CN109967074A - A kind of preparation method and application of the titanium dioxide optical catalyst of silver load - Google Patents
A kind of preparation method and application of the titanium dioxide optical catalyst of silver load Download PDFInfo
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- CN109967074A CN109967074A CN201910212489.1A CN201910212489A CN109967074A CN 109967074 A CN109967074 A CN 109967074A CN 201910212489 A CN201910212489 A CN 201910212489A CN 109967074 A CN109967074 A CN 109967074A
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 78
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 239000003054 catalyst Substances 0.000 title claims abstract description 23
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 23
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 21
- 239000004332 silver Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 230000003287 optical effect Effects 0.000 title claims abstract description 17
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 42
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000002131 composite material Substances 0.000 claims abstract description 23
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000011941 photocatalyst Substances 0.000 claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229960000583 acetic acid Drugs 0.000 claims abstract description 14
- 239000008367 deionised water Substances 0.000 claims abstract description 14
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 14
- 239000012362 glacial acetic acid Substances 0.000 claims abstract description 14
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 11
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000006194 liquid suspension Substances 0.000 claims abstract description 8
- 229960000935 dehydrated alcohol Drugs 0.000 claims abstract description 7
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 7
- 239000002904 solvent Substances 0.000 claims abstract description 7
- 238000004090 dissolution Methods 0.000 claims abstract description 5
- 239000012046 mixed solvent Substances 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract 2
- 230000015556 catabolic process Effects 0.000 claims description 11
- 238000006731 degradation reaction Methods 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 10
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 claims description 9
- 229940012189 methyl orange Drugs 0.000 claims description 9
- 230000003197 catalytic effect Effects 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- 239000003344 environmental pollutant Substances 0.000 claims description 4
- 231100000719 pollutant Toxicity 0.000 claims description 4
- 229910021649 silver-doped titanium dioxide Inorganic materials 0.000 claims description 4
- 229910052724 xenon Inorganic materials 0.000 claims description 4
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 3
- 230000002035 prolonged effect Effects 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 15
- 230000000694 effects Effects 0.000 abstract description 10
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 abstract description 10
- 239000000463 material Substances 0.000 abstract description 8
- 238000005516 engineering process Methods 0.000 abstract description 6
- 238000000926 separation method Methods 0.000 abstract description 5
- 238000002198 surface plasmon resonance spectroscopy Methods 0.000 abstract description 5
- 238000005215 recombination Methods 0.000 abstract description 4
- 230000006798 recombination Effects 0.000 abstract description 4
- 239000002105 nanoparticle Substances 0.000 abstract description 3
- 238000000746 purification Methods 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 230000004044 response Effects 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 238000013019 agitation Methods 0.000 description 13
- 235000019441 ethanol Nutrition 0.000 description 10
- 230000001699 photocatalysis Effects 0.000 description 10
- 238000003760 magnetic stirring Methods 0.000 description 9
- 238000007146 photocatalysis Methods 0.000 description 7
- 150000001875 compounds Chemical class 0.000 description 6
- 239000000975 dye Substances 0.000 description 6
- 238000005259 measurement Methods 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 5
- 150000001298 alcohols Chemical class 0.000 description 5
- 239000013078 crystal Substances 0.000 description 5
- 229960004756 ethanol Drugs 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 229910001220 stainless steel Inorganic materials 0.000 description 5
- 239000010935 stainless steel Substances 0.000 description 5
- 239000003643 water by type Substances 0.000 description 5
- 229910000510 noble metal Inorganic materials 0.000 description 4
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 4
- 239000000725 suspension Substances 0.000 description 4
- 230000003321 amplification Effects 0.000 description 3
