sunshine gross energy to visible light, develop and develop visible-light photocatalysis material efficiently, expand the wave-length coverage that sunshine absorbs, and become the research focus of present photocatalysis research field.The silver chlorate photochemical catalyst is a kind of photochemical catalyst that has photocatalytic activity under radiation of visible light, but still has the lower problem of photocatalytic activity.
 
Summary of the invention
The objective of the invention is provides a kind of silver chlorate-silver orthophosphate composite photo-catalyst in order to improve silver chlorate photochemical catalyst photocatalytic activity.
Another object of the present invention provides the preparation method of above-mentioned a kind of silver chlorate-silver orthophosphate composite photo-catalyst.This preparation method is simple, do not need cost and complex equipment, synthesis condition gentleness.
Technical scheme of the present invention
A kind of silver chlorate-silver orthophosphate composite photo-catalyst, promptly visible photochemical catalyst silver chlorate carries out the catalyst of surface modification load silver orthophosphate gained, the wherein molar percentage of silver chlorate and silver orthophosphate, i.e. silver chlorate: silver orthophosphate is 1:0～0.3.Be non-TiO 2Catalyst is a kind of NEW TYPE OF COMPOSITE visible light catalyst.
The preparation method of a kind of silver chlorate-silver orthophosphate composite photo-catalyst, step is as follows:
Sodium chloride and sodium phosphate are dissolved in the deionized water, stir, obtain the mixed solution of phosphate anion and chlorion;
Described villaumite and phosphate are preferably its sodium salt;
Other gets silver nitrate and is dissolved in the deionized water, stirs, and obtains silver ion solution;
The mol ratio of described chlorion, phosphate anion and silver ion, i.e. chlorion: phosphate anion: silver ion is 1:0～0.3:1～2;
With the silver ion solution that makes under uninterrupted stirring, slowly splash in the mixed solution of above-mentioned phosphate anion and chlorion, continue to stir, silver chlorate and silver orthophosphate are produced with precipitation form, just obtain silver chlorate-silver orthophosphate composite photo-catalyst nano particle.
The particle diameter of the silver chlorate of above-mentioned gained-silver orthophosphate composite photo-catalyst nano particle is 10～100nm.
Above-mentioned a kind of silver chlorate-silver orthophosphate composite photo-catalyst is applied to the photocatalysis degradation organic contaminant methylene blue.
Beneficial effect of the present invention
The present invention utilizes silver orthophosphate that the silver chlorate photochemical catalyst is carried out surface modification first, and obtain a kind of silver chlorate-silver orthophosphate composite photo-catalyst, be applied to the photocatalysis degradation organic contaminant methylene blue, can significantly improve the reactivity of silver chlorate photochemical catalyst.Secondly the preparation method of silver chlorate of the present invention-silver orthophosphate composite photo-catalyst is simple, helps large-scale popularization.
Description of drawings
The Ag of Fig. 1, embodiment 1 gained 3PO 4X-ray diffraction (XRD) figure of the silver/silver chloride visible light catalyst of/AgCl composite photo-catalyst and embodiment 2 gained, arrow marks the diffraction maximum into silver orthophosphate
The Ag of Fig. 2, embodiment 1 gained 3PO 4The uv-visible absorption spectra of the silver/silver chloride visible light catalyst of/AgCl composite photo-catalyst and embodiment 2 gained
The Ag of Fig. 3, embodiment 1 gained 3PO 4The silver/silver chloride visible light catalyst of/AgCl composite photo-catalyst and embodiment 2 gained carries out the uv-visible absorption spectra after the light-catalyzed reaction
The Ag of Fig. 4, embodiment 1 gained 3PO 4The catalytic activity situation of the light degradation band look dyestuff methylene blue of the silver/silver chloride visible light catalyst of/AgCl composite photo-catalyst and embodiment 2 gained, curve a is the methylene blue light degradation situation when not having catalyst among the figure, curve b is the situation of silver chlorate photochemical catalyst light degradation methylene blue, and curve c is the situation of silver orthophosphate/silver chlorate composite photo-catalyst light degradation methylene blue
The Ag of Fig. 5, embodiment 1 gained 3PO 4The stability of catalytic activity situation of change schematic diagram of/AgCl composite photo-catalyst light degradation band look dyestuff methylene blue.
