CN112844372B - Bismuth molybdate thermal catalyst containing oxygen vacancy and preparation method and application thereof - Google Patents
Bismuth molybdate thermal catalyst containing oxygen vacancy and preparation method and application thereof Download PDFInfo
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- CN112844372B CN112844372B CN202110191014.6A CN202110191014A CN112844372B CN 112844372 B CN112844372 B CN 112844372B CN 202110191014 A CN202110191014 A CN 202110191014A CN 112844372 B CN112844372 B CN 112844372B
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- bismuth
- containing oxygen
- oxygen vacancies
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- DKUYEPUUXLQPPX-UHFFFAOYSA-N dibismuth;molybdenum;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Mo].[Mo].[Bi+3].[Bi+3] DKUYEPUUXLQPPX-UHFFFAOYSA-N 0.000 title claims abstract description 39
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 239000001301 oxygen Substances 0.000 title claims abstract description 34
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 34
- 239000003054 catalyst Substances 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000001257 hydrogen Substances 0.000 claims abstract description 13
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 13
- 238000001354 calcination Methods 0.000 claims abstract description 12
- 230000003197 catalytic effect Effects 0.000 claims abstract description 11
- 150000001621 bismuth Chemical class 0.000 claims abstract description 10
- 239000002243 precursor Substances 0.000 claims abstract description 10
- 150000002751 molybdenum Chemical class 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 5
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 4
- 238000000227 grinding Methods 0.000 claims abstract description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 29
- 239000007789 gas Substances 0.000 claims description 11
- 230000015556 catabolic process Effects 0.000 claims description 8
- 238000006731 degradation reaction Methods 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 239000003344 environmental pollutant Substances 0.000 claims description 5
- 231100000719 pollutant Toxicity 0.000 claims description 5
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical group [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 4
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 4
- 239000011609 ammonium molybdate Substances 0.000 claims description 4
- 229940010552 ammonium molybdate Drugs 0.000 claims description 4
- FBXVOTBTGXARNA-UHFFFAOYSA-N bismuth;trinitrate;pentahydrate Chemical group O.O.O.O.O.[Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FBXVOTBTGXARNA-UHFFFAOYSA-N 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 3
- QYIGOGBGVKONDY-UHFFFAOYSA-N 1-(2-bromo-5-chlorophenyl)-3-methylpyrazole Chemical compound N1=C(C)C=CN1C1=CC(Cl)=CC=C1Br QYIGOGBGVKONDY-UHFFFAOYSA-N 0.000 claims description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 2
- 229910052797 bismuth Inorganic materials 0.000 claims description 2
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 2
- JHXKRIRFYBPWGE-UHFFFAOYSA-K bismuth chloride Chemical compound Cl[Bi](Cl)Cl JHXKRIRFYBPWGE-UHFFFAOYSA-K 0.000 claims description 2
- 229910052750 molybdenum Inorganic materials 0.000 claims description 2
- 239000011733 molybdenum Substances 0.000 claims description 2
- 235000015393 sodium molybdate Nutrition 0.000 claims description 2
- 239000011684 sodium molybdate Substances 0.000 claims description 2
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 230000007704 transition Effects 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 229910017299 Mo—O Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 230000006652 catabolic pathway Effects 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/31—Chromium, molybdenum or tungsten combined with bismuth
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8668—Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/84—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by UV- or VIS- data
Abstract
The invention relates to a bismuth molybdate thermal catalyst containing oxygen vacancies, and a preparation method and application thereof. The preparation method comprises the following steps: adding molybdenum salt and bismuth salt into deionized water, and stirring to fully dissolve the molybdenum salt and the bismuth salt; adding polyethylene glycol, and continuing stirring to obtain sol; drying the sol in a drying oven to obtain a precursor; grinding the obtained precursor, and calcining in a hydrogen environment to obtain the target product. The bismuth molybdate containing oxygen vacancies is prepared by using the molybdenum salt and the bismuth salt, and the bismuth molybdate containing oxygen vacancies has the advantages of low-cost and easily obtained raw materials, low cost and environmental friendliness. And the synthesized bismuth molybdate has stable structure and higher thermocatalytic activity. The bismuth molybdate thermocatalytic material containing oxygen vacancies provided by the invention has the advantages that the oxygen vacancies can form donor energy levels under a conduction band, so that the band gap width is reduced, the energy of electron transition is reduced, and good catalytic activity is shown.
Description
Technical Field
The invention belongs to the technical field of thermocatalytic materials, and particularly relates to a bismuth molybdate thermocatalyst containing oxygen vacancies, and a preparation method and application thereof.
Background
With the advancement of society and the development of economy, environmental and energy problems are becoming more urgent, and how to efficiently treat environmental pollution and find clean energy which can replace fossil fuel is a core problem of sustainable development in the twenty-first century. Catalytic technology has wide development prospect in the aspect of solar energy environmental purification at present, and degradation of harmful organic matters and inorganic matters is generally carried out through photocatalysis, thermocatalysis, electrocatalytic degradation and the like. Among them, thermocatalysis is an effective degradation pathway, and has received extensive attention from researchers in recent years.
Bismuth molybdