CN106732588A - Catalyst of Cr (VI) and its preparation method and application in one kind conversion aqueous solution - Google Patents
Catalyst of Cr (VI) and its preparation method and application in one kind conversion aqueous solution Download PDFInfo
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- CN106732588A CN106732588A CN201611004573.7A CN201611004573A CN106732588A CN 106732588 A CN106732588 A CN 106732588A CN 201611004573 A CN201611004573 A CN 201611004573A CN 106732588 A CN106732588 A CN 106732588A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- 239000007864 aqueous solution Substances 0.000 title claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 title abstract description 23
- 229910003256 NaTaO3 Inorganic materials 0.000 claims abstract description 69
- 239000010931 gold Substances 0.000 claims abstract description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 16
- 238000009835 boiling Methods 0.000 claims abstract description 15
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052737 gold Inorganic materials 0.000 claims abstract description 8
- 229910052709 silver Inorganic materials 0.000 claims abstract description 8
- 239000002253 acid Substances 0.000 claims abstract description 7
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 7
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 6
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 8
- 239000006260 foam Substances 0.000 claims description 8
- 239000000725 suspension Substances 0.000 claims description 7
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 6
- 238000004821 distillation Methods 0.000 claims description 6
- 239000000376 reactant Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 239000006228 supernatant Substances 0.000 claims description 6
- 238000013019 agitation Methods 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000005187 foaming Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 239000013049 sediment Substances 0.000 claims description 3
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 claims description 3
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- 238000005119 centrifugation Methods 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(III) oxide Inorganic materials O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 claims description 2
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 2
- 239000000843 powder Substances 0.000 abstract description 10
- 230000001699 photocatalysis Effects 0.000 abstract description 8
- 239000007788 liquid Substances 0.000 abstract description 5
- 239000000126 substance Substances 0.000 abstract description 2
- 238000003912 environmental pollution Methods 0.000 abstract 1
- 239000011651 chromium Substances 0.000 description 40
- 238000006555 catalytic reaction Methods 0.000 description 7
- 238000007146 photocatalysis Methods 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 235000019441 ethanol Nutrition 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- KSPIHGBHKVISFI-UHFFFAOYSA-N Diphenylcarbazide Chemical compound C=1C=CC=CC=1NNC(=O)NNC1=CC=CC=C1 KSPIHGBHKVISFI-UHFFFAOYSA-N 0.000 description 3
- 239000010419 fine particle Substances 0.000 description 3
- 238000005286 illumination Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000002798 spectrophotometry method Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 230000009466 transformation Effects 0.000 description 3
- 238000009827 uniform distribution Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000010531 catalytic reduction reaction Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- -1 rare-earth ion Chemical class 0.000 description 2
- 230000006641 stabilisation Effects 0.000 description 2
- 238000011105 stabilization Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 206010005003 Bladder cancer Diseases 0.000 description 1
- 206010007269 Carcinogenicity Diseases 0.000 description 1
- 244000131522 Citrus pyriformis Species 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 201000001531 bladder carcinoma Diseases 0.000 description 1
- 230000007670 carcinogenicity Effects 0.000 description 1
- 231100000260 carcinogenicity Toxicity 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- ZCDOYSPFYFSLEW-UHFFFAOYSA-N chromate(2-) Chemical compound [O-][Cr]([O-])(=O)=O ZCDOYSPFYFSLEW-UHFFFAOYSA-N 0.000 description 1
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000006184 cosolvent Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- SOCTUWSJJQCPFX-UHFFFAOYSA-N dichromate(2-) Chemical compound [O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O SOCTUWSJJQCPFX-UHFFFAOYSA-N 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 235000020188 drinking water Nutrition 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- RJHLTVSLYWWTEF-UHFFFAOYSA-K gold trichloride Chemical class Cl[Au](Cl)Cl RJHLTVSLYWWTEF-UHFFFAOYSA-K 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 201000007270 liver cancer Diseases 0.000 description 1
- 208000014018 liver neoplasm Diseases 0.000 description 1
- 229910052752 metalloid Inorganic materials 0.000 description 1
- 150000002738 metalloids Chemical class 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 239000008239 natural water Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 238000001259 photo etching Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229940035637 spectrum-4 Drugs 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
- 208000010570 urinary bladder carcinoma Diseases 0.000 description 1
- 239000003643 water by type 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
- 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
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/66—Silver or gold
- B01J23/68—Silver or gold with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/682—Silver or gold with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with vanadium, niobium, tantalum or polonium
-
- 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
-
- 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
- C02F1/70—Treatment of water, waste water, or sewage by reduction
-
- 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
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
-
- 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
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Catalysts (AREA)
Abstract
Catalyst the present invention relates to Cr (VI) in one kind conversion aqueous solution and its preparation method and application.The technical scheme of use is：By NaTaO3And Er3+:YAlO3Synthesize Er with the method for ultrasonic disperse and liquid boiling3+:YAlO3/NaTaO3.Finally, by NaTaO obtained above3/Er3+:YAlO3Powder and the dissolving of gold chloride, chloroplatinic acid or silver nitrate in ethanol, X/NaTaO are synthesized with the method for ultrasonic disperse and liquid boiling3/Er3+:YAlO3(X=Ag, Au and Pt).Under sunlight, X/NaTaO is used3/Er3+:YAlO3(X=Ag, Au and Pt) makees catalyst, photocatalytic conversion Cr (VI).The inventive method is simply novel, low cost, and the generation of no accessory substance can't cause environmental pollution.