The specific embodiment
Also in conjunction with the accompanying drawings the present invention is further set forth below by embodiment, but the present invention is not limited only to this.
Embodiment 1
The preparation of the visible light catalyst that a kind of silver chlorate-silver orthophosphate is compound comprises the steps:
Taking by weighing 1.1688g is 0.02mol NaCl solid, and 0.7602g is the Na of 0.002mol 3PO 412H 2O is dissolved in the 200ml deionized water, stirs 10min, obtains the mixed solution of phosphate anion and chlorion;
Other takes by weighing 4.4166g is 0.026mol AgNO 3Be dissolved in the 200ml deionized water, stirred ten minutes, obtain liquor argenti nitratis ophthalmicus;
With dropper liquor argenti nitratis ophthalmicus slowly is added drop-wise in the mixed solution of above-mentioned prepared phosphate anion and chlorion, dropwises the back and continue to stir 4～5 hours, suspension is filtered, washing, 60 ℃ of oven dry, grinds the Ag that obtains yellow 3PO 4And the mol ratio of AgCl, i.e. chlorion: phosphate anion is the Ag of 1:0.1 3PO 4/ AgCl composite photo-catalyst nano particle, its particle diameter are 10～100nm.
Embodiment 2
When the mole of the silver orthophosphate of load was 0, promptly a kind of silver/silver chloride visible light Preparation of catalysts comprised the steps:
Taking by weighing 1.1688g is that 0.02mol NaCl solid is dissolved in the 200ml deionized water, stirs 10min, obtains sodium chloride solution;
Other takes by weighing the AgNO that 3.3974g is 0.02mol 3Be dissolved in the 200ml deionized water, stir 10min, obtain liquor argenti nitratis ophthalmicus;
With dropper liquor argenti nitratis ophthalmicus slowly is added drop-wise in the above-mentioned prepared sodium chloride solution, continues after dropwising to stir 4～5 hours, suspension filtration, washing, 60 ℃ of oven dry, grindings are obtained yellow silver/silver chloride visible light catalyst.
Fig. 1 is the Ag of the foregoing description 1 gained 3PO 4X-ray diffraction (XRD) figure of the silver/silver chloride visible light catalyst of/AgCl composite photo-catalyst and embodiment 2 gained, by contrasting with the XRD database, embodiment 2 prepared silver chlorates are pure phase as can be known, the Ag of embodiment 1 gained 3PO 4/ AgCl composite photo-catalyst is by silver chlorate and the silver orthophosphate two-phase is compound constitutes.
Fig. 2 is the Ag of the foregoing description 1 gained 3PO 4The UV, visible light extinction spectrum of the silver/silver chloride visible light catalyst of/AgCl composite photo-catalyst and embodiment 2 gained, as can be seen from Figure 2, Ag 3PO 4(400～800nm) have more weak visible absorption ability to/AgCl composite photo-catalyst in the visible region.
Application Example 1
Ag 3PO 4/ AgCl composite photo-catalyst and AgCl photocatalyst applications are in the light degradation methylene blue
The Ag that embodiment 1 is obtained 3PO 4The AgCl photocatalyst powder of/AgCl composite photo-catalyst and embodiment 2 gained is carried out the experiment of methylene blue photocatalytic degradation.
Take by weighing 0.1g Ag respectively 3PO 4/ AgCl composite photo-catalyst powder and 0.1gAgCl photocatalyst powder divide to be clipped to add in the 100 mL methylene blue solutions (20 mg/L), and lucifuge stirs 30 min, makes methylene blue solution reach absorption/desorption balance at catalyst surface;
Open light source then and carry out light-catalyzed reaction, get 3 mL reactant liquors respectively,, utilize Tianjin, island UV2550 spectrophotometer to detect through the micro porous filtration membrane filtration every 3-10 min;
Determine the change in concentration of methylene blue in the solution according to the variation of solution 640 nm place absorbances.Light source utilizes the 300W xenon lamp, uses optical filter to make incident light be visible light (420nm～800nm).Utilize the high water layer of 10cm to filter infrared ray in the light source, prevent that reacting liquid temperature from raising, and makes the light degradation reaction temperature be stabilized in room temperature state.
In the light-catalyzed reaction process, catalyst surface is covered by precious metals ag nano particle (black) gradually, thereby makes Ag 3PO 4/ AgCl composite photo-catalyst and AgCl photochemical catalyst have the ability of the full spectral absorption of 400～800nm visible light.
Fig. 3 is the Ag of embodiment 1 gained 3PO 4The silver/silver chloride visible light catalyst of/AgCl composite photo-catalyst and embodiment 2 gained is through the reacted UV, visible light extinction spectrum of photocatalytic degradation methylene blue.As can be seen from Figure 3, after photoinduction excites, Ag 3PO 4(400～800nm) have tangible visible absorption ability to/AgCl composite photo-catalyst in the visible region.So Ag of the present invention 3PO 4/ AgCl composite photo-catalyst can be regarded a kind of novel visible light catalyst.
The degraded situation of methylene blue as shown in Figure 4, as can be seen from Figure 4, when not having catalyst to add, methylene blue is not degraded substantially, and (curve is a); Add after the photochemical catalyst AgCl of embodiment 2 gained, methylene blue is degraded (curve b) substantially fully behind illumination 90 min; And the Ag of interpolation embodiment 1 gained 3PO 4/ AgCl composite photo-catalyst nano particle is a photochemical catalyst, and methylene blue is degraded (curve c) substantially fully behind illumination 45 min.A kind of Ag as can be seen from Figure 4 of the present invention 3PO 4/ AgCl composite photo-catalyst has visible light photocatalysis performance efficiently.
Application Example 2
Ag 3PO 4/ AgCl composite photo-catalyst is applied to the light degradation methylene blue, tests the stability of its photocatalytic activity
Ag with embodiment 1 gained 3PO 4/ AgCl composite photo-catalyst powder carries out the experiment of methylene blue photocatalytic degradation, and operating procedure obtains Ag with Application Example 1 3PO 4First set reaction activity change situation schematic diagram such as Fig. 5 of/AgCl composite photo-catalyst light degradation methylene blue dye.
After treating that methylene blue photocatalytic degradation experiment reaction finishes,, obtain Ag with reacting liquid filtering, drying 3PO 4/ AgCl composite photo-catalyst.
With the Ag that obtains 3PO 4/ AgCl composite photo-catalyst adds in the 100 mL methylene blue solutions (20 mg/L), and lucifuge stirs 30 min, makes methylene blue solution reach absorption/desorption balance at catalyst surface;
Open light source then and carry out light-catalyzed reaction, get 3 mL reactant liquors,, utilize Tianjin, island UV2550 spectrophotometer to detect through the micro porous filtration membrane filtration every 3-10 min;
Determine the change in concentration of methylene blue in the solution to obtain Ag according to the variation of solution 640 nm place absorbances 3PO 4The ACTIVITY CHANGE OF FT situation schematic diagram such as Fig. 5 second time of/AgCl composite photo-catalyst light degradation methylene blue dye.
As can be seen from Figure 5, Ag 3PO 4/ AgCl photocatalytic degradation methylene blue the second time reactivity and the first set reaction activity change less.So a kind of Ag of the present invention 3PO 4/ AgCl composite photo-catalyst visible light photocatalysis is used for the active more stable of degradation of methylene blue dyestuff.
Above-mentioned specific embodiment just is used for the present invention that explains, rather than limits the invention, and in spirit of the present invention and rights protection scope, any modification and change to the present invention makes all fall into protection scope of the present invention.

Claims (3)

1. silver chlorate-silver orthophosphate composite photo-catalyst, it is characterized in that the visible light catalyst silver chlorate is carried out the catalyst of silver orthophosphate composite load gained, wherein the molar percentage of silver chlorate and silver orthophosphate, i.e. silver chlorate: silver orthophosphate is 1:0～0.3.
2. a kind of silver chlorate as claimed in claim 1-silver orthophosphate composite photo-catalyst, the grain diameter that it is characterized in that described this catalyst is 10～100nm.
