CN105964250A - Ag10Si4O13 photocatalyst with visible-light response and preparation method and application thereof - Google Patents
Ag10Si4O13 photocatalyst with visible-light response and preparation method and application thereof Download PDFInfo
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- CN105964250A CN105964250A CN201610403707.6A CN201610403707A CN105964250A CN 105964250 A CN105964250 A CN 105964250A CN 201610403707 A CN201610403707 A CN 201610403707A CN 105964250 A CN105964250 A CN 105964250A
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 24
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000001301 oxygen Substances 0.000 claims abstract description 14
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000008367 deionised water Substances 0.000 claims abstract description 12
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 12
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 10
- 238000000227 grinding Methods 0.000 claims abstract description 9
- 239000004115 Sodium Silicate Substances 0.000 claims abstract description 6
- 235000019795 sodium metasilicate Nutrition 0.000 claims abstract description 6
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052911 sodium silicate Inorganic materials 0.000 claims abstract description 6
- 239000002957 persistent organic pollutant Substances 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- 238000001556 precipitation Methods 0.000 claims abstract description 3
- 238000000926 separation method Methods 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- IJKVHSBPTUYDLN-UHFFFAOYSA-N dihydroxy(oxo)silane Chemical compound O[Si](O)=O IJKVHSBPTUYDLN-UHFFFAOYSA-N 0.000 claims description 7
- 238000003801 milling Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 12
- 238000007146 photocatalysis Methods 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 5
- 239000002243 precursor Substances 0.000 abstract description 5
- 238000010521 absorption reaction Methods 0.000 abstract description 4
- 238000000034 method Methods 0.000 abstract description 4
- 239000002105 nanoparticle Substances 0.000 abstract description 2
- 230000000593 degrading effect Effects 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 230000001788 irregular Effects 0.000 abstract 1
- 239000000047 product Substances 0.000 description 19
- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 description 9
- 238000010438 heat treatment Methods 0.000 description 8
- 229960000907 methylthioninium chloride Drugs 0.000 description 8
- -1 Silicate compound Chemical class 0.000 description 6
- 238000000354 decomposition reaction Methods 0.000 description 6
- 239000000975 dye Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 230000015556 catabolic process Effects 0.000 description 5
- 238000006731 degradation reaction Methods 0.000 description 5
- 230000003287 optical effect Effects 0.000 description 5
- 238000006555 catalytic reaction Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 238000002425 crystallisation Methods 0.000 description 4
- 230000008025 crystallization Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000003746 solid phase reaction Methods 0.000 description 4
- 238000010671 solid-state reaction Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000004570 mortar (masonry) Substances 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 239000007790 solid phase Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 235000020188 drinking water Nutrition 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000003760 hair shine Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000001507 sample dispersion Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 230000009897 systematic effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 229910001428 transition metal ion Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/48—Silver or gold
- B01J23/50—Silver
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/042—Decomposition of water
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/02—Processes for making hydrogen or synthesis gas
- C01B2203/0266—Processes for making hydrogen or synthesis gas containing a decomposition step
- C01B2203/0277—Processes for making hydrogen or synthesis gas containing a decomposition step containing a catalytic decomposition step
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
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- Environmental & Geological Engineering (AREA)
- Hydrology & Water Resources (AREA)
- General Health & Medical Sciences (AREA)
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Abstract
The invention discloses a preparation method of an Ag10Si4O13 photocatalyst with visible-light response. The method includes the following steps that firstly, sodium metasilicate and silver nitrate are mixed according to the molar ratio of 1:(2-4) and evenly ground; secondly, the mixture obtained through grinding is added into deionized water and stirred, separation precipitation, washing and drying are conducted, and a precursor is obtained; thirdly, the precursor is heated to 300-500 DEG C at normal pressure and preserved for 3-5 hours, and the Ag10Si4O13 photocatalyst is obtained. Ag10Si4O13 synthesized through the method is composed of irregular nanoparticles, has high absorption in a visible light area, has high photocatalystic activity, and has the effects of decomposing water-produced oxygen through photocatalysis and degrading organic pollutants.
Description
Technical field
The present invention relates to a kind of there is visible light-responded Ag10Si4O13Photocatalyst and its preparation method and application, belongs to and partly leads
Body photocatalyst technology field.
Background technology
Utilize semiconductor light-catalyst that the low-density solar energy luminous energy being difficult to collect is changed into electric energy and the change that high density easily utilizes
Can become one of the most most active research field.Especially in photochemical catalyzing and utilize photooxidative degradation
Unique advantage that pollutant control environment aspect shows, has caused the extensive concern of countries in the world scientist, has the most half-and-half led
Body photocatalyst carries out theory and experimentation widely will have very important strategy and realistic meaning.