- 238000004043 dyeing Methods 0.000 description 3
- 238000003199 nucleic acid amplification method Methods 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 230000008033 biological extinction Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- 239000010970 precious metal Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229910001923 silver oxide Inorganic materials 0.000 description 2
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Substances [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 description 2
- 230000005476 size effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- -1 Methyl Chemical group 0.000 description 1
- 206010070834 Sensitisation Diseases 0.000 description 1
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000002500 effect on skin Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 239000002421 finishing Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000002703 mutagenesis Methods 0.000 description 1
- 231100000350 mutagenesis Toxicity 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000000985 reflectance spectrum Methods 0.000 description 1
- 238000004153 renaturation Methods 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 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
- 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
-
- 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
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/16—Reducing
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/30—Ion-exchange
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/343—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of ultrasonic wave energy
-
- 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
- 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
- C02F2101/34—Organic compounds containing oxygen
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- 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
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- 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
- C02F2101/40—Organic compounds containing sulfur
-
- 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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- Chemical Kinetics & Catalysis (AREA)
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- Plasma & Fusion (AREA)
- Optics & Photonics (AREA)
- Life Sciences & Earth Sciences (AREA)
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- Catalysts (AREA)
Abstract
The invention belongs to field of material synthesis technology, more particularly to a kind of preparation method and application of the titanium dioxide optical catalyst of silver load, weigh silver nitrate, it is dissolved in the in the mixed solvent of dehydrated alcohol, ethylene glycol, deionized water, glacial acetic acid and butyl titanate, ultrasonic dissolution obtains forerunner's liquid suspension, be transferred in hydrothermal reaction kettle later and carry out solvent thermal reaction, most afterwards through washing, filter, be dried to obtain Ag TiO2Composite photo-catalyst.The present invention is prepared for Ag@TiO by hydrothermal synthesis method2Plasma composite photo-catalyst, due to the surface plasmon resonance effect of Ag nanoparticle in the composite photo-catalyst, good absorbing properties are made it have, not only accelerate the separation of photo-generated carrier, the recombination probability for reducing photo-generate electron-hole pair, has also obviously expanded TiO2Spectral response range makes it have good practical value and potential application prospect in fields such as water body purifications.
Description
Technical field
The invention belongs to field of material synthesis technology more particularly to a kind of preparations of the titanium dioxide optical catalyst of silver load
Method and application.
Background technique
It is shown according to statistics, the 35% of the total discharged volume of industrial waste water of dyeing waste water amount Zhan of annual China's discharge,
As endangering maximum to the mankind and be difficult to the important pollution sources administered.With the development and final finishing technology of dye industry
Progress, New-type adjuvant, dyestuff, finishing agent etc. are widely used in dyeing, but are difficult to degrade, and its is toxic, organic
The content of ingredient is also more and more, some even carcinogenic, mutagenesis, aberration inducing organic matter, to environment especially water environment
Threat and harm it is also increasing.Therefore exploiting economy effective technology handles dyeing waste water, has become current environmental protection
The project that worker pays close attention to.In recent years, excellent applied to the efficient of wastewater treatment, energy-saving and environmental protection etc. due to photocatalysis technology
Different feature, making it just becomes the research hotspot of environment chemical engineering field.
Nano-titanium dioxide (TiO2) photochemical catalyst, the unique physics having, chemical property, such as small size effect
It answers, skin effect, quantum size effect, macro quanta tunnel effect etc., has always been considered as being a kind of close to ideal photocatalysis
One of material.But there is also apparent disadvantages for it: band gap is big, only ultraviolet light and near ultraviolet of the wavelength less than 400nm
Light can just excite TiO2Photo-generated carrier is generated, is allowed to show photocatalytic activity；And quantum efficiency is lower.Restricted T iO2Light
Two deciding factors of catalytic efficiency are the photo-generated carriers of competition and the capture of the compound of photo-generated carrier and capture
The compound competition between Charge transfer on interface.Therefore, theoretically, inhibit the compound of photo-generated carrier, improve interface electricity
Sub- transfer rate constant is the effective ways for improving photocatalysis performance.Presently, absorption and benefit of the photochemical catalyst to light are improved
Research work is concentrated mainly on on visible light catalyst, such as using doping metals/nonmetallic ion, carried noble metal with
And the spectral response range that the methods of hetero-junctions, dye sensitization improve photochemical catalyst is constructed, and then improve efficiency of light absorption；Pass through
Regulate and control the methods of catalyst structure, size, defect, specific surface area, active site and exposure crystal face to improve the extinction energy of itself
Power and electron-hole separative efficiency, and then improve photocatalytic degradation efficiency.TiO2Photocatalysis efficiency and sun light utilization efficiency mention
Height can also be realized by surface modification appropriate.Therefore, in order to further increase TiO2Photocatalysis performance, make full use of
Sunlight resource can organically combine precious metal doping and semiconductors coupling method, and building has plasma resonance effect
Heterojunction composite.The surface plasmon resonance effect of precious metals ag can not only extend the visible light of semiconductor material
Absorption region, and can be used as electronics capture trap capture electronics, accelerate the separation of photo-generate electron-hole, effectively inhibition photoproduction
Carrier it is compound.Its surface electronic can also be made to be quickly transferred to nanometer Ag surface simultaneously for semiconductor material containing Ag, had
Effect protects material containing Ag not to be reduced, and therefore substantially increases the visible light catalytic performance and stability of material.Meanwhile by
In foring intermediate level, the titanium dioxide of doping metals can also absorb more light, therefore can more effectively utilize the sun
Energy.
In recent years, silver ion becomes because it adulterates simple process, higher chemical stability, good extinction characteristic etc.
The metal-doped element for being used to improve optically catalytic TiO 2 performance with development prospect.However, preparation has a variety of nanometers
The method of the silver/titanium dioxide photochemical catalyst of structure is but rarely reported.Meanwhile the silver/titanium dioxide light of reported preparation is urged
The efficiency of agent degradable organic pollutant under visible light illumination requires further improvement.
Summary of the invention
One of the objects of the present invention is to provide a kind of preparation methods of the titanium dioxide optical catalyst of simple silver load.
To achieve the above object, the present invention adopts the following technical scheme:
A kind of preparation method of the titanium dioxide optical catalyst of silver load, includes the following steps: to weigh silver nitrate, is dissolved in nothing
Water-ethanol, deionized water, the in the mixed solvent of glacial acetic acid and butyl titanate, ultrasonic dissolution obtain forerunner's liquid suspension, then will
Forerunner's liquid suspension, which is transferred in hydrothermal reaction kettle, carries out solvent thermal reaction, most afterwards through centrifugation, wash, be dried to obtain Ag/TiO2
Composite photo-catalyst specifically comprises the following steps:
(1) butyl titanate is dispersed in the mixed solution of dehydrated alcohol, deionized water, glacial acetic acid, is sufficiently stirred
It mixes to obtain suspending liquid A；
(2) particles of silver nitrate is slowly added in ethylene glycol solution, solution B is obtained after ultrasonic dissolution；
(3) solution B is slowly added in suspending liquid A, obtains forerunner's liquid suspension C；
(4) forerunner's liquid suspension C is transferred in hydrothermal reaction kettle and carries out solvent thermal reaction, after fully reacting, be centrifuged, wash
It washs, be dried to obtain Ag/TiO2Composite photo-catalyst.
Preferably, the molar ratio for the titanium dioxide that the silver nitrate and reaction generate is 0~40:100.
Preferably, the molar ratio for the titanium dioxide that the silver nitrate and reaction generate is 1:5.
Preferably, the solvent thermal reaction temperature is 200~220 DEG C, and the reaction time is 18~24 hours.
Preferably, the in the mixed solvent of the dehydrated alcohol, deionized water and glacial acetic acid, dehydrated alcohol, deionized water with
The volume ratio of glacial acetic acid is 12:2:1.
Preferably, the ratio between the silver nitrate and ethylene glycol are 0.1~0.3mmol:20ml.