3. the preparation method of a kind of silver chlorate as claimed in claim 1 or 2-silver orthophosphate composite photo-catalyst, the step
Suddenly as follows:
Sodium chloride and sodium phosphate are dissolved in the deionized water, stir, obtain the mixed solution of phosphate anion and chlorion;
Other gets silver nitrate and is dissolved in the deionized water, stirs, and obtains silver ion solution;
The mol ratio of described chlorion, phosphate anion and silver ion, i.e. chlorion: phosphate anion: silver ion is 1:0～0.3:1～2;
With the silver ion solution that makes under uninterrupted stirring, slowly splash in the mixed solution of above-mentioned phosphate anion and chlorion, continue to stir, silver chlorate and silver orthophosphate are produced with precipitation form, just obtain silver chlorate of the present invention-silver orthophosphate composite photo-catalyst.
CN2011101379399A 2011-05-26 2011-05-26 Silver chloride-silver phosphate composite photocatalyst and preparation method thereof Pending CN102247874A (en)

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN102698782A (en) * 2012-06-25 2012-10-03 武汉理工大学 Dendrite silver phosphate visible light catalyst and preparation method thereof
CN102698780A (en) * 2012-06-15 2012-10-03 桂林理工大学 Silver halide/ silver phosphate heterojunction membrane visible photo-catalysis material and preparation method thereof
CN103028428A (en) * 2013-01-16 2013-04-10 华东理工大学 Method for preparing composite visual light catalytic material Ag3PO4 and g-C3N4
CN103537307A (en) * 2012-07-16 2014-01-29 中国科学院理化技术研究所 Graphene-silver phosphate composite photocatalyst and preparation method and application thereof
CN103920517A (en) * 2014-03-24 2014-07-16 江苏大学 Composite visible light photocatalyst and its preparation method
CN106925308A (en) * 2017-04-06 2017-07-07 太原理工大学 A kind of surface plasma nano catalysis material and its preparation method and application
CN108325542A (en) * 2018-02-02 2018-07-27 华北理工大学 A kind of netted Ag/Ag3PO4The synthetic method of/AgCl composite photocatalyst materials
CN112742484A (en) * 2019-10-29 2021-05-04 天津工业大学 Novel method for loading silver phosphate photocatalyst on surface of cotton fabric
CN113797945A (en) * 2021-10-03 2021-12-17 桂林理工大学 Ag/AgCl/Ag3PO4Preparation method of heterojunction composite photocatalyst

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Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN102600870B (en) * 2012-03-13 2014-11-05 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
CN102698780A (en) * 2012-06-15 2012-10-03 桂林理工大学 Silver halide/ silver phosphate heterojunction membrane visible photo-catalysis material and preparation method thereof
CN102698782A (en) * 2012-06-25 2012-10-03 武汉理工大学 Dendrite silver phosphate visible light catalyst and preparation method thereof
CN103537307A (en) * 2012-07-16 2014-01-29 中国科学院理化技术研究所 Graphene-silver phosphate composite photocatalyst and preparation method and application thereof
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
CN103028428A (en) * 2013-01-16 2013-04-10 华东理工大学 Method for preparing composite visual light catalytic material Ag3PO4 and g-C3N4
CN103920517A (en) * 2014-03-24 2014-07-16 江苏大学 Composite visible light photocatalyst and its preparation method
CN106925308A (en) * 2017-04-06 2017-07-07 太原理工大学 A kind of surface plasma nano catalysis material and its preparation method and application
CN108325542A (en) * 2018-02-02 2018-07-27 华北理工大学 A kind of netted Ag/Ag3PO4The synthetic method of/AgCl composite photocatalyst materials
CN108325542B (en) * 2018-02-02 2020-12-08 华北理工大学 Net-shaped Ag/Ag3PO4Synthetic method of/AgCl composite photocatalytic material
CN112742484A (en) * 2019-10-29 2021-05-04 天津工业大学 Novel method for loading silver phosphate photocatalyst on surface of cotton fabric
CN113797945A (en) * 2021-10-03 2021-12-17 桂林理工大学 Ag/AgCl/Ag3PO4Preparation method of heterojunction composite photocatalyst

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Application publication date: 20111123