In all problems of the restriction actual application of photocatalysis technology at present, it is most important that how to improve the photocatalyst profit to luminous energy
Use efficiency.In solar spectrum, ultraviolet light accounts for all energy 3～4%, and visible ray accounting is but more than 40%, therefore,
Researching and developing visible light-responded photocatalyst is the research emphasis improving Solar use efficiency, has critically important theory
And practical significance.
Silicate compound is widely used in Industrial Catalysis frequently as catalysis material, but at present about silicate compound conduct
The report of photocatalyst material is less.Especially money base silicate compound, owing to its synthetic reaction condition is harsh, generally needs
Wanting high oxygen press strip part, this greatly constrains the systematic study of money base silicate compound.Therefore, from silicate compound
Middle discovery synthesis have the money base silicate material of high efficiency photocatalysis activity, have ten for expanding the actual application of photocatalyst
Divide important meaning.
Summary of the invention
For above-mentioned prior art, it is an object of the invention to provide and a kind of there is visible light-responded Ag10Si4O13Photocatalyst and
Its preparation method.
It is a further object of the present invention to provide this Ag10Si4O13Photocatalyst is at degradable organic pollutant and decomposes in Aquatic product oxygen
Application.
For achieving the above object, the present invention adopts the following technical scheme that
A first aspect of the present invention, it is provided that a kind of have visible light-responded Ag10Si4O13The preparation method of photocatalyst, step
As follows:
(1) by sodium metasilicate and silver nitrate 1:(2-4 in molar ratio) mixing, it is ground to uniformly；
(2) mixture that grinding obtains is joined in deionized water, stirring, precipitation separation, washing, it is dried, obtains presoma；
(3) presoma is heated to 300-500 DEG C at ambient pressure, and keeps 3-5 hour, obtain Ag10Si4O13Photocatalyst.
Preferably, in step (1), metasilicic acid is received and the mol ratio of silver nitrate is 1:3.Metasilicic acid is received and the addition of silver nitrate
Amount can affect the Ag of preparation10Si4O13The structure composition of photocatalyst, the amount that metasilicic acid is received by the present invention and silver nitrate adds is carried out
Investigate, it was found that metasilicic acid is received and silver nitrate 1:(2-4 in molar ratio) add and be advisable, it is possible to farthest generate mesh
Mark product；Receiving when metasilicic acid adds fashionable with silver nitrate 1:3 in molar ratio, Ag10Si4O13Productivity the highest.
Preferably, in step (1), milling time is 15-25min, further, and preferably 20min.Permissible by grinding
Improve the contact situation of reactant in the solid state reaction of the present invention, to increase the defect density being conducive to reaction, improve reaction
Thermodynamics and kinetics condition, enables solid state reaction to be smoothed out.Milling time is optimized by the present invention, it was found that
If milling time is too short, then reactant is insufficient contact；If milling time is long, then on the one hand extend generated time, increase
Add production cost, on the other hand also may can affect the crystal configuration of product.Find through multiple comparison test, during grinding
Between be advisable with 15-25min.
Preferably, in step (2), the ratio grinding mixture and the deionized water addition obtained is (0.5-1.5) mmol:
10ml。
Preferably, in step (2), washing uses deionized water and washes of absolute alcohol.
Preferably, in step (3), presoma is heated at ambient pressure 400 DEG C.Presoma is carried out heat treatment can change
The crystal phase structure of product, and the crystal phase structure of product is closely related with its photocatalytic activity, heat treatment temperature is carried out by the present invention
Investigate, it was found that the temperature of heat treatment higher than 500 DEG C or all cannot generate the crystalline A g of the present invention less than 300 DEG C10Si4O13。
Preferably, in step (3), carry out being warming up to heating-up temperature with the speed of 5 DEG C/min.
Ag prepared by said method10Si4O13Photocatalyst, is made up of random nano-particle, at transition metal ions (Ag+)
In the presence of, the SiO in silicate4Tetrahedron easily distorts and produces polarization, by controlling the tetrahedral arrangement meeting of these polarity
An internal polarization electric field is built at material internal；It addition, the coordination environment of the transition metal of complexity is that light induced electron is connected many
Transfer between the body of face provides probability.Therefore, the Ag that prepared by said method10Si4O13There is high efficiency photocatalysis activity.
