CN111495364A - Catalyst with dark photocatalytic activity and preparation method and application thereof - Google Patents
Catalyst with dark photocatalytic activity and preparation method and application thereof Download PDFInfo
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- CN111495364A CN111495364A CN202010408312.1A CN202010408312A CN111495364A CN 111495364 A CN111495364 A CN 111495364A CN 202010408312 A CN202010408312 A CN 202010408312A CN 111495364 A CN111495364 A CN 111495364A
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- sodium bismuthate
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- 239000003054 catalyst Substances 0.000 title claims abstract description 42
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title abstract description 7
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 50
- PNYYBUOBTVHFDN-UHFFFAOYSA-N sodium bismuthate Chemical compound [Na+].[O-][Bi](=O)=O PNYYBUOBTVHFDN-UHFFFAOYSA-N 0.000 claims abstract description 33
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 11
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 9
- 238000005406 washing Methods 0.000 claims abstract description 9
- 239000002957 persistent organic pollutant Substances 0.000 claims abstract description 8
- 239000012295 chemical reaction liquid Substances 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- 239000008367 deionised water Substances 0.000 claims description 26
- 229910021641 deionized water Inorganic materials 0.000 claims description 26
- 239000000843 powder Substances 0.000 claims description 26
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims description 22
- 239000000725 suspension Substances 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000009210 therapy by ultrasound Methods 0.000 claims description 8
- 229910009112 xH2O Inorganic materials 0.000 claims description 8
- 239000002135 nanosheet Substances 0.000 claims description 4
- 230000000593 degrading effect Effects 0.000 claims description 3
- 239000002105 nanoparticle Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 10
- 238000005286 illumination Methods 0.000 abstract description 6
- 230000015556 catabolic process Effects 0.000 description 7
- 238000006731 degradation reaction Methods 0.000 description 7
- 238000002156 mixing Methods 0.000 description 6
- 239000013078 crystal Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000003915 air pollution Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 238000003911 water pollution Methods 0.000 description 2
- 101710134784 Agnoprotein Proteins 0.000 description 1
- 241000282414 Homo sapiens Species 0.000 description 1
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 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 description 1
- 229940012189 methyl orange Drugs 0.000 description 1
- 238000007709 nanocrystallization Methods 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 238000002256 photodeposition Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 229910001868 water Inorganic materials 0.000 description 1
Images
Classifications
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- 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
- B01J23/681—Silver or gold with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with arsenic, antimony or bismuth
-
- B01J35/39—
-
- B01J35/393—
-
- 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
-
- 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 invention provides a catalyst with dark photocatalytic activity and a preparation method and application thereof, wherein the method comprises the following steps of 1, 100: (3-20) reacting the mixed system of sodium bismuthate and silver nitrate under the irradiation of light to obtain a reaction solution; and 2, separating products in the reaction liquid, and then sequentially washing and drying to obtain the catalyst with dark photocatalytic activity. Under the illumination condition, the sodium bismuthate is excited to generate a photoproduction electron-hole pair, and the capacitance characteristic of the Ag simple substance enables the sodium bismuthate to store photoproduction electrons of the sodium bismuthate during illumination; under dark light, photo-generated electrons stored by the Ag simple substance are released and react with O2And H2Reaction of O molecule to generate activityO is2 ‑And OH radicals, O produced2 ‑And OH free radicals can further react with organic pollutants so as to degrade the organic pollutants, and the method has good application prospect.
Description
Technical Field
The invention belongs to the field of functional materials, and particularly relates to a catalyst with dark photocatalytic activity, and a preparation method and application thereof.
Background
At present, the environmental pollution, especially air pollution and water pollution, is more serious, and the normal life of human beings is influenced. The photocatalysis technology can be used for treating air pollution and water pollution, has good effect, takes sunlight as a driving force, has low cost and has obvious advantages.
However, most of the photocatalytic reactions reported at present can only be carried out under the condition of illumination, the illumination is stopped, and the reaction is also stopped immediately. Solar energy is a typical intermittent energy source with strong dispersive and regional characteristics. Continuous sterilization and disinfection are needed in special places such as hospitals under dark light, but the existing photocatalytic material cannot meet the practical application requirement of degrading organic pollutants under dark light.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a catalyst with dark photocatalytic activity, a preparation method and application thereof, the operation is simple, the reaction condition is mild, and the prepared Ag/NaBiO3·2H2O/NaBiO3·xH2The O catalyst can degrade organic pollutants under dark light.
The invention is realized by the following technical scheme:
a method for preparing a catalyst with dark photocatalytic activity comprises the following steps,
step 1, according to 100: (3-20) reacting the mixed system of sodium bismuthate and silver nitrate under the irradiation of light to obtain a reaction solution;
and 2, separating products in the reaction liquid, and then sequentially washing and drying to obtain the catalyst with dark photocatalytic activity.
Preferably, in the step 1, the sodium bismuthate powder is dispersed into deionized water, a brown suspension is obtained after the sodium bismuthate powder is uniformly stirred, and then silver nitrate solution dissolved by the deionized water is added into the brown suspension to obtain a mixed system of the sodium bismuthate and the silver nitrate.
Further, carrying out ultrasonic treatment on silver nitrate powder in deionized water for 30-60 min.
Preferably, in the mixed system in the step 1, the concentration of the silver nitrate is 0.15-1 g/L.
Preferably, the light in step 1 is natural light.
Preferably, the reaction described in step 1 is carried out for 0.5 to 2 h.
Preferably, in the step 2, the product in the reaction solution is washed by deionized water and absolute ethyl alcohol in sequence and then dried at the constant temperature of 70-90 ℃ for 12-18 h.
A catalyst having a dark photocatalytic activity obtained by the method for producing a catalyst having a dark photocatalytic activity according to any one of the above.
Furthermore, the catalyst is prepared from Ag and NaBiO3·2H2O/NaBiO3·xH2O, wherein Ag is in the form of nano-particles, NaBiO3·2H2O/NaBiO3·xH2O is a nanocrystallized form assembled by nanosheets.
The catalyst can degrade organic pollutants in dark light.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention relates to Ag/NaBiO with dark photocatalytic activity3·2H2O/NaBiO3·xH2Preparation method of O catalyst, sodium bismuthate and AgNO3The Ag/NaBiO with dark photocatalytic activity is prepared by a photo-deposition method3·2H2O/NaBiO3·xH2And (3) an O catalyst. AgThe simple substance has a capacitance characteristic, under the illumination condition, the sodium bismuthate is excited to generate a photoproduction electron-hole pair, and the capacitance characteristic of the Ag simple substance enables the Ag simple substance to store photoproduction electrons of the sodium bismuthate during illumination; under dark light, photo-generated electrons stored by the Ag simple substance are released and react with O2And H2O molecule reacts to form active-O2 -And OH radicals, O produced2 -And OH radicals can further react with organic contaminants, thereby degrading them. The capacitance characteristic of the Ag simple substance ensures that the prepared Ag/NaBiO3·2H2O/NaBiO3·xH2The O catalyst can degrade organic pollutants under dark light, and has good application prospect.
Drawings
FIG. 1 is an XRD pattern of the powder of the present invention, in which a-e are XRD patterns of sodium bismuthate and powders prepared in examples 1-4, respectively.
FIG. 2 is an XPS chart of catalyst powders prepared according to the present invention, wherein c and e are XPS charts of high resolution Ag 3d of powders prepared in examples 2 and 4, respectively.
FIG. 3 is an SEM image of the catalyst powder prepared in example 4 of the present invention.
FIG. 4 is a degradation curve of MO in dark light, wherein a-e are degradation diagrams of sodium bismuthate and powders prepared in examples 1-4.
Detailed Description
The present invention will now be described in further detail with reference to specific examples, which are intended to be illustrative, but not limiting, of the invention.
The invention relates to Ag/NaBiO with dark photocatalytic activity3·2H2O/NaBiO3·xH2The preparation method of the O catalyst specifically comprises the following steps,
step 1, dispersing 0.3g of sodium bismuthate powder into 30m L deionized water, and uniformly stirring to obtain a brown suspension, wherein the sodium bismuthate powder contains NaBiO3·2H2O and NaBiO3·xH2O two-phase substances;
step 2: a certain amount of AgNO3Dissolving the powder into 30m L deionized water, and performing ultrasonic treatment for 30-60min to obtain a transparent solution, AgNO3The concentration of the solution is 0.3-2 g/L;
and step 3: mixing AgNO3Slowly adding the solution into the sodium bismuthate suspension, stirring under natural light irradiation, and reacting for 0.5-2h, wherein the reaction time is short;
and 4, step 4: washing the obtained product with deionized water and anhydrous ethanol for 3-5 times, and drying at 70-90 deg.C for 12-18h to obtain Ag/NaBiO3·2H2O/NaBiO3·xH2And (3) an O catalyst.
AgNO during the reaction3And NaBiO3·2H2O/NaBiO3·xH2The mass ratio of O is 100: (3-20). Ag in the form of nano-particles, NaBiO3·2H2O/NaBiO3·xH2O is in a nanocrystallization shape formed by assembling nanosheets, organic pollutants can be degraded under the dark light, and the degradation rate of methyl orange after reaction for 30min under the dark light condition can reach 76.73% -79.22%.
Example 1:
step 1, dispersing 0.3g of sodium bismuthate powder into 30m L deionized water, and uniformly stirring to obtain a brown suspension;
step 2: 0.009g of AgNO3Dissolving the powder into 30m L deionized water, and carrying out ultrasonic treatment for 30min to obtain a transparent solution;
and step 3: mixing AgNO3Slowly adding the solution into the sodium bismuthate suspension, and stirring for 2 hours under the irradiation of natural light;
and 4, step 4: washing the obtained product with deionized water and anhydrous ethanol for 3 times respectively, and drying at constant temperature of 70 ℃ for 12h to obtain Ag/NaBiO3·2H2O/NaBiO3·xH2And (3) an O catalyst.
Example 2:
step 1, dispersing 0.3g of sodium bismuthate powder into 30m L deionized water, and uniformly stirring to obtain a brown suspension;
step 2: 0.03g of AgNO3Dissolving the powder into 30m L deionized water, and carrying out ultrasonic treatment for 50min to obtain a transparent solution;
and step 3: mixing AgNO3Slowly adding the solution into the sodium bismuthate suspension, and stirring for 1h under the irradiation of natural light;
and 4, step 4: washing the obtained product with deionized water and anhydrous ethanol for 3 times respectively, and drying at constant temperature of 70 ℃ for 12h to obtain Ag/NaBiO3·2H2O/NaBiO3·xH2And (3) an O catalyst.
Example 3:
step 1, dispersing 0.3g of sodium bismuthate powder into 30m L deionized water, and uniformly stirring to obtain a brown suspension;
step 2: 0.015g of AgNO3Dissolving the powder into 30m L deionized water, and carrying out ultrasonic treatment for 40min to obtain a transparent solution;
and step 3: mixing AgNO3Slowly adding the solution into the sodium bismuthate suspension, and stirring for 1.5 hours under the irradiation of natural light;
and 4, step 4: washing the obtained product with deionized water and anhydrous ethanol for 4 times respectively, and drying at constant temperature of 80 ℃ for 14h to obtain Ag/NaBiO3·2H2O/NaBiO3·xH2And (3) an O catalyst.
Example 4:
step 1, dispersing 0.3g of sodium bismuthate powder into 30m L deionized water, and uniformly stirring to obtain a brown suspension;
step 2: 0.06g of AgNO3Dissolving the powder into 30m L deionized water, and carrying out ultrasonic treatment for 30min to obtain a transparent solution;
and step 3: mixing AgNO3Slowly adding the solution into the sodium bismuthate suspension, and stirring for 2 hours under the irradiation of natural light;
and 4, step 4: washing the obtained product with deionized water and anhydrous ethanol for 4 times respectively, and drying at constant temperature of 80 ℃ for 12h to obtain Ag/NaBiO3·2H2O/NaBiO3·xH2And (3) an O catalyst.
Example 5:
step 1, dispersing 0.3g of sodium bismuthate powder into 30m L deionized water, and uniformly stirring to obtain a brown suspension;
step 2: 0.045g of AgNO3Dissolving the powder into 30m L deionized water, and carrying out ultrasonic treatment for 60min to obtain a transparent solution;
and step 3: mixing AgNO3Slowly adding the solution into the sodium bismuthate suspension, and stirring for 0.5h under the irradiation of natural light;
and 4, step 4: washing the obtained product with deionized water and anhydrous ethanol for 5 times respectively, and drying at constant temperature of 90 ℃ for 18h to obtain Ag/NaBiO3·2H2O/NaBiO3·xH2And (3) an O catalyst.
In fig. 1, diffraction peaks at diffraction angles 2 θ of 11.9 °, 18.3 °, 21.9 °, and 34.2 ° correspond to NaBiO respectively3·2H2The (001), (100), (101) and (111) crystal planes of O have diffraction peaks at diffraction angles 2 θ of 28.9 °, 32.2 ° and 36.4 ° corresponding to NaBiO3·xH2And (104), (110) and (113) crystal planes of O. After loading the Ag simple substance, NaBiO along with the increase of Ag loading3·2H2O and NaBiO3·xH2The main peak intensity of O gradually decreases. And NaBiO3·xH2The diffraction peak of the (104) crystal face of O is obviously enhanced, and the NaBiO is proved to be generated during the reaction3·2H2Partial conversion of O to NaBiO3·xH2O, resulting in a change in the relative amounts of the two.
The peaks at 367.38eV and 373.38eV in FIG. 2 correspond to Ag 3d, respectively5/2And Ag 3d3/2The characteristic peak of the metal Ag proves to be successfully deposited on the NaBiO3·2H2O and NaBiO3·xH2On the two phases O, i.e. the sodium bismuthate surface.
From FIG. 3, it can be seen that Ag/NaBiO3·2H2O/NaBiO3·xH2Sodium bismuthate NaBiO in O catalyst3·2H2O/NaBiO3·xH2O is in a nano state formed by self-assembly of nano sheets, and the Ag simple substance is in a nano granular state.
FIG. 4 is a graph of the degradation rate of sodium bismuthate and the catalyst powder prepared by the present invention to MO under the dark light condition versus time, in which a-e are degradation diagrams of sodium bismuthate and the powders prepared in examples 1-4 under the dark light condition, respectively. C/C of ordinate in FIG. 40Is the ratio of the concentration of the MO after degradation to its initial concentration. As can be seen from the figure, the prepared Ag/NaBiO3/NaBiO3·xH2The O catalyst showed significantly higher catalytic activity than the initial sodium bismuthate, with the Ag/NaBiO prepared in example 2, example 3 and example 43/NaBiO3·xH2After the O catalyst reacts for 30min under the dark light condition, the degradation efficiency of the MO with the initial concentration of 5 mg/L can reach 77.89%, 79.22% and 76.73%.
Claims (10)
1. A method for preparing a catalyst with dark photocatalytic activity is characterized by comprising the following steps,
step 1, according to 100: (3-20) reacting the mixed system of sodium bismuthate and silver nitrate under the irradiation of light to obtain a reaction solution;
and 2, separating products in the reaction liquid, and then sequentially washing and drying to obtain the catalyst with dark photocatalytic activity.
2. The method for preparing a catalyst with dark photocatalytic activity according to claim 1, wherein step 1 comprises dispersing sodium bismuthate powder in deionized water, stirring uniformly to obtain a brown suspension, and adding silver nitrate solution dissolved in deionized water into the brown suspension to obtain a mixed system of sodium bismuthate and silver nitrate.
3. The method for preparing the catalyst with dark photocatalytic activity according to claim 2, wherein the silver nitrate powder is subjected to ultrasonic treatment in deionized water for 30-60 min.
4. The method for preparing a catalyst with dark photocatalytic activity according to claim 1, wherein the concentration of silver nitrate in the mixed system of step 1 is 0.15-1 g/L.
5. The method of claim 1, wherein the light in step 1 is natural light.
6. The method for preparing a catalyst with dark photocatalytic activity according to claim 1, wherein the reaction in step 1 is performed for 0.5 to 2 hours.
7. The method for preparing a catalyst with dark photocatalytic activity according to claim 1, wherein in step 2, the product in the reaction solution is washed sequentially with deionized water and absolute ethanol and then dried at a constant temperature of 70-90 ℃ for 12-18 h.
8. A catalyst having a dark photocatalytic activity obtained by the method for producing a catalyst having a dark photocatalytic activity according to any one of claims 1 to 7.
9. The catalyst of claim 8, wherein the catalyst is selected from the group consisting of Ag, NaBiO3·2H2O/NaBiO3·xH2O, wherein Ag is in the form of nano-particles, NaBiO3·2H2O/NaBiO3·xH2O is a nanocrystallized form assembled by nanosheets.
10. A dark-photocatalytic-active catalyst according to claim 8 or claim 9, characterized in that the catalyst is capable of degrading organic pollutants in dark light.
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CN107744835A (en) * | 2017-10-12 | 2018-03-02 | 湖北工业大学 | A kind of preparation method of sodium bismuthate base visible light catalytic paper material |
CN108786808A (en) * | 2018-06-26 | 2018-11-13 | 陕西科技大学 | A kind of Ag/BiO2-x/Bi2O3/Bi2O2.75Composite photo-catalyst and preparation method and application |
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Title |
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