The second object of the present invention is to provide a kind of purposes of the titanium dioxide optical catalyst of silver load.
A kind of titanium dioxide optical catalyst of silver load is degraded the purposes of methyl orange pollutant under visible light.
Preferably, when the load capacity of Ag is Ag@TiO2When, the Ag@TiO2When the mass fraction of Ag is 20% in compound system
Optimal photocatalysis performance is shown, in 300W xenon lamp prolonged exposure 120min, methyl orange degradation rate can reach 99.99%.
The present invention prepares Ag@TiO by hydrothermal synthesis-ion exchange-reduction method2Plasma composite photo-catalyst, should
The surface plasmon resonance effect of nanometer Ag in composite photo-catalyst, makes it have good absorbing properties, not only accelerates
The separation of photo-generated carrier, reduces the recombination probability of photo-generate electron-hole pair, has highly efficient light under ultraviolet light
Catalytic activity and stability have efficient killing and degradation effect to dyes pollutant, in fields such as water body purifications
With good practical value and potential application prospect.The composite photo-catalyst preparation method has simple and easy and again simultaneously
The features such as renaturation is good, and the recycling to noble metal is realized, reaction process green non-pollution；It specifically includes such as lower section
Face:
(1) the preparation method simple process, easily controllable, environmentally protective that the present invention uses, and realize to noble metal
Recycling；
(2) in the present invention, Ag nano particles are in TiO2Surface in situ reduction building Ag@TiO2Plasma composite photocatalyst
Agent has biggish specific surface area and good visible absorption performance；
(3) Ag@TiO prepared by the present invention2Plasma composite photo-catalyst photocatalytic activity compares TiO2It significantly improves,
Under the irradiation of 300W xenon lamp, 0.05g Ag@TiO2The methyl orange sewage that plasma composite photo-catalyst is 10mg/L to concentration
Degradation rate is up to 99.99% in 120min.
Detailed description of the invention
Attached drawing 1 is the scanning electron microscope (SEM) photograph that sample is prepared according to 1 the method for embodiment；
Attached drawing 2 is the scanning electron microscope (SEM) photograph that sample is prepared according to 2 the method for embodiment；
Attached drawing 3 is the scanning electron microscope (SEM) photograph that sample is prepared according to 3 the method for embodiment；
Attached drawing 4 is the photocatalytic degradation lab diagram that sample is prepared according to each embodiment the method；
Attached drawing 5 is the ultraviolet-visible diffuse reflectance spectrum that sample is prepared according to each embodiment the method.
Specific embodiment
Below by way of specific embodiment, the invention will be further described, facilitates those skilled in the art more
It is fully understood by the present invention, but do not limit the invention in any way.
The present invention is prepared for Ag@TiO by hydrothermal synthesis method2Plasma composite photo-catalyst, the composite photo-catalyst
The surface plasmon resonance effect of middle nanometer Ag makes it have good visible absorption performance；Not only accelerate photoproduction load
The separation for flowing son reduces the recombination probability of photo-generate electron-hole pair, and has efficient photocatalytic activity and stability,
There is efficient degradation effect to dyes pollutant, there is good practical value and potential in fields such as water body purifications
Application prospect.The composite photo-catalyst preparation method has the characteristics that simple and easy and reproducible simultaneously, and realizes
Recycling to noble metal, reaction process green non-pollution.
Embodiment 1
Step 1 is transferred to flask with 12 milliliters of dehydrated alcohols of pipette measurement, 2 ml deionized waters and 1 milliliter of glacial acetic acid
It in A, is stirred for uniformly with magnetic stirring apparatus, then measures 0.5 milliliter of butyl titanate with pipette and be added in flask A,
It is stirred 30 minutes under magnetic agitation, obtains suspending liquid A；
Step 2 separately takes a beaker B, measures 10 milliliters of ethylene glycol with pipette, weighs 49.6 milligrams of nitre with electronic balance
Sour silver crystal, is added in the flask B equipped with ethylene glycol, and continue magnetic agitation 30 minutes under magnetic stirring, obtains solution
B；
Mixed liquor in flask B is slowly added in flask A by step 3, is continued magnetic agitation 30 minutes, is obtained presoma
Suspension C；
Above-mentioned mixed liquor is slowly transferred in 50 milliliters of polytetrafluoroethyllining lining stainless steel autoclave by step 4,
It is heated 22 hours at 210 DEG C.Reaction terminates after being cooled to room temperature, is washed 3 times, is then transferred into respectively with deionized water and ethyl alcohol
It is dried 10 hours at 70 DEG C in baking oven, obtaining molar ratio is Ag:TiO2The Ag@TiO of=20:1002Plasma complex light is urged
Agent product.
The scanning electron microscope of sample prepared by embodiment 1 is as shown in Figure 1, Fig. 1 a and Fig. 1 b are shown under different amplification
Ag@TiO2Scanning figure, as can be seen from the figure Ag@TiO2Pattern be nanometer sheet close to 50nm, be self-assembled into it is spherical, it is long
Width is evenly distributed, and thickness is well-balanced.
Embodiment 2
Step 1 is transferred to flask with 12 milliliters of dehydrated alcohols of pipette measurement, 2 ml deionized waters and 1 milliliter of glacial acetic acid
It in A, is stirred for uniformly with magnetic stirring apparatus, then measures 0.5 milliliter of butyl titanate with pipette and be added in flask A,
It is stirred 30 minutes under magnetic agitation, obtains suspending liquid A；
Step 2 separately takes a beaker B, measures 10 milliliters of ethylene glycol with pipette, weighs 12.4 milligrams of nitre with electronic balance
Sour silver crystal, is added in the flask B equipped with ethylene glycol, and continue magnetic agitation 30 minutes under magnetic stirring, obtains solution
B；
Mixed liquor in flask B is slowly added in flask A by step 3, is continued magnetic agitation 30 minutes, is obtained presoma
Suspension C；
Above-mentioned mixed liquor is slowly transferred in 50 milliliters of polytetrafluoroethyllining lining stainless steel autoclave by step 4,
It is heated 22 hours at 200 DEG C.Reaction terminates after being cooled to room temperature, is washed 3 times, is then transferred into respectively with deionized water and ethyl alcohol
It is dried 10 hours at 70 DEG C in baking oven, obtaining molar ratio is Ag:TiO2The Ag@TiO of=5:1002Plasma composite photocatalyst
Agent product.
The scanning electron microscope of sample prepared by embodiment 2 is as shown in Fig. 2, Fig. 2 a and Fig. 2 b are shown under different amplification
Ag@TiO2Scanning figure, as can be seen from the figure Ag@TiO2Pattern be uniform club shaped structure, length 500nm, width is about
100nm is evenly distributed, and thickness is well-balanced, without apparent agglomeration.
Embodiment 3
Step 1 is transferred to flask with 12 milliliters of dehydrated alcohols of pipette measurement, 2 ml deionized waters and 1 milliliter of glacial acetic acid
It in A, is stirred for uniformly with magnetic stirring apparatus, then measures 0.5 milliliter of butyl titanate with pipette and be added in flask A,
It is stirred 30 minutes under magnetic agitation, obtains suspending liquid A；
Step 2 separately takes a beaker B, measures 10 milliliters of ethylene glycol with pipette, weighs 24.8 milligrams of nitre with electronic balance
Sour silver crystal, is added in the flask B equipped with ethylene glycol, and continue magnetic agitation 30 minutes under magnetic stirring, obtains solution
B；
Mixed liquor in flask B is slowly added in flask A by step 3, is continued magnetic agitation 30 minutes, is obtained presoma
Suspension C；
Above-mentioned mixed liquor is slowly transferred in 50 milliliters of polytetrafluoroethyllining lining stainless steel autoclave by step 4,
It is heated 22 hours at 240 DEG C.Reaction terminates after being cooled to room temperature, is washed 3 times, is then transferred into respectively with deionized water and ethyl alcohol
It is dried 10 hours at 70 DEG C in baking oven, obtaining molar ratio is Ag:TiO2The Ag@TiO of=10:1002Plasma complex light is urged
Agent product.
Embodiment 4
Step 1 is transferred to flask with 12 milliliters of dehydrated alcohols of pipette measurement, 2 ml deionized waters and 1 milliliter of glacial acetic acid
It in A, is stirred for uniformly with magnetic stirring apparatus, then measures 0.5 milliliter of butyl titanate with pipette and be added in flask A,
It is stirred 30 minutes under magnetic agitation, obtains suspending liquid A；
Step 2 separately takes a beaker B, measures 10 milliliters of ethylene glycol with pipette, weighs 99.2 milligrams of nitre with electronic balance
Sour silver crystal, is added in the flask B equipped with ethylene glycol, and continue magnetic agitation 30 minutes under magnetic stirring, obtains solution
B；
Mixed liquor in flask B is slowly added in flask A by step 3, is continued magnetic agitation 30 minutes, is obtained presoma
Suspension C；
Above-mentioned mixed liquor is slowly transferred in 50 milliliters of polytetrafluoroethyllining lining stainless steel autoclave by step 4,
It is heated 18 hours at 220 DEG C.Reaction terminates after being cooled to room temperature, is washed 3 times, is then transferred into respectively with deionized water and ethyl alcohol
It is dried 10 hours at 70 DEG C in baking oven, obtaining molar ratio is Ag:TiO2The Ag@TiO of=40:1002Plasma complex light is urged
Agent product.
The scanning electron microscope of sample prepared by embodiment 4 is as shown in Figure 1, Fig. 3 a and Fig. 3 b are shown under different amplification
Ag@TiO2Scanning figure, as can be seen from the figure Ag@TiO2Pattern be nano wire close to 1um, be evenly distributed, without apparent
Agglomeration.
Embodiment 5
Step 1 is transferred to flask with 12 milliliters of dehydrated alcohols of pipette measurement, 2 ml deionized waters and 1 milliliter of glacial acetic acid
It in A, is stirred for uniformly with magnetic stirring apparatus, then measures 0.5 milliliter of butyl titanate with pipette and be added in flask A,
It is stirred 30 minutes under magnetic agitation, obtains suspending liquid A；
Suspending liquid A is slowly transferred in 50 milliliters of polytetrafluoroethyllining lining stainless steel autoclave by step 2,200
It is heated 24 hours at DEG C.Reaction terminates after being cooled to room temperature, is washed 3 times respectively with deionized water and ethyl alcohol, is then transferred into baking
It is dried 10 hours at 70 DEG C in case, pure TiO2Photocatalyst product.
Above-mentioned gained Ag@TiO2Plasma composite photo-catalyst is applied to the visible light catalytic of dyestuff contaminant methyl orange
Degradation:
Using 300W xenon lamp as light source, it is aided with optical filter and filters ultraviolet light, makes 420~760nm of its wave-length coverage, it will
The methyl orange solution of 50mL 10mol/L is added in 50mL reactor, and 25mg Ag@TiO prepared by the present invention is added2Plasma
Bluk recombination photochemical catalyst, dark adsorption carry out light-catalyzed reaction after reaching balance, and separated in time samples in reaction process, from
It takes supernatant liquor in the absorbance of ultraviolet-visible spectrophotometer measurement 552nm wavelength Methyl Orange solution after heart separation, obtains
The residual concentration of methyl orange solution calculates degradation rate with this.