A second aspect of the present invention, it is provided that above-mentioned Ag10Si4O13Photocatalyst is in decomposing Aquatic product oxygen and degradable organic pollutant
Application.
Beneficial effects of the present invention:
(1) Ag prepared by the present invention10Si4O13Photocatalyst has visible light-responded, through experimental studies have found that, and Ag10Si4O13
Demonstrate preferable photocatalytic activity, under visible ray shines, decompose Aquatic product oxygen 110umol at 2.5 hours, degraded 98% in 50 minutes
Methylene blue organic dyestuff.Under full light (300nm-1100nm), its photooxidative degradation methylene blue efficiency is than commodity TiO2
(P25) more outstanding.Therefore, the Ag that prepared by the present invention10Si4O13Photocatalyst has decomposition Aquatic product oxygen and degraded sky simultaneously
The double effects of gas, waste water, surface water or Organic Pollutants of Drinking Water, this is the money base silicate compound institute of existing report
Do not possess.
(2) Ag of the present invention10Si4O13Photocatalyst uses solid state reaction kinetics, is initially formed presoma, then through room temperature, height
Temperature solid state reaction crystallization, forms thermodynamically stable Ag10Si4O13Crystal.Preparation synthetic method condition is simple, it is not necessary to high
Oxygen press strip part, it is not necessary to add organic solvent, reaction condition is gentle, is more suitable for large-scale production and actual application, has higher
Commercial applications prospect.
Accompanying drawing explanation
Fig. 1 is presoma of the present invention, crystalline A g10Si4O13The X ray picture of standard card；
Fig. 2 is the optical absorption map of product of the present invention；
Fig. 3 is the SEM figure of product of the present invention；
Fig. 4 is that the embodiment of the present invention product photocatalyst and the N doping P25 that are formed are for Photocatalytic Activity for Degradation organic dyestuff
Methylene blue contrasts；
Fig. 5 is total carbon content (TC) in solution before and after photocatalyst Photocatalytic Activity for Degradation organic dyestuff methylene blue, organic
Carbon content (TOC) and inorganic carbon amounts (IC) variation diagram；
Fig. 6 is that the photocatalyst of embodiment of the present invention product formation is for photocatalysis Decomposition Aquatic product oxygen yield figure.
Detailed description of the invention
The present invention is further illustrated in conjunction with the embodiments, it should explanation, following embodiment merely to explain the present invention,
Its content is not defined.
Embodiment 1:
Weigh 3mmol sodium metasilicate and 9mmol silver nitrate is put in agate mortar, grind 20 minutes until color even.So
After uniform for grinding mixture is all poured in 100mL beaker, add 100mL deionized water stir ten minutes.Finally will
Precipitate and separate with deionized water and washes of absolute alcohol, is finally being dried at room temperature for, i.e. can get presoma.
The precursor powder of gained is placed in crucible, is then heated to 400 degrees Celsius with the speed of 5 degrees Celsius per minute and protects
Hold 4 hours, carry out secondary solid-phase heat treatment, i.e. obtain the Ag that crystallinity is good10Si4O13。
Presoma and crystalline A g to preparation10Si4O13Carry out structural characterization and performance test, wherein, presoma and crystallization
Ag10Si4O13X-ray diffractogram as shown in Figure 1；Crystalline A g10Si4O13Optical absorption map as shown in Figure 2；Crystallization
Ag10Si4O13SEM scheme as shown in Figure 3.
As seen from Figure 1, it is essentially amorphous phase without the presoma of heat treatment, after 4 hours heat treatments, product
Showing preferable crystallinity, composition is Ag10Si4O13, obvious miscellaneous peak does not occur.As seen from Figure 2, crystallization
Ag10Si4O13The strongest absorption is had at visible regime.As seen from Figure 3, the Ag that the present embodiment obtains10Si4O13Product is
The granule of 2 microns, the most special pattern.
Embodiment 2:
Weigh 3mmol sodium metasilicate and 6mmol silver nitrate is put in agate mortar, grind 20 minutes until color even.So
After uniform for grinding mixture is all poured in 100mL beaker, add 100mL deionized water stir ten minutes.Finally will
Precipitate and separate with deionized water and washes of absolute alcohol, is finally being dried at room temperature for, i.e. can get presoma.
The precursor powder of gained is placed in crucible, is then heated to 300 degrees Celsius with the speed of 5 degrees Celsius per minute and protects
Hold 3 hours, carry out secondary solid-phase heat treatment, i.e. obtain the Ag that crystallinity is good10Si4O13。
Embodiment 3:
Weigh 3mmol sodium metasilicate and 12mmol silver nitrate is put in agate mortar, grind 20 minutes until color even.
Then uniform for grinding mixture is all poured in 100mL beaker, add 100mL deionized water and stir ten minutes.Finally
By precipitate and separate and with deionized water and washes of absolute alcohol, finally it is being dried at room temperature for, i.e. can get presoma.
The precursor powder of gained is placed in crucible, is then heated to 500 degrees Celsius with the speed of 5 degrees Celsius per minute and protects
Hold 5 hours, carry out secondary solid-phase heat treatment, i.e. obtain the Ag that crystallinity is good10Si4O13。
Performance test:
1. photocatalytically degradating organic dye test
Common 100mL glass beaker is carried out under normal temperature and pressure.Light source selects the 300W xenon lamp equipped with optical filter so that
Optical source wavelength is more than 420nm.The photocatalytic activity of sample is evaluated with methylene blue.Weigh 50mg germne sample dispersion 50
In ml methylene blue B solution (20mg/L).Before light-catalyzed reaction test, lucifuge magnetic agitation 30min makes methylene blue in catalysis
Agent surface reaches adsorption equilibrium, samples 3ml, centrifugation every 10min, take supernatant UV, visible light spectrophotometric after logical light
Measurement amount absorbance.
The crystalline A g of embodiment 1 preparation10Si4O13Photocatalytically degradating organic dye test result as illustrated in figures 4-5, as seen from the figure,
Photocatalyst is tested through photocatalytically degradating organic dye methylene blue under visible light, and photocatalyst can be at 50 minutes by methylene blue
Degraded 98%, its photocatalytic activity is higher than N doping P25.
2. photocatalysis Decomposition Aquatic product oxygen test
The glass container system having recirculated cooling water (5 DEG C) to close in connection carries out and carries out, and vacuum condition is-97KPa.At top
The light source irradiated selects the 300W xenon lamp equipped with optical filter so that optical source wavelength is more than 420nm.Enter every 0.5h after logical light
Row test, gas chromatograph the peak area value recorded is converted into the yield of oxygen.
The crystalline A g of embodiment 1 preparation10Si4O13Photocatalysis Decomposition Aquatic product oxygen result as shown in Figure 6, Fig. 6 can see
Going out, photocatalyst can produce about 110umol oxygen by decomposition water in 2.5h under visible light.
Above detection and analysis integrated demonstrate the product that the present invention obtains and have visible light-responded for Photocatalyzed Hydrogen Production
Photocatalyst.And in terms of light degradation organic pollution and decomposition Aquatic product oxygen, there is preferable using value.
Claims (10)
1. one kind has visible light-responded Ag10Si4O13The preparation method of photocatalyst, it is characterised in that step is as follows:
(1) by sodium metasilicate and silver nitrate 1:(2-4 in molar ratio) mixing, it is ground to uniformly；
(2) mixture that grinding obtains is joined in deionized water, stirring, precipitation separation, washing, it is dried, obtains presoma；
(3) presoma is heated to 300-500 DEG C at ambient pressure, and keeps 3-5 hour, obtain Ag10Si4O13Photocatalyst.
2. preparation method as claimed in claim 1, it is characterised in that in step (1), metasilicic acid is received and the rubbing of silver nitrate
That ratio is 1:3.
3. preparation method as claimed in claim 1, it is characterised in that in step (1), milling time is 15-25min；
It is preferably 20min.
4. preparation method as claimed in claim 1, it is characterised in that in step (2), grinds the mixture that obtains and goes
The ratio of ionized water addition is (0.5-1.5) mmol:10ml.
5. preparation method as claimed in claim 1, it is characterised in that in step (2), washing uses deionized water
And washes of absolute alcohol.
6. preparation method as claimed in claim 1, it is characterised in that in step (3), presoma is heated at ambient pressure
To 400 DEG C.
7. preparation method as claimed in claim 1, it is characterised in that in step (3), rise with the speed of 5 DEG C/min
Temperature is to heating-up temperature.
8. the Ag that the preparation method described in any one of claim 1-7 prepares10Si4O13Photocatalyst.
9. the Ag described in claim 810Si4O13Photocatalyst purposes in degradable organic pollutant.
10. the Ag described in claim 810Si4O13Photocatalyst purposes in decomposing Aquatic product oxygen.
Priority Applications (1)
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| CN109647383A (en) * | 2019-01-28 | 2019-04-19 | 兰州理工大学 | A kind of nanometer of silver silicate photochemical catalyst and the preparation method and application thereof |
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