CN107159280A - A kind of catalyst for converting aqueous solution nitrite and its preparation method and application - Google Patents
A kind of catalyst for converting aqueous solution nitrite and its preparation method and application Download PDFInfo
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- CN107159280A CN107159280A CN201710350886.6A CN201710350886A CN107159280A CN 107159280 A CN107159280 A CN 107159280A CN 201710350886 A CN201710350886 A CN 201710350886A CN 107159280 A CN107159280 A CN 107159280A
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- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- 239000003054 catalyst Substances 0.000 title claims abstract description 31
- 239000007864 aqueous solution Substances 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 13
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 32
- 239000000843 powder Substances 0.000 claims description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- 238000006243 chemical reaction Methods 0.000 claims description 16
- 238000000227 grinding Methods 0.000 claims description 14
- 239000012153 distilled water Substances 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 229910001868 water Inorganic materials 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- 235000019441 ethanol Nutrition 0.000 claims description 8
- 239000006260 foam Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 7
- 150000001875 compounds Chemical class 0.000 claims description 7
- 229910004042 HAuCl4 Inorganic materials 0.000 claims description 6
- 238000013019 agitation Methods 0.000 claims description 6
- YKYOUMDCQGMQQO-UHFFFAOYSA-L cadmium dichloride Chemical compound Cl[Cd]Cl YKYOUMDCQGMQQO-UHFFFAOYSA-L 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000001556 precipitation Methods 0.000 claims description 6
- 239000000047 product Substances 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 238000005187 foaming Methods 0.000 claims description 4
- 229910021389 graphene Inorganic materials 0.000 claims description 4
- 239000000376 reactant Substances 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 239000006228 supernatant Substances 0.000 claims description 3
- 239000000725 suspension Substances 0.000 claims description 3
- 101150003085 Pdcl gene Proteins 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
- 230000002045 lasting effect Effects 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- -1 polytetrafluoroethylene Polymers 0.000 claims description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 2
- 239000002244 precipitate Substances 0.000 claims description 2
- 239000013049 sediment Substances 0.000 claims description 2
- 238000002604 ultrasonography Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 abstract description 6
- 239000003344 environmental pollutant Substances 0.000 abstract description 3
- 231100000719 pollutant Toxicity 0.000 abstract description 3
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 230000006872 improvement Effects 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 238000009835 boiling Methods 0.000 abstract 1
- 238000003912 environmental pollution Methods 0.000 abstract 1
- 238000003837 high-temperature calcination Methods 0.000 abstract 1
- 239000011941 photocatalyst Substances 0.000 abstract 1
- 238000011282 treatment Methods 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 9
- 239000013078 crystal Substances 0.000 description 7
- 229910002651 NO3 Inorganic materials 0.000 description 6
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 6
- 239000004065 semiconductor Substances 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000008279 sol Substances 0.000 description 4
- 230000036541 health Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 230000009466 transformation Effects 0.000 description 3
- 238000010792 warming Methods 0.000 description 3
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- SFOQXWSZZPWNCL-UHFFFAOYSA-K bismuth;phosphate Chemical compound [Bi+3].[O-]P([O-])([O-])=O SFOQXWSZZPWNCL-UHFFFAOYSA-K 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 235000015165 citric acid Nutrition 0.000 description 2
- 239000003651 drinking water Substances 0.000 description 2
- 235000020188 drinking water Nutrition 0.000 description 2
- 229910000474 mercury oxide Inorganic materials 0.000 description 2
- UKWHYYKOEPRTIC-UHFFFAOYSA-N mercury(ii) oxide Chemical compound [Hg]=O UKWHYYKOEPRTIC-UHFFFAOYSA-N 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000000967 suction filtration Methods 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 208000003174 Brain Neoplasms Diseases 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 108010054147 Hemoglobins Proteins 0.000 description 1
- 102000001554 Hemoglobins Human genes 0.000 description 1
- 206010020772 Hypertension Diseases 0.000 description 1
- 208000005016 Intestinal Neoplasms Diseases 0.000 description 1
- 108010061951 Methemoglobin Proteins 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 229910002666 PdCl2 Inorganic materials 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 1
- 208000005718 Stomach Neoplasms Diseases 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000357 carcinogen Toxicity 0.000 description 1
- 239000003183 carcinogenic agent Substances 0.000 description 1
- IKNAJTLCCWPIQD-UHFFFAOYSA-K cerium(3+);lanthanum(3+);neodymium(3+);oxygen(2-);phosphate Chemical compound [O-2].[La+3].[Ce+3].[Nd+3].[O-]P([O-])([O-])=O IKNAJTLCCWPIQD-UHFFFAOYSA-K 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000006184 cosolvent Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- VDQVEACBQKUUSU-UHFFFAOYSA-M disodium;sulfanide Chemical compound [Na+].[Na+].[SH-] VDQVEACBQKUUSU-UHFFFAOYSA-M 0.000 description 1
- 206010017758 gastric cancer Diseases 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 201000002313 intestinal cancer Diseases 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 208000032839 leukemia Diseases 0.000 description 1
- 229910052590 monazite Inorganic materials 0.000 description 1
- 239000000618 nitrogen fertilizer Substances 0.000 description 1
- XKLJHFLUAHKGGU-UHFFFAOYSA-N nitrous amide Chemical compound ON=N XKLJHFLUAHKGGU-UHFFFAOYSA-N 0.000 description 1
- GQPLMRYTRLFLPF-UHFFFAOYSA-N nitrous oxide Inorganic materials [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 239000011236 particulate material Substances 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 229910052979 sodium sulfide Inorganic materials 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 201000011549 stomach cancer Diseases 0.000 description 1
- 238000003786 synthesis reaction Methods 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
- 238000011426 transformation method Methods 0.000 description 1
- 239000012780 transparent material 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/186—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
-
- B01J35/39—
-
- 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
- C02F2101/10—Inorganic compounds
- C02F2101/16—Nitrogen compounds, e.g. ammonia
- C02F2101/166—Nitrites
-
- 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
-
- 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
Abstract
The present invention relates to a kind of catalyst for converting aqueous solution nitrite and its preparation method and application.The technical scheme of use is：It is prepared for turning light luminescent material Er using sol-gal process3+:YAlO3, Er has been respectively synthesized followed by hydro-thermal method3+:YAlO3@BiPO4And CdS.Finally, new sunlight catalytic system Er has been synthesized with boiling liquid method and high-temperature calcination3+:YAlO3@(PdS/BiPO4)/(Au/rGO)/CdS.Under sunshine irradiation, with improvement Z-type Er3+:YAlO3@(PdS/BiPO4)/(Au/rGO)/CdS photocatalyst treatments nitrite and other pollutants.The inventive method is simply novel, and cost is low, 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 the synthesis of new catalyst and utilization catalyst are to the water body Central Asia
The method that nitrate is converted.
Background technology
In nature, nitrite is typically the product that ammonia is aoxidized generation by nitrite bacteria, is also nitrate degraded
During metastable intermediate product.With developing rapidly for modern industry and agricultural, the concentration of Nitrite by
In the excess emissions of trade effluent, the excessive use of nitrogenous fertilizer and incomplete abiotic denitrification process and significantly rise.Nitrous
Hydrochlorate is a kind of inorganic environment pollutant for having very big toxicity to health.Once excess intake, nitrite will be with blood
Hemoglobin in liquid is combined, and ferrihemoglobin is generated, so as to cause human body to be poisoned.In addition, the excessive nitrite of intake
Carcinogen nitrosamine can be changed into vivo, cause the diseases such as hypertension, stomach cancer, intestinal cancer, leukaemia and brain tumor.Cause
This, the World Health Organization proposes, the nitrite concentration peak in drinking water is 3mg/L.In order to meet health demand, remove
Nitrite in drinking water is very necessary.
Photocatalysis technology because its can directly using absorb light remove water body in pollutant and easily separated reuse and by
Extensive concern.This characteristic is mainly appeared in metal oxide and combined metal oxide semiconductor, such as TiO2Because of it
Catalytic activity is of a relatively high, and physicochemical properties are stable, and are widely used.However, for removing the natrium nitrosum in water body,
The semiconductor for needing selection one to have compared with Strong oxdiative ability and reducing power, is acid group and ammonia by Nitrite transformation, this is just
It is required that one of a relatively high conduction band of selection and the broadband semiconductor of relatively low valence band.By inquiry, bismuth phosphate is as a kind of new
Type nonmetal oxyacid acid group semiconductor, there is three kinds of principal crystalline phase structures：Monoclinic phase, monoclinic phase monazite and hexagonal phase.But make
For a broadband semiconductor, bismuth phosphate is absorbed the poor ability of sunshine, the photon energy can only be obtained using ultraviolet light, and purple
Outer light only accounts for the 5% of solar spectrum, and this makes the utilization rate of solar energy become minimum.In order to obtain higher solar energy utilization ratio,
Must develop can utilize the catalyst of visible ray.
The content of the invention
It is an object of the invention to design to synthesize a kind of new catalyst Er that can be used for converting aqueous solution nitrite3 +:YAlO3@(PdS/BiPO4)/(Au/rGO)/CdS.Compound involved in the present invention belongs to new catalyst, is applied to Asia
Nitrate transformation, method is simple, pollution-free, catalyst stabilization and is easily isolated.
The technical solution adopted by the present invention is as follows：A kind of catalyst for converting aqueous solution nitrite, the catalyst
For Er3+:YAlO3@(PdS/BiPO4)/(Au/rGO)/CdS。
A kind of preparation method of the catalyst of above-mentioned conversion aqueous solution nitrite, method is as follows：
1) under magnetic agitation, by Er3+:YAlO3@BiPO4Powder is distributed to Na2In S solution, PdCl is then added dropwise2It is molten
Liquid, reacts 10-15min.By centrifugation, precipitation is cleaned with distilled water, 60 degrees Celsius dry 10 hours.By obtained powder in horse
Not calcined 3-4 hours at 180-220 DEG C in stove, cooling obtains Er3+:YAlO3@(PdS/BiPO4) compound；
2) graphene oxide (GO) and N are added in alcohol2H4·H2O, ultrasonic disperse 50-60min, obtain rGO solution, so
After sequentially add HAuCl4·4H2O and Er3+:YAlO3@(PdS/BiPO4) compound, ultrasonic disperse 2-3h, reactant is scrubbed,
After drying, grinding calcines 2-3h at 180-220 DEG C in Muffle furnace, obtains Er3+:YAlO3@(PdS/BiPO4)/(Au/rGO) powder
End；
3) graphene oxide (GO) and N are added in alcohol2H4·H2O, ultrasonic disperse 50-60min, is then sequentially added
HAuCl4·4H2O and CdS, ultrasonic disperse 2-3h, reactant is scrubbed, after drying, grinding, in Muffle furnace at 180-220 DEG C
2-3h is calcined, (Au/rGO)/CdS powder is obtained；
4) by Er3+:YAlO3@(PdS/BiPO4)/(Au/rGO) powder and (Au/rGO)/CdS powder add in alcohol, surpass
Sound disperses 50-60min, filtering, precipitates scrubbed, after drying, and grinding is placed in 2000-2500 DEG C of Muffle furnace and calcines 2-3h, obtains
Er3+:YAlO3@(PdS/BiPO4)/(Au/rGO)/CdS powder.
A kind of preparation method of the catalyst of above-mentioned conversion aqueous solution nitrite, in mass ratio, Er3+:YAlO3@
(PdS/BiPO4)/(Au/rGO):(Au/rGO)/CdS=1:1.
A kind of preparation method of the catalyst of above-mentioned conversion aqueous solution nitrite, described Er3+:YAlO3@
BiPO4Preparation method be：By H3PO4With Bi (NO3)3·6H2O is mixed, and magnetic agitation 1-2h, obtains suspension, so at room temperature
Afterwards, Er is added3+:YAlO3, 1-2h is persistently stirred, mixed liquor is transferred in hydrothermal reaction kettle, 70- is reacted under the conditions of 100 DEG C
75h, is cooled to room temperature, abandons supernatant, and sediment is washed with deionized to neutrality, dries, obtain Er3+:YAlO3@BiPO4。
A kind of preparation method of the catalyst of above-mentioned conversion aqueous solution nitrite, described CdS preparation method
It is：By CdCl2·2.5H2O is dissolved in distilled water, adds Na2The S aqueous solution, persistently stirs after 30-40min, is transferred to polytetrafluoro
In ethene bushing, it is put into baking oven, at 100 DEG C, is incubated 4-5h, natural cooling, suction filtration is washed with distilled water and absolute ethyl alcohol
Wash, product is dried, grinding obtains CdS powder.
A kind of preparation method of the catalyst of above-mentioned conversion aqueous solution nitrite, described Er3+:YAlO3System
Preparation 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, stop when solution is in thick, must foam glutinous colloidal solution, foaming is sticked into colloidal solution in 75-
35-40h is heated at 85 DEG C, foam sol is obtained, foam sol is heated after 50-60min at 500 DEG C, 2- is calcined at 1100 DEG C
3h, cooling, obtains Er3+:YAlO3。
Application of the above-mentioned catalyst in conversion aqueous solution nitrite.Method is as follows：In containing nitrite
In solution, the catalyst described in claim 1 is added, is irradiated under normal temperature, solar irradiation
A kind of application of above-mentioned conversion aqueous solution nitrite, method is as follows：In the solution containing nitrite,
Add catalyst improvement Z-type Er3+:YAlO3@(PdS/BiPO4)/(Au/rGO)/CdS, irradiates under normal temperature, solar irradiation.
The beneficial effects of the invention are as follows：The present invention have studied on the basis of a variety of photocatalysis technologies for nitrite
To improve Z-type Er3+:YAlO3@(PdS/BiPO4)/(Au/rGO) skill of Nitrite transformation is carried out based on/CdS nano-complexes
Art.By the method for the present invention, nitrite concentration can be down to below 3ppm, without influenceing other quality index.With it is other
Photocatalysis technology is compared, and process of the present invention is simple, and normal temperature and pressure is carried out, mild condition, and using solar energy, nitrite
Conversion ratio reaches more than 90%.
Brief description of the drawings
Fig. 1 a are Er3+:YAlO3XRD.
Fig. 1 b are Er3+:YAlO3SEM figure.
Fig. 2 a are Er3+:YAlO3@BiPO4XRD.
Fig. 2 b are Er3+:YAlO3@BiPO4SEM figure.
Fig. 3 a are Er3+:YAlO3@(PdS/BiPO4) XRD.
Fig. 3 b are Er3+:YAlO3@(PdS/BiPO4) SEM figure.
Fig. 4 a are Er3+:YAlO3@(PdS/BiPO4)/(Au/rGO) XRD.
Fig. 4 b are Er3+:YAlO3@(PdS/BiPO4)/(Au/rGO) SEM figure.
Fig. 5 a are CdS XRDs.
Fig. 5 b are CdS SEM figures.
Fig. 6 a are (Au/rGO)/CdS XRDs.
Fig. 6 b are (Au/rGO)/CdS SEM figures.
Fig. 7 a are Er3+:YAlO3@(PdS/BiPO4)/(Au/rGO)/CdS powder XRD.
Fig. 7 b are Er3+:YAlO3@(PdS/BiPO4)/(Au/rGO)/CdS powder SEM figure.
Embodiment
(1) preparation of the catalyst of conversion aqueous solution nitrite
1.Er3+:YAlO3Prepare：By 0.0464g Er2O3、2.7281g Y2O3Dissolved under conditions of magnetic force heating stirring
In 250ml concentrated nitric acids, water white transparency is stirred continuously until, earth solution is obtained.Weigh 9.0633g Al (NO3)3·9H2O is simultaneously molten
Solution under normal temperature condition, is stirred with glass bar, is then slowly added in earth solution in distilled water.Weigh
30.4649g citric acids are dissolved in the beaker equipped with distilled water as chelating agent and cosolvent, are stirring evenly and then adding into
State in mixed solution.Then, by above-mentioned mixed solution, continuous heating is stirred under the conditions of 50-60 DEG C, when solution is in thick
Stop, must foaming glutinous colloidal solution, then the glutinous colloidal solution of above-mentioned gained foaming is placed in air dry oven, 80 DEG C of constant temperature
Heat drying 36h, obtains foam sol.By obtained foam sol, it is put into Muffle furnace and heats 50min under the conditions of 500 DEG C, so
Muffle furnace is warming up to 1100 DEG C afterwards and 2h is calcined, cooled down, grinding obtains Er3+:YAlO3Powder.
2.Er3+:YAlO3@BiPO4Prepare：By 100mL H3PO4(12M) pours into beaker, the Bi (NO with 10mmol3)3·
6H2O is mixed, and magnetic agitation 1h, obtains suspension at room temperature, then, according to Er3+:YAlO3And BiPO4Mass ratio 0.3:1.0
Ratio, by Er3+:YAlO3Add in above-mentioned mixed liquor, lasting stirring.After 1.0h to be mixed is well mixed to solution, it will mix
Liquid is transferred in 50ml hydrothermal reaction kettles, and 72h is reacted under the conditions of 100 DEG C.Question response is completed, after reactor natural cooling, will
Supernatant is outwelled, and is left reaction gained white powder, is washed with deionized to neutrality, 12h is dried under the conditions of 60 DEG C, is ground
Mill, obtains Er3+:YAlO3@BiPO4Powder, is collected standby.
It is prepared by 3.CdS：Weigh 6.0mmol CdCl2·2.5H2O is dissolved in 40mL distilled water.By 6.0mmol Na2S is dissolved in
It is slowly added into dropwise in above-mentioned solution after appropriate distilled water, has orange-yellow precipitation generation, persistently stir 30min, then, will
Precipitation and solution are transferred in 50mL polytetrafluoroethylene bushings in the lump, and charge weight is no more than the 80% of capacity.By this polytetrafluoroethyl-ne
Alkene bushing is put into stainless steel cauldron, and reactor is put into baking oven, and baking oven is warming up to 100 DEG C, keeps this temperature 4 hours.Instead
After the completion of answering, natural cooling further takes out reactor, has bright yellow mercury oxide to occur, this yellow mercury oxide is transferred in Buchner funnel,
Suction filtration, and washed several times with distilled water and absolute ethyl alcohol, product is put into baking oven, is warming up to 80 DEG C, keeps this temperature 3 hours, grinding,
Obtain CdS powder.
4.Er3+:YAlO3@(PdS/BiPO4) compound preparation：Under the conditions of magnetic agitation, by 1.00g Er3+:YAlO3@
BiPO4Powder is distributed to 90ml PdCl2In solution (11mmol/L), then, 2ml Na are added dropwise2S solution (0.50mol/
L), 10-15min is reacted, centrifugation cleans precipitation with distilled water, after 60 DEG C dry 10 hours, product is forged for 200 DEG C in Muffle furnace
Burn 3 hours, cooling obtains Er3+:YAlO3@(PdS/BiPO4) compound.
5.Er3+:YAlO3@(PdS/BiPO4)/(Au/rGO) prepare：By 4.0mL GO (3.00mg/mL) and 0.461mL
N2H4·H2O (85%) is added in 16mL alcohol, ultrasonic disperse 60min (frequencies:80kHz, power output:50W), rGO is obtained molten
Liquid.Then, by HAuCl4·4H2O (97%) and 1.00g Er3+:YAlO3@(PdS/BiPO4) the above-mentioned rGO solution of powder addition
In, ultrasonic fully dispersed 2h.Finally, the mixture obtained for several times with alcohol washes, then 60 DEG C of drying, 12 hours are by grinding
Afterwards, it is put into 200 DEG C of Muffle furnace to calcine 2 hours, obtains Er3+:YAlO3@(PdS/BiPO4)/(Au/rGO) powder.
(6. Au/rGO)/CdS preparation：By 4.0mL GO (3.00mg/mL) and 0.461mL N2H4·H2O (85%) adds
Enter 16mL alcohol, 60 minutes (frequencies of ultrasonic disperse:80kHz, power output:50W), rGO solution is obtained.Then, by HAuCl4·
4H2O (97%) and 1.00g CdS powder are added in above-mentioned rGO solution, fully dispersed 2 hours of ultrasound.Finally, alcohol washes are used
The mixture obtained for several times, is then dried 12 hours for 60 DEG C, after grinding, is put into 200 DEG C of Muffle furnace and is calcined 2 hours, obtains (Au/
rGO)/CdS。
7. by 1.0g Er3+:YAlO3@(PdS/BiPO4) and 1.0g (Au/rGO)/CdS added in alcohol, ultrasonic disperse
50-60min.Filtering, gained precipitation is respectively washed 3 times with deionized water and alcohol, then 12h is dried under the conditions of 60 DEG C,
After grinding, it is placed in 2000 DEG C of Muffle furnaces and calcines 2h, after reaction terminates, grinding is collected, and obtains Er3+:YAlO3@(PdS/BiPO4)/
(Au/rGO)/CdS powder.
(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
33-0040 data are basically identical, and the sample being indicated above after heat treatment is single body-centered cubic structure, is not all occurred
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, shape is presented in irregular side in gained crystal
Shape, Average Particle Diameters are in 80nm.Size distribution is dispersed also preferable than more uniform.Illustrate sample preparation success.
The Er of preparation3+:YAlO3@BiPO4XRD as shown in Figure 2 a, found out by Fig. 2 a, BiPO4θ=18.13 ° of characteristic peak 2
(- 101), 2 θ=22.32 ° (- 111), 2 θ=26.03 ° (110), and 2 θ=29.58 ° (200), 2 θ=34.82 ° (- 202), 2 θ=
46.98 ° (301), 2 θ=49.24 (212) and 2 θ=53.25 ° (203) this and BiPO4Standard card (JCPDS card No.80-
0209) data are basically identical, and it is monoclinic crystal structure to be indicated above the sample after processing, other dephasigns does not occur.
The Er of preparation3+:YAlO3@BiPO4SEM as shown in Figure 2 b, found out by Fig. 2 b, Er3+:YAlO3And BiPO4Well
Form clad structure.The BiPO of preparation4Crystal is about 300nm.
The Er of preparation3+:YAlO3@(PdS/BiPO4) XRD and SEM as best shown in figures 3 a and 3b.The Er it can be seen from Fig. 3 a3 +:YAlO3@(PdS/BiPO4) while having Er3+:YAlO3And BiPO4Characteristic peak, have no other dephasigns appearance, this explanation Er3 +:YAlO3And BiPO4Compound obvious influence is not produced on crystal structure.Found out by Fig. 3 b, BiPO4Area load one
A little about 30nm particle, these particles are PdS.Illustrate that composite catalyst is successfully prepared.
The Er of preparation3+:YAlO3@(PdS/BiPO4)/(Au/rGO) XRD and SEM it is as shown in Figs. 4a and 4b.Can by Fig. 4 a
To find out, Er3+:YAlO3@(PdS/BiPO4)/(Au/rGO) while having Er3+:YAlO3And BiPO4Characteristic peak, and do not find
The obvious characteristic peak for representing PdS, Au and rGO, this is probably due to the small test limit arrived less than XRD spectrum of their usage amount.
Found out by Fig. 4 b, Er3+:YAlO3@(PdS/BiPO4) surface covered by rGO, the particulate material for having some small is distributed in above,
Belong to Au particles.This shows Er3+:YAlO3@(PdS/BiPO4)/(Au/rGO) formed well.
The CdS of preparation XRD and SEM is as shown in figure 5a and 5b.θ=24.91 ° of CdS characteristic peaks 2 it can be seen from Fig. 5 a
(100), 2 θ=26.52 ° (002), 2 θ=28.34 ° (101), 2 θ=37.01 ° (102), 2 θ=43.85 ° (110), 2 θ=
48.17 ° (103) and 2 θ=52.3 ° (112) and CdS standard cards (JCPDS No.41-1049) data are basically identical, thus table
There are not other dephasigns in sample after the reason of daylight.Find out there are many uniform spherical crystal particles in figure by Fig. 5 b, diameter exists
Between 40-60nm, this belongs to traditional crystal form of the CdS particles of Nano grade.
(the Au/rGO)/CdS prepared XRD and SEM is as shown in figure 6 a and 6b.It can not find in way it can be seen from Fig. 6 a
The obvious characteristic peak for representing Au and rGO, this is probably due to the small test limit arrived less than XRD spectrum of their usage amount.They
Presence other detection method will be used to be identified.Found out by Fig. 6 b, CdS and Au particles are both dispersed on rGO.This shows
(Au/rGO)/CdS is successfully prepared.
The Er of preparation3+:YAlO3@(PdS/BiPO4)/(Au/rGO)/CdS XRD and SEM as illustrated in figs. 7 a and 7b.By scheming
7a can be seen that up-conversion luminescent material Er3+:YAlO3Characteristic peak and BiPO4Characteristic peak.Found out by Fig. 7 b, Er3+:
YAlO3@(PdS/BiPO4)/(Au/rGO)/CdS configuration, be made up of different particles, can be clearly from figure
Go out, CdS and Au particles are distributed in Er3+:YAlO3@(PdS/BiPO4) on surface.RGO is because be transparent material, it is more difficult to distinguished
Not.
(3) Nitrite transformation method
In the test tube of light-catalyzed reaction instrument, 50mL natrium nitrosums (NaNO is added2) solution (10.0ppm) and 50mg Er3 +:YAlO3@(PdS/BiPO4)/(Au/rGO)/CdS, under normal temperature simulated solar illumination, magnetic agitation is opened, 120min is reacted,
Reaction is finished, and catalyst and solution are separated.
With liquid chromatogram measuring aqueous solution nitrite concentration, conversion ratio is more than 90%.
Claims (8)
1. a kind of catalyst for converting aqueous solution nitrite, it is characterised in that described catalyst is Er3+:YAlO3@
(PdS/BiPO4)/(Au/rGO)/CdS。
2. a kind of preparation method of the catalyst of conversion aqueous solution nitrite described in claim 1, it is characterised in that side
Method is as follows：
1) under magnetic agitation, by Er3+:YAlO3@BiPO4Powder is distributed to Na2In S solution, PdCl is then added dropwise2Solution,
React 10-15min；By centrifugation, precipitation is cleaned with distilled water, 60 degrees Celsius dry 10 hours；By obtained powder in Muffle
Calcined 3-4 hours at 180-220 DEG C in stove, cooling obtains Er3+:YAlO3@(PdS/BiPO4) compound；
2) graphene oxide and N are added in alcohol2H4·H2O, ultrasonic disperse 50-60min, then sequentially adds HAuCl4·
4H2O and Er3+:YAlO3@(PdS/BiPO4) compound, ultrasonic disperse 2-3h, reactant is scrubbed, after drying, grinding, in Muffle
2-3h is calcined at 180-220 DEG C in stove, Er is obtained3+:YAlO3@(PdS/BiPO4)/(Au/rGO) powder；
3) graphene oxide and N are added in alcohol2H4·H2O, ultrasonic disperse 50-60min, then sequentially adds HAuCl4·
4H2O and CdS, ultrasonic disperse 2-3h, reactant is scrubbed, after drying, and grinding calcines 2- in Muffle furnace at 180-220 DEG C
3h, obtains (Au/rGO)/CdS powder；
4) by Er3+:YAlO3@(PdS/BiPO4)/(Au/rGO) powder is with (Au/rGO)/CdS powder addition alcohol, and ultrasound is divided
50-60min is dissipated, filtering precipitates scrubbed, after drying, and grinding is placed in 2000-2500 DEG C of Muffle furnace and calcines 2-3h, obtains Er3+:
YAlO3@(PdS/BiPO4)/(Au/rGO)/CdS powder.
3. a kind of preparation method of catalyst for converting aqueous solution nitrite according to claim 2, its feature exists
In, in mass ratio, Er3+:YAlO3@(PdS/BiPO4)/(Au/rGO):(Au/rGO)/CdS=1:1.
4. a kind of preparation method of catalyst for converting aqueous solution nitrite according to claim 2, its feature exists
In described Er3+:YAlO3@BiPO4Preparation method be：By H3PO4With Bi (NO3)3·6H2O is mixed, and magnetic force is stirred at room temperature
1-2h is mixed, suspension is obtained, then, Er is added3+:YAlO3, 1-2h is persistently stirred, mixed liquor is transferred in hydrothermal reaction kettle,
70-75h is reacted under the conditions of 100 DEG C, room temperature is cooled to, supernatant is abandoned, sediment is washed with deionized to neutrality, dries, obtain
Er3+:YAlO3@BiPO4。
5. a kind of preparation method of catalyst for converting aqueous solution nitrite according to claim 2, its feature exists
In described CdS preparation method is：By CdCl2·2.5H2O is dissolved in distilled water, adds Na2The S aqueous solution, lasting stirring
After 30-40min, it is transferred in polytetrafluoroethylene bushing, is put into baking oven, at 100 DEG C, is incubated 4-5h, natural cooling is taken out
Filter, is washed with distilled water and absolute ethyl alcohol, and product is dried, and grinding obtains CdS powder.
6. a kind of preparation method of catalyst for converting aqueous solution nitrite according to claim 2, its feature exists
In described Er3+:YAlO3Preparation method be：By Er2O3And Y2O3It is dissolved in concentrated nitric acid, then sequentially adds Al (NO3)3
The aqueous 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,
By the glutinous colloidal solution of foaming in heating 35-40h at 75-85 DEG C, foam sol is obtained, foam sol is heated into 50- at 500 DEG C
After 60min, 2-3h is calcined at 1100 DEG C, cooling obtains Er3+:YAlO3。
7. application of the catalyst in conversion aqueous solution nitrite described in claim 1.
8. application according to claim 8, it is characterised in that method is as follows：In the solution containing nitrite, add
Catalyst described in claim 1, irradiates under normal temperature, solar irradiation.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109433273A (en) * | 2018-12-18 | 2019-03-08 | 辽宁大学 | A kind of novel photocatalyst NiGa2O4/AQ/MoO3And its preparation method and application |
| CN110670075A (en) * | 2019-10-24 | 2020-01-10 | 莫林祥 | La2O3Photoanode composite material with-CdS photo-induced cathodic protection performance |
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| CN103084197A (en) * | 2013-01-21 | 2013-05-08 | 辽宁大学 | Er<3+>:Yb0.20Y2.80Al5N0.10F0.10O11.80/Pt-TiO2 photocatalyst and application thereof to preparation of hydrogen by splitting water under photocatalysis |
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2017
- 2017-05-18 CN CN201710350886.6A patent/CN107159280A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103084197A (en) * | 2013-01-21 | 2013-05-08 | 辽宁大学 | Er<3+>:Yb0.20Y2.80Al5N0.10F0.10O11.80/Pt-TiO2 photocatalyst and application thereof to preparation of hydrogen by splitting water under photocatalysis |
Non-Patent Citations (1)
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|---|
| YIDI WANG ET AL.: "Amodified Z-scheme Er3+:YAlO3@(PdS/BiPO4)/(Au/rGO)/CdS photocatalyst for enhanced solar-light photocatalytic conversion of nitrite", 《CHEMICAL ENGINEERING JOURNAL》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109433273A (en) * | 2018-12-18 | 2019-03-08 | 辽宁大学 | A kind of novel photocatalyst NiGa2O4/AQ/MoO3And its preparation method and application |
| CN109433273B (en) * | 2018-12-18 | 2021-08-24 | 辽宁大学 | Photocatalyst NiGa2O4/AQ/MoO3And preparation method and application thereof |
| CN110670075A (en) * | 2019-10-24 | 2020-01-10 | 莫林祥 | La2O3Photoanode composite material with-CdS photo-induced cathodic protection performance |
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Inventor after: Song Youtao Inventor after: Lan Yu Inventor after: Wang Yidi Inventor after: Wang Jun Inventor before: Lan Yu Inventor before: Wang Yidi Inventor before: Song Youtao Inventor before: Wang Jun |
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Application publication date: 20170915 |