Description
Technical field
The invention belongs to chemical catalysis field, more particularly to new catalyst synthesis and using catalyst to Cr in water body
(VI) method for being converted.
Background technology
With the development of the modern industry, the Cr VI (Cr (VI)) in natural water and industrial wastewater has become environment
One big harm.Cr (VI) is mainly derived from the industries such as mining, plating, Treatment of Metal Surface, process hides, printing and dyeing and casting, not
Under the conditions of same concentration or pH, Cr (VI) is with chromate (HCrO4-/CrO4 2-) and bichromate (Cr2O7 2-) form enter ring
Border.Research shows, Cr (VI) has a carcinogenicity higher than 1000 times of Cr (III), and generally have dissolubility higher, toxicity,
Unstability and bioactivity.If containing Cr (VI) in drinking water, human body can be increased and suffer from liver cancer, cutaneum carcinoma and carcinoma of urinary bladder
Possibility.Conversely, appropriate Cr (III) is element necessary to human body, therefore, it is very that Cr (VI) is reduced into Cr (III)
It is necessary.
Photocatalysis technology directly using pollutant in the light removal water body for absorbing, and easily separated reuse, and can be received because of it
To extensive concern, such as TiO2Because its catalysis activity is of a relatively high, physicochemical properties stabilization, and be widely used.For going
Except the Cr (VI) in water body, it would be desirable to a semiconductor having compared with Strong oxdiative ability and reducing power is selected, by Cr (VI)
Cr (III) is converted into, this requires that we select the broadband semiconductor of an of a relatively high conduction band and relatively low valence band.Through adjusting
Look into, perovskite NaTaO3It is a kind of novel metalloid wide-band-gap semiconductor material, with photo catalytic reduction performance higher, but because
It is with band gap wider, NaTaO3Ultraviolet light can only be absorbed carries out light-catalyzed reaction.Ultraviolet light only accounts for solar spectrum
4%, this makes the utilization rate of solar energy become minimum.In order to obtain solar energy utilization ratio higher, it is necessary to which developing to utilize
The catalyst of visible ray.
The content of the invention
Can be used to convert the new catalyst X/ of Cr (VI) in the aqueous solution it is an object of the invention to design synthesis one kind
NaTaO3/Er3+:YAlO3(X=Ag, Au and Pt).Compound involved in the present invention belongs to new rare metal catalyst, will
It is applied to Cr (VI) conversions, and method is simple, pollution-free, catalyst stabilization and is easily isolated.
The technical solution adopted by the present invention is as follows：One kind converts the catalyst of Cr (VI) in the aqueous solution, and the catalyst is
X/NaTaO3/Er3+:YAlO3, wherein, X=Ag, Au or Pt.
The preparation method of the catalyst of Cr (VI) in a kind of above-mentioned conversion aqueous solution, method is as follows：
1) by Er3+:YAlO3And NaTaO3Mixing, plus deionized water, ultrasonic disperse 15-25min；30- is heated at the boiling point
40min, and magnetic agitation, after reactant is with distillation water filtration and cleaning, 500 DEG C of heating 2-3h, obtain NaTaO in Muffle furnace3/
Er3+:YAlO3；
2) by NaTaO3/Er3+:YAlO3With the dissolving of gold chloride, chloroplatinic acid or silver nitrate in ethanol, ultrasonic disperse 30-40
Minute, suspension is obtained, suspension is heated to boiling point, heated 30-40 minutes under boiling point, reactant distillation water filtration and washing
Afterwards, 1-2h is calcined at 350 DEG C, is ground, obtain X/NaTaO3/Er3+:YAlO3；Wherein X=Ag, Au or Pt.
The preparation method of the catalyst of Cr (VI) in a kind of above-mentioned conversion aqueous solution, in mass ratio, Er3+:YAlO3:
NaTaO3=3:7.
The preparation method of the catalyst of Cr (VI) in a kind of above-mentioned conversion aqueous solution, described gold chloride, chloroplatinic acid or
The addition of silver nitrate is NaTaO3/Er3+:YAlO3The 1-2% of quality.
The preparation method of the catalyst of Cr (VI), described NaTaO in a kind of above-mentioned conversion aqueous solution3Preparation method
It is：By Ta2O5And NaOH, add water after stirring, it is transferred in hydrothermal reaction kettle, 15-17h is processed at 180 DEG C, it is cooled to
Room temperature, abandons supernatant, and sediment is washed with deionized to neutrality, and centrifugation is dried, and obtains NaTaO3。
The preparation method of the catalyst of Cr (VI) in a kind of above-mentioned conversion aqueous solution, in molar ratio, Ta:Na=1:10.
The preparation method of the catalyst of Cr (VI), described Er in a kind of above-mentioned conversion aqueous solution3+:YAlO3Preparation
Method is：By Er2O3And Y2O3It is dissolved in concentrated nitric acid, then sequentially adds Al (NO3)3The aqueous solution and aqueous citric acid solution, in
50-60 DEG C of heating stirring, stops when solution is in thick, and must foam glutinous colloidal solution, and foaming is sticked into colloidal solution in 75-85
35-40h is heated at DEG C, foam sol is obtained, after foam sol is heated into 50-60min at 500 DEG C, 2-3h is calcined at 1100 DEG C,
Cooling, obtains Er3+:YAlO3。
Application of the above-mentioned catalyst in Cr (VI) in converting the aqueous solution.Method is as follows：In the solution containing Cr (VI)
In, add above-mentioned catalyst X/NaTaO3/Er3+:YAlO3, irradiated under normal temperature, solar irradiation.
The beneficial effects of the invention are as follows：
1. of the invention, in order to improve NaTaO3Photocatalysis efficiency, and then hexavalent chromium is more effectively converted, by upper turn
Photo etching Er3+:YAlO3With NaTaO3It is combined together, in the combination of this photochemical catalyst, Er3+:YAlO3Can by absorb can
Seeing that light is converted into can be by NaTaO3The ultraviolet light for directly utilizing, so that the NaTaO with band gap wider3Can be more effectively
Light-catalyzed reaction is carried out using sunshine.
2. the present invention, excite electron-hole pair using sunshine and improve the purpose of photocatalysis efficiency to reach, and add
A small amount of precious metal such as gold, silver in semiconductor surface, by using a photocatalytic system for triple hetero-junctions, Ke Yiti
High visible absorbs and photocatalysis efficiency, illustrates the optimal light catalytic reduction efficiency for Cr VI.
3. the present invention have studied with NaTaO on the basis of various photocatalysis technologies for Cr (VI)3Turn light hair on compound
Luminescent material and add cocatalyst carry out Cr (VI) conversion technology.By the method for the present invention, Cr (VI) concentration can be down to
Below 0.05ppm, without influenceing other quality index.Compared with other photocatalysis technologies, process of the present invention is simple, normal temperature and pressure
Carry out, mild condition, and using solar energy, conversion ratio reaches more than 97%.
Brief description of the drawings
Fig. 1 a are Er3+:YAlO3XRD.
Fig. 1 b are Er3+:YAlO3SEM figure.
Fig. 2 a are NaTaO3XRD.
Fig. 2 b are NaTaO3SEM figure.
Fig. 3 a are NaTaO3/Er3+:YAlO3XRD.
Fig. 3 b are NaTaO3/Er3+:YAlO3SEM figure.
Fig. 4 a are Ag/NaTaO3/Er3+:YAlO3XRD.
Fig. 4 b are Ag/NaTaO3/Er3+:YAlO3SEM figure.
Fig. 5 a are Au/NaTaO3/Er3+:YAlO3XRD.
Fig. 5 b are Au/NaTaO3/Er3+:YAlO3SEM figure.
Fig. 6 a are Pt/NaTaO3/Er3+:YAlO3XRD.
Fig. 6 b are Pt/NaTaO3/Er3+:YAlO3SEM figure.
Specific embodiment
The catalyst Ag/NaTaO of embodiment 13/Er3+:YAlO3
(1) preparation method
1.NaTaO3Prepare：By 1.7540g Ta2O5With 3.1750g NaOH (Ta/Na mol ratios 1:10), add 25mL's
After distilled water stirs, it is transferred in water heating kettle, room temperature is cooled to after processing 15h at 180 DEG C.Treat that water heating kettle is cooled down completely
Afterwards, take out, abandon supernatant, obtain white powder, be neutral by white powder deionized water centrifuge washing to the eluate, then use
Absolute ethyl alcohol is rinsed twice.Finally product is dried 12 hours in 60 DEG C of baking ovens, NaTaO is obtained3, it is standby.
2.Er3+:YAlO3Prepare：By 0.0232g Er2O3、1.3640g Y2O3It is dissolved in concentrated nitric acid, and magnetic force is heated
Stirring is until water white transparency, obtains rare-earth ion solution.Then a beaker is separately taken, 4.5316g Al (NO are weighed3)3·9H2O dissolves
In distilled water, stirred and be slowly added in above-mentioned rare-earth ion solution with glass bar at room temperature.Weigh 15.2325g lemons
Lemon acid is then added in above-mentioned solution as chelating agent and cosolvent and with distillation water dissolves.Then stirred in 50-60 DEG C of heating
Mix, stop when solution is in thick.Generation is not precipitated in this process, finally gives the glutinous colloidal solution of foaming.Will hair
The glutinous colloidal solution of bubble is put into baking oven, 80 DEG C of heated at constant temperature 36h.Until solvent evaporated does not have sediment to generate in drying process,
Finally give foam sol.The foam sol that will be obtained heats 50min at 500 DEG C, then calcines 2h at 1100 DEG C.Finally, from
The material of sintering is taken out in high temperature furnace and room temperature is cooled in atmosphere and obtains Er3+:YAlO3Powder.
3.NaTaO3/Er3+:YAlO3Prepare：By Er3+:YAlO3And NaTaO3(mass ratio is 3 for mixing:7).It is placed on afterwards
In beaker, and 50mL deionized waters are poured into, carry out more than ultrasonic disperse 15min.Heating 30min is stirred with magnetic force at the boiling point
Mix.After reactant is with distillation water filtration and cleaning, crucible is put into, in Muffle furnace, 500 DEG C are dried 2h, 2 DEG C/min of heat rate, are obtained
To target product NaTaO3/Er3+:YAlO3。
4.Ag/NaTaO3/Er3+:YAlO3Prepare：By 1g NaTaO3/Er3+:YAlO3Powder and 0.01g silver nitrates are dissolved in
In 200mL ethanol, and using ultrasonic fully dispersed 30 minutes (80kHZ, ultrasonic power output is 50W), suspension is obtained, will be outstanding
Supernatant liquid is heated to boiling point, keeps constant temperature 30 minutes at the boiling point, and after reactant filtering and washing, the powder separated is 350
1h is calcined at DEG C, is finally ground, obtain Ag/NaTaO3/Er3+:YAlO3。
(2) characterize data
The Er of preparation3+:YAlO3XRD as shown in Figure 1a, found out by Fig. 1 a, the diffraction peak of sample and JCPDS standard cards
The data of 33-0040 are basically identical, are indicated above the sample after heat treatment and are single body-centered cubic structure, all do not occur
Other dephasigns.This explanation Er3+The doping of ion does not produce obvious influence on crystal structure.
The Er of preparation3+:YAlO3SEM as shown in Figure 1 b, found out by Fig. 1 b, gained crystal present spherical or spherical, grain
Footpath is 40-60nm, and size distribution is dispersed also preferable than more uniform.Illustrate sample preparation success.
The NaTaO of preparation3XRD as shown in Figure 2 a, found out by Fig. 2 a, NaTaO3θ=22.85 ° of characteristic peak 2 (100), 2 θ
=32.55 ° (110), 2 θ=40.23 ° (111), 2 θ=46.67 ° (200) and 2 θ=52.58 ° (210), this and NaTaO3Standard
Card (JCPDS card 74-2488) data are basically identical, and the sample being indicated above after heat treatment is single cube structure,
There are not other dephasigns.
The NaTaO of preparation3SEM as shown in Figure 2 b, found out by Fig. 2 b, NaTaO3It is cube, 220nm is long for presentation, this table
The bright NaTaO for having prepared3Crystal be shown to be (100) and (110) face.
The NaTaO of preparation3/Er3+:YAlO3XRD and SEM as best shown in figures 3 a and 3b.NaTaO can be seen that by Fig. 3 a3/
Er3+:YAlO3There is NaTaO simultaneously3And Er3+:YAlO3Characteristic peak, has no the appearance of other dephasigns, this explanation NaTaO3And Er3+:
YAlO3Compound obvious influence is not produced on crystal structure.Found out by Fig. 3 b, NaTaO3Be rendered as 220nm it is long cube
Body, light conversion agent Er3+:YAlO3It is rendered as spherical being evenly distributed in NaTaO3Cube face, illustrates that composite catalyst is prepared into
Work(.
The Ag/NaTaO of preparation3/Er3+:YAlO3XRD and SEM it is as shown in Figs. 4a and 4b.Ag/ can be seen that by Fig. 4 a
NaTaO3/Er3+:YAlO3There is NaTaO simultaneously3And Er3+:YAlO3Characteristic peak, without find Ag characteristic peak, this explanation due to
The amount of cocatalyst Ag is little and is evenly distributed in NaTaO3/Er3+:YAlO3Surface, cause it not to be checked out feature
Peak.Found out by Fig. 4 b, in NaTaO3Cube face, in addition to some spherical light conversion agents are uniform-distribution with, some fine particles
It is observed, a small amount of cocatalyst Ag of this explanation is successfully attached to catalyst surface.
(3) Cr (VI) method for transformation
In the test tube of light-catalyzed reaction instrument, 50mL Cr (VI) solution (1ppm) and 50mgAg/NaTaO are added3/Er3+:
YAlO3, under normal temperature simulated solar illumination, magnetic agitation is opened, 120min is reacted, reaction finishes, catalyst and solution is entered
Row is separated.
Cr (VI) concentration is determined with diphenyl carbazide spectrophotometry, conversion ratio is obtained and is reached more than 95%.
The catalyst Au/NaTaO of embodiment 23/Er3+:YAlO3
(1) preparation method
1.NaTaO3Prepare：With embodiment 1
2.Er3+:YAlO3Prepare：With embodiment 1
3.NaTaO3/Er3+:YAlO3Prepare：With embodiment 1
4.Au/NaTaO3/Er3+:YAlO3Prepare：By 1g NaTaO3/Er3+:YAlO3Powder and 0.01g gold chlorides are dissolved in
In 200mL ethanol, and using ultrasonic fully dispersed 30 minutes (80kHZ, ultrasonic power output is 50W), suspension is obtained, will be outstanding
Supernatant liquid is heated to boiling point, keeps constant temperature 30 minutes at the boiling point, and after filtering and washing, the powder separated is forged at 350 DEG C
1h is burnt, is finally ground, obtain Au/NaTaO3/Er3+:YAlO3。
(2) characterize data
The Au/NaTaO of preparation3/Er3+:YAlO3XRD and SEM as shown in figure 5a and 5b.Au/ can be seen that by Fig. 4 a
NaTaO3/Er3+:YAlO3There is NaTaO simultaneously3And Er3+:YAlO3Characteristic peak, without find Au characteristic peak, this explanation due to
The amount of cocatalyst Au is little and is evenly distributed in NaTaO3/Er3+:YAlO3Surface, cause it not to be checked out feature
Peak.Found out by Fig. 4 b, in NaTaO3Cube face, in addition to some spherical light conversion agents are uniform-distribution with, some fine particles
It is observed, a small amount of cocatalyst Au of this explanation is successfully attached to catalyst surface.
(3) Cr (VI) method for transformation
In the test tube of light-catalyzed reaction instrument, 50mL Cr (VI) solution (1ppm) and 50mg catalyst Au/ are added
NaTaO3/Er:YAlO3, under normal temperature simulated solar illumination, magnetic agitation is opened, 120min is reacted, reaction is finished, by catalyst
Separated with solution.
Cr (VI) concentration is determined with diphenyl carbazide spectrophotometry, conversion ratio is obtained and is reached more than 98%.
Embodiment 3Pt/NaTaO3/Er3+:YAlO3
(1) preparation method
1.NaTaO3Prepare：With embodiment 1
2.Er3+:YAlO3Prepare：With embodiment 1
3.NaTaO3/Er3+:YAlO3Prepare：With embodiment 1
4.Pt/NaTaO3/Er3+:YAlO3Prepare：By 1g NaTaO3/Er3+:YAlO3Powder and 0.01g chloroplatinic acids are dissolved in
In 200mL ethanol, and using ultrasonic fully dispersed 30 minutes (80kHZ, ultrasonic power output is 50W), suspension is obtained, will be outstanding
Supernatant liquid is heated to boiling point, keeps constant temperature 30 minutes at the boiling point, and after filtering and washing, the powder separated is forged at 350 DEG C
1h is burnt, is finally ground, obtain Pt/NaTaO3/Er3+:YAlO3。
(2) characterize data：
The Pt/NaTaO of preparation3/Er3+:YAlO3XRD and SEM as shown in figure 6 a and 6b.Pt/ can be seen that by Fig. 6 a
NaTaO3/Er3+:YAlO3There is NaTaO simultaneously3And Er3+:YAlO3Characteristic peak, without find Pt characteristic peak, this explanation due to
The amount of cocatalyst Pt is little and is evenly distributed in NaTaO3/Er3+:YAlO3Surface, cause it not to be checked out feature
Peak.Found out by Fig. 6 b, in NaTaO3Cube face, in addition to some spherical light conversion agents are uniform-distribution with, some fine particles
It is observed, a small amount of cocatalyst Pt of this explanation is successfully attached to catalyst surface.
(3) Cr (VI) method for transformation
In the test tube of light-catalyzed reaction instrument, add 50mL Cr (VI) solution (1ppm) and with 50mg catalyst Pts/
NaTaO3/Er3+:YAlO3, under normal temperature simulated solar illumination, magnetic agitation is opened, 120min is reacted, reaction is finished, will be catalyzed
Agent and solution are separated.
Cr (VI) concentration is determined with diphenyl carbazide spectrophotometry, conversion ratio is obtained and is reached more than 96%.
Claims (9)
1. one kind converts the catalyst of Cr (VI) in the aqueous solution, it is characterised in that the catalyst is X/NaTaO3/Er3+:
YAlO3, wherein, X=Ag, Au or Pt.
2. the one kind described in claim 1 converts the preparation method of the catalyst of Cr (VI) in the aqueous solution, it is characterised in that method
It is as follows：
1) by Er3+:YAlO3And NaTaO3Mixing, plus deionized water, ultrasonic disperse 15-25min；30- is heated at the boiling point
40min, and magnetic agitation, after reactant is with distillation water filtration and cleaning, 500 DEG C of heating 2-3h, obtain NaTaO in Muffle furnace3/
Er3+:YAlO3；
2) by NaTaO3/Er3+:YAlO3With the dissolving of gold chloride, chloroplatinic acid or silver nitrate in ethanol, ultrasonic disperse 30-40 minutes,
Suspension is obtained, suspension is heated to boiling point, heated 30-40 minutes under boiling point, after reactant is used distillation water filtration and is washed,
1-2h is calcined at 350 DEG C, is ground, obtain X/NaTaO3/Er3+:YAlO3；Wherein X=Ag, Au or Pt.
3. one kind according to claim 2 converts the preparation method of the catalyst of Cr (VI) in the aqueous solution, it is characterised in that
In mass ratio, Er3+:YAlO3:NaTaO3=3:7.
4. one kind according to claim 2 converts the preparation method of the catalyst of Cr (VI) in the aqueous solution, it is characterised in that
The addition of described gold chloride, chloroplatinic acid or silver nitrate is NaTaO3/Er3+:YAlO3The 1-2% of quality.
5. one kind according to claim 2 converts the preparation method of the catalyst of Cr (VI) in the aqueous solution, it is characterised in that
Described NaTaO3Preparation method be：By Ta2O5And NaOH, add water after stirring, it is transferred in hydrothermal reaction kettle, 180
15-17h is processed at DEG C, room temperature is cooled to, supernatant is abandoned, sediment is washed with deionized to neutrality, and centrifugation is dried, obtained
NaTaO3。
6. one kind according to claim 5 converts the preparation method of the catalyst of Cr (VI) in the aqueous solution, it is characterised in that
In molar ratio, Ta:Na=1:10.
7. one kind according to claim 1 converts the preparation method of the catalyst of Cr (VI) in the aqueous solution, it is characterised in that
Described Er3+:YAlO3Preparation method be：By Er2O3And Y2O3It is dissolved in concentrated nitric acid, then sequentially adds Al (NO3)3Water
Solution and aqueous citric acid solution, in 50-60 DEG C of heating stirring, stop when solution is in thick, and must foam glutinous colloidal solution, will
The glutinous colloidal solution of foaming obtains foam sol in 35-40h is heated at 75-85 DEG C, and foam sol is heated into 50- at 500 DEG C
After 60min, 2-3h is calcined at 1100 DEG C, cooling obtains Er3+:YAlO3。
8. application of the catalyst described in claim 1 in Cr (VI) in converting the aqueous solution.
9. application according to claim 8, it is characterised in that method is as follows：In the solution containing Cr (VI), power is added
Profit requires the catalyst described in 1, is irradiated under normal temperature, solar irradiation.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107335442A (en) * | 2017-06-23 | 2017-11-10 | 常州大学 | Composite photocatalyst material and its preparation method and application is changed on a kind of Er ions yttrium aluminate/concave convex rod |
| CN109078645A (en) * | 2018-09-04 | 2018-12-25 | 辽宁大学 | A kind of photochemical catalyst and its preparation method and application of novel cladding Z-type structure |
| CN112221481A (en) * | 2020-08-31 | 2021-01-15 | 广东工业大学 | Catalyst for converting Cr (VI) in water by Z-shaped structure and preparation method and application thereof |
-
2016
- 2016-11-15 CN CN201611004573.7A patent/CN106732588B/en active Active
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|---|
| CHUNXIAO LU等: ""The effect of different co-catalysts (CuO, MoS2 and Pt) on hydrogen production of Er3+:YAlO3/NaTaO3 by visible-light-induced methanol splitting"", 《ENERGY》 * |
| QIAN CHENG等: ""Hexavalent chromium removal using metal oxide photocatalysts"", 《APPLIED CATALYSIS B: ENVIRONMENTAL》 * |
| YUN LI等: ""Visible-light driven photocatalyst (Er3+:YAlO3/Pt-NaTaO3) for hydrogen production from water splitting"", 《INTERNATIONAL JOURNAL OF HYDROGEN ENERGY》 * |
| 周娴等: ""基于 Er3+：YAlO3 /TiO2的可见光催化降解室内甲醛"", 《发光学报》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107335442A (en) * | 2017-06-23 | 2017-11-10 | 常州大学 | Composite photocatalyst material and its preparation method and application is changed on a kind of Er ions yttrium aluminate/concave convex rod |
| CN109078645A (en) * | 2018-09-04 | 2018-12-25 | 辽宁大学 | A kind of photochemical catalyst and its preparation method and application of novel cladding Z-type structure |
| CN109078645B (en) * | 2018-09-04 | 2021-04-30 | 辽宁大学 | Photocatalyst coated with Z-shaped structure and preparation method and application thereof |
| CN112221481A (en) * | 2020-08-31 | 2021-01-15 | 广东工业大学 | Catalyst for converting Cr (VI) in water by Z-shaped structure and preparation method and application thereof |
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