From fig. 4, it can be seen that pure TiO2Methyl orange is hardly degraded in degradation experiment, and the influence to experiment can be ignored.Separately
Outside, under visible light photograph, Ag@TiO2Plasma composite photo-catalyst shows good photocatalytic activity, photocatalysis performance
It is substantially better than TiO2, 100% can reach to the degradation rate of methyl orange within the 120min reaction time.Therefore, there will be silver nanoparticle
The TiO of particle and good photocatalytic activity2Forming composite construction can be such that photo-generate electron-hole effectively divides in composite material surface
From, while the surface plasmon resonance effect of nanometer Ag improves the visible absorption performance of composite material, enhances compound
The visible light catalytic performance of material.When the load capacity of Ag occupies Ag@TiO2Mass fraction 20% when, the Ag@TiO2Compound system
Optimal catalytic performance is shown, in visible light prolonged exposure 120min, methyl orange degradation rate can reach 99.99%.
Taking the above-mentioned ideal embodiment according to the present invention as inspiration, through the above description, relevant staff is complete
Various changes and amendments can be carried out without departing from the scope of the technological thought of the present invention' entirely.The technology of this invention
Property range is not limited to the contents of the specification, it is necessary to which the technical scope thereof is determined according to the scope of the claim.
Claims (8)
1. a kind of preparation method of the titanium dioxide optical catalyst of silver load, which is characterized in that weigh silver nitrate, be dissolved in anhydrous second
Alcohol, ethylene glycol, deionized water, the in the mixed solvent of glacial acetic acid and butyl titanate, ultrasonic dissolution obtain forerunner's liquid suspension, it
After be transferred in hydrothermal reaction kettle and carry out solvent thermal reaction, most afterwards through washing, filter, be dried to obtain Ag/TiO2Composite photocatalyst
Agent；
Specifically comprise the following steps:
(1) butyl titanate is dispersed in the mixed solution of dehydrated alcohol, deionized water, glacial acetic acid, is sufficiently stirred
To suspending liquid A；
(2) particles of silver nitrate is slowly added in ethylene glycol solution, solution B is obtained after dissolution；
(3) solution B is slowly added in suspending liquid A, obtains forerunner's liquid suspension C；
(4) forerunner's liquid suspension C is transferred in hydrothermal reaction kettle and carries out solvent thermal reaction, after fully reacting, be centrifuged, wash,
It is dried to obtain Ag/TiO2Composite photo-catalyst.
2. a kind of preparation method of the titanium dioxide optical catalyst of silver load according to claim 1, it is characterised in that: institute
The molar ratio for the titanium dioxide that the silver nitrate and reaction stated generate is 0~40:100.
3. a kind of preparation method of the titanium dioxide optical catalyst of silver load according to claim 2, it is characterised in that: institute
The molar ratio for the titanium dioxide that the silver nitrate and reaction stated generate is 1:5.
4. a kind of preparation method of the titanium dioxide optical catalyst of silver load according to claim 1, it is characterised in that: institute
Stating solvent thermal reaction temperature is 200~220 DEG C, and the reaction time is 18~24 hours.
5. a kind of preparation method of the titanium dioxide optical catalyst of silver load according to claim 1, it is characterised in that: institute
The in the mixed solvent of dehydrated alcohol, deionized water and glacial acetic acid is stated, the volume ratio of dehydrated alcohol, deionized water and glacial acetic acid is
12:2:1。
6. a kind of preparation method of the titanium dioxide optical catalyst of silver load according to claim 1, it is characterised in that: institute
Stating the ratio between silver nitrate and ethylene glycol is 0.1~0.3mmol:20ml.
7. the titanium dioxide optical catalyst of the silver load of preparation method preparation according to claim 1 is under simulated visible light
The purposes of degradation methyl orange pollutant.
8. the titanium dioxide optical catalyst of silver load according to claim 7 declines solution methyl orange pollution in simulated visible light
The purposes of object, it is characterised in that: when the load capacity of Ag occupies Ag@TiO2Mass fraction 20% when, the Ag@TiO2Compound system
Optimal catalytic performance is shown, in 300W xenon lamp prolonged exposure 120min, the degradation rate of methyl orange can reach 99.99%.
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