CN115957744B - ZnWO (zinc-oxygen) device 4 Preparation method and application of photocatalyst - Google Patents
ZnWO (zinc-oxygen) device 4 Preparation method and application of photocatalyst Download PDFInfo
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- CN115957744B CN115957744B CN202310043350.5A CN202310043350A CN115957744B CN 115957744 B CN115957744 B CN 115957744B CN 202310043350 A CN202310043350 A CN 202310043350A CN 115957744 B CN115957744 B CN 115957744B
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- ammonium tungstate
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims description 4
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000001257 hydrogen Substances 0.000 claims abstract description 14
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 14
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 13
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 10
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims abstract description 9
- 235000002906 tartaric acid Nutrition 0.000 claims abstract description 9
- 239000011975 tartaric acid Substances 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- 238000001354 calcination Methods 0.000 claims abstract description 5
- 238000000227 grinding Methods 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 230000001007 puffing effect Effects 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 27
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- 239000007789 gas Substances 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 8
- YZYKBQUWMPUVEN-UHFFFAOYSA-N zafuleptine Chemical compound OC(=O)CCCCCC(C(C)C)NCC1=CC=C(F)C=C1 YZYKBQUWMPUVEN-UHFFFAOYSA-N 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- 238000013375 chromatographic separation Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 239000011701 zinc Substances 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 12
- 239000000463 material Substances 0.000 abstract description 3
- 230000033116 oxidation-reduction process Effects 0.000 abstract description 2
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 abstract 1
- 230000003197 catalytic effect Effects 0.000 abstract 1
- 239000004246 zinc acetate Substances 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 6
- 238000004817 gas chromatography Methods 0.000 description 4
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 3
- MKYBYDHXWVHEJW-UHFFFAOYSA-N N-[1-oxo-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propan-2-yl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(C(C)NC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 MKYBYDHXWVHEJW-UHFFFAOYSA-N 0.000 description 3
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 3
- -1 tungstate radicals Chemical class 0.000 description 3
- 229910001930 tungsten oxide Inorganic materials 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 150000002978 peroxides Chemical class 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000003421 catalytic decomposition reaction Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000010526 radical polymerization reaction Methods 0.000 description 1
- 239000013074 reference sample Substances 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 229940095064 tartrate Drugs 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention relates to a ZnWO 4 A preparation method and application of a photocatalyst belong to the technical field of photocatalytic materials. The preparation method comprises the following steps: stirring ammonium tungstate in hydrogen peroxide solution until dissolving, dissolving zinc acetate in deionized water, adding tartaric acid, stirring until dissolving, mixing the two solutions, stirring, placing in a baking oven, drying and puffing the sample, grinding, placing in a muffle furnace for calcination, washing, and drying to obtain ZnWO 4 A photocatalyst. The invention has stronger photocatalytic oxidation-reduction capability, increases visible light catalytic activity, has better photocatalytic hydrogen evolution performance, and has great development and application prospects in the aspect of photocatalytic green clean energy.
Description
Technical Field
The invention belongs to the technical field of photocatalytic materials, and in particular relates to a ZnWO 4 A preparation method and application of a photocatalyst.
Background
The photocatalysis technology is a technology for converting solar energy into high added value chemicals, and has good application potential in the aspects of developing clean energy, relieving increasingly serious energy crisis and environmental problems. Solar photocatalytic water splitting to produce hydrogen and convert and store solar energy in a clean, efficient, low-cost and large-scale manner has become one of the most important subjects in the field of energy research.
ZnWO 4 Is a common photocatalyst, is applied to the fields of environment and energy due to the excellent stability, but ZnWO 4 As a hydrogen evolution photocatalyst, no report has been made yet, and ZnWO 4 The photocatalyst has the advantages of fewer preparation methods, single preparation material, and quicker photo-generated carrier recombination, so that the photocatalyst has poorer photocatalytic performance.
Disclosure of Invention
In order to solve the defects in the prior art, the invention provides a ZnWO 4 A preparation method and application of a photocatalyst.
The invention adopts the technical scheme that:
ZnWO (zinc-oxygen) device 4 The preparation method of the photocatalyst comprises the following steps: stirring ammonium tungstate in a hydrogen peroxide solution until the ammonium tungstate is dissolved to obtain a solution A; dissolving zinc acetate dihydrate in deionized water, adding tartaric acid, and stirring until the solution is dissolved to obtain a solution B; mixing the solution A and the solution B, stirring, placing in a baking oven, drying, puffing, grinding, placing in a muffle furnace for calcining, naturally cooling, washing, centrifuging, and drying at 60deg.C to obtain ZnWO 4 A photocatalyst.
Further, a ZnWO as described above 4 Preparation method of photocatalyst, wherein the ammonium tungstate is hydrated ammonium tungstate, and molecular formula is H 40 N 10 O 41 W 12 ·xH 2 O, molecular weight 3042.58.
Further, a ZnWO as described above 4 The preparation method of the photocatalyst comprises the steps of adding ammonium tungstate hydrate, zinc acetate dihydrate and tartaric acid according to a molar ratio of W to Zn to tartaric acid=1:1:3.
Further, a ZnWO as described above 4 A method for preparing a photocatalyst, wherein the concentration of the hydrogen peroxide solution is 30%.
Further, a ZnWO as described above 4 The temperature of the oven is set to be 80 ℃.
Further, a ZnWO as described above 4 Preparation of photocatalystA method, wherein the calcining conditions are as follows: heating to 400 ℃ at 2 ℃/min, heating to 600 ℃ at 1 ℃/min, and maintaining at 600 ℃ for 240min.
ZnWO prepared by the preparation method of any one of the above 4 The application of the photocatalyst in catalyzing hydrogen evolution under the irradiation of visible light.
Further, the application method comprises the following steps: under normal temperature and pressure, 20mL of aqueous methanol solution, 20. Mu.L of aqueous chloroplatinic acid solution and then 20mg of ZnWO are added to a vessel 4 Photocatalyst, ultrasonic for 10min, dispersing liquid; argon is introduced into the container at the rate of 40mL/min for 30min, the container is sealed, 1000 mu L of the gas in the container is taken out by a microinjector every 15min under the condition of visible light irradiation, and the gas component is detected by a gas chromatographic separation technology method to determine the concentration of hydrogen evolution.
Further, in the above application, the concentration of the aqueous methanol solution is 1.25mol/L.
Further, in the above application, the concentration of the aqueous solution of chloroplatinic acid is 1% by weight.
The beneficial effects of the invention are as follows:
1. ZnWO of the invention 4 In the preparation process of the photocatalyst, the hydrogen peroxide solution can be used for dissolving a large amount of ammonium tungstate which is almost insoluble in other solutions, and the peroxy radical is used as an initiator, so that free radical polymerization can be promoted, and zinc ions and tungstate radicals can be better complexed by tartrate radicals. In addition, the peroxy radical can inhibit the transition from tungstate radical to tungsten oxide crystal phase.
2. ZnWO of the invention 4 The photocatalyst has better photocatalytic performance, ammonium tungstate is dissolved in hydrogen peroxide solution, peroxide can be provided by hydrogen peroxide, and due to the existence of the peroxide, exciton dissociation is induced to generate holes, so that the generation of photo-generated carriers is promoted, the hole electron recombination time is inhibited, and the photocatalytic performance and the solar energy utilization efficiency are improved.
3. ZnWO of the invention 4 The photocatalyst has better photocatalytic water splitting and hydrogen separating performance, and ZnWO is adopted at present 4 The method has not been reported in the field of photocatalytic hydrogen evolution, and has the advantages of simple and convenient operation, low cost,The conditions are mild, and the large-scale production is facilitated.
Drawings
FIG. 1 shows ZnWO prepared in example 1 4 ZnWO prepared in example 2 4 -2 XRD pattern of the photocatalyst.
FIG. 2 shows ZnWO prepared in example 1 4 ZnWO prepared in example 2 4 -2 hydrogen evolution contrast schematic of photocatalyst.
FIG. 3 shows different H's detected by gas chromatography 2 And (3) a graph of the relationship between the volume and the gas chromatographic peak area.
Detailed Description
Example 1
ZnWO 4 The preparation method of the photocatalyst comprises the following steps:
2.55g of ammonium tungstate hydrate is stirred in 20mL of 30% hydrogen peroxide solution to be dissolved, so as to obtain solution A; 2.19g of zinc acetate dihydrate is dissolved in 10mL of deionized water, and 4.5g of tartaric acid is added and stirred until dissolved, so as to obtain a solution B; then mixing the solution A and the solution B, stirring, placing in an oven at 80 ℃, drying and puffing the sample, grinding, placing in a muffle furnace, heating to 400 ℃ at 2 ℃/min, heating to 600 ℃ at 1 ℃/min, keeping at 600 ℃ for 240min, naturally cooling, centrifugally washing, placing in an oven at 60 ℃ and drying to obtain ZnWO 4 Photocatalyst, noted ZnWO 4 -1。
Example 2
Comparative ZnWO 4 The preparation method of (2) is as follows:
uniformly stirring 2.55g of ammonium tungstate hydrate in 20mL of deionized water to obtain a solution A; 2.19g of zinc acetate dihydrate is dissolved in 10mL of deionized water, and 4.5g of tartaric acid is added and stirred until the zinc acetate dihydrate is dissolved, so as to obtain a solution B; then mixing the solution A and the solution B, uniformly stirring, placing in an oven at 80 ℃, drying and puffing the sample, grinding, placing in a muffle furnace, heating to 400 ℃ at 2 ℃/min, heating to 600 ℃ at 1 ℃/min, keeping at 600 ℃ for 240min, naturally cooling, centrifugally washing, and placing in an oven at 60 ℃ for drying to obtain a reference sample ZnWO 4 Photocatalyst, noted ZnWO 4 -2。
FIG. 1 shows ZnWO prepared in example 1 4 ZnWO prepared in example 2 4 -2 XRD pattern of the photocatalyst. As can be seen from FIG. 1, znWO 4 The diffraction peak of the-1 sample is sharp, which shows that the crystallinity of the product is good, corresponding to XRD standard card JCPDS15-0774, but ZnWO 4 The sample-2 has obvious diffraction peaks at angles of 22.5 degrees and 33.6 degrees, which correspond to the diffraction angles of tungsten oxide, and shows that the peroxy radical can inhibit the growth of the crystal phase of the tungsten oxide.
EXAMPLE 3ZnWO 4 Application of photocatalyst in catalytic decomposition of water under irradiation of visible light
1) Under normal temperature and pressure, 20mL of 1.25mol/L aqueous methanol solution was added to a vessel, 20. Mu.L of 1wt% aqueous chloroplatinic acid solution was added, and then 20mg of ZnWO prepared in example 1 was added 4 1, photocatalyst, ultrasonic treatment is carried out for 10min, and dispersion is carried out; argon is introduced into the container at the rate of 40mL/min for 30min, the container is sealed, 1000 mu L of gas in the container is taken out by a microinjector every 15min under the condition of visible light irradiation, the gas component of the sample is detected by adopting a gas chromatographic separation technology, and the hydrogen evolution concentration is measured.
2) According to step 1), except that ZnWO prepared in example 1 is used 4 -1 photocatalyst replacement with ZnWO prepared in example 2 4 And 2, taking 1000 mu L of gas in a container by using a microinjector every 15min, detecting the gas component of the sample by using a gas chromatographic separation technology, and measuring the concentration of hydrogen evolution.
FIG. 3 shows different H's detected using gas chromatographic separation techniques 2 The relationship between the volume and the gas chromatography peak area is shown as a standard curve in fig. 3, and the fitting degree is 0.9993, which shows that the two have good linear relationship, and the gas chromatography peak area and the substance concentration can be converted through the standard curve.
The peak area of the extracted gas was measured by gas chromatography, and then converted into its hydrogen evolution concentration by a hydrogen peak area standard curve, as shown in FIG. 2, after one hour, znWO 4 -1 production of H 2 The amount is 178.56 mu mol/L, znWO 4 -2 production of H 2 The amount is 43.45 mu mol/L, znWO 4 -1 is significantly better than ZnWO 4 And (2) a sample shows that the photo-generated electron transfer capability is stronger after hydrogen peroxide is added, and the electron hole pair has stronger oxidation-reduction capability.
Claims (7)
1. ZnWO (zinc-oxygen) device 4 The application of the photocatalyst in catalyzing hydrogen evolution under the irradiation of visible light is characterized by comprising the following steps: under normal temperature and pressure, 20mL of aqueous methanol solution, 20. Mu.L of aqueous chloroplatinic acid solution and then 20mg of ZnWO are added to a vessel 4 Photocatalyst, ultrasonic for 10min, dispersing liquid; argon is introduced into the container at the speed of 40mL/min for 30min, the container is sealed, 1000 mu L of gas in the container is taken out by a microinjector every 15min under the condition of visible light irradiation, the gas component is detected by a gas chromatographic separation technology method, and the hydrogen evolution concentration is measured;
the ZnWO 4 The preparation method of the photocatalyst comprises the following steps: stirring ammonium tungstate in a hydrogen peroxide solution until the ammonium tungstate is dissolved to obtain a solution A; dissolving zinc acetate dihydrate in deionized water, adding tartaric acid, and stirring until the solution is dissolved to obtain a solution B; mixing the solution A and the solution B, stirring, placing in a baking oven, drying, puffing, grinding, placing in a muffle furnace for calcining, naturally cooling, washing, centrifuging, and drying at 60deg.C to obtain ZnWO 4 A photocatalyst;
the addition amount of the ammonium tungstate and the zinc acetate dihydrate is calculated as the molar ratio of W to Zn=1:1;
the oven was set at a temperature of 80 ℃.
2. The use according to claim 1, wherein the ammonium tungstate is hydrated ammonium tungstate of formula H 40 N 10 O 41 W 12 ·xH 2 O, molecular weight 3042.58.
3. Use according to claim 2, characterized in that the ammonium tungstate hydrate, zinc acetate dihydrate and tartaric acid are added in a molar ratio W: zn: tartaric acid = 1:1:3.
4. The use according to claim 1, wherein the hydrogen peroxide solution has a concentration of 30%.
5. The use according to claim 1, characterized in that the conditions of calcination are: heating to 400 ℃ at 2 ℃/min, heating to 600 ℃ at 1 ℃/min, and maintaining at 600 ℃ for 240min.
6. Use according to claim 1, characterized in that the concentration of the aqueous methanol solution is 1.25mol/L.
7. Use according to claim 1, characterized in that the concentration of the aqueous solution of chloroplatinic acid is 1% by weight.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310043350.5A CN115957744B (en) | 2023-01-29 | 2023-01-29 | ZnWO (zinc-oxygen) device 4 Preparation method and application of photocatalyst |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202310043350.5A CN115957744B (en) | 2023-01-29 | 2023-01-29 | ZnWO (zinc-oxygen) device 4 Preparation method and application of photocatalyst |
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| CN115957744B true CN115957744B (en) | 2023-11-10 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102557141A (en) * | 2012-03-02 | 2012-07-11 | 河北联合大学 | Structure-oriented synthetic method of zinc tungstate nanometer sheet |
| CN106140141A (en) * | 2016-06-21 | 2016-11-23 | 常州工程职业技术学院 | A kind of oxygen-containing defected ZnWO4catalysis material and preparation method thereof |
| CN108585111A (en) * | 2018-05-12 | 2018-09-28 | 辽宁大学 | The method that semi-conducting material Zinc Tungstate is catalyzed ultrasonotomography Meloxicam |
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2023
- 2023-01-29 CN CN202310043350.5A patent/CN115957744B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102557141A (en) * | 2012-03-02 | 2012-07-11 | 河北联合大学 | Structure-oriented synthetic method of zinc tungstate nanometer sheet |
| CN106140141A (en) * | 2016-06-21 | 2016-11-23 | 常州工程职业技术学院 | A kind of oxygen-containing defected ZnWO4catalysis material and preparation method thereof |
| CN108585111A (en) * | 2018-05-12 | 2018-09-28 | 辽宁大学 | The method that semi-conducting material Zinc Tungstate is catalyzed ultrasonotomography Meloxicam |
Non-Patent Citations (4)
| Title |
|---|
| "Effects of tungsten source and tartrate additive on the microstructure and photoluminescence of hydrothermally crystallized ZnWO4";Mei‑Ting Li et al.;《Tungsten》;第1卷;第266-275页 * |
| "Photocatalytic Activity of Nanosized ZnWO, Prepared by the Sol-gel Method";WU Yan et al.;《CHEM. RES. CHINESE U.》;第23卷(第4期);第465-468页 * |
| "PHOTOCATALYTIC ACTIVITY OF ZnWO4 NANOPARTICLES PREPARED BY COMBUSTION SYNTHESIS";J. Grabis et al.;《Latvian Journal of Chemistry》;第93-98页 * |
| "三维多孔锌钨氧化物异质结的制备、 组分调控与光催化性能";刘美宏等;《高等学校化学学报》;第40卷(第11期);第2367-2374页 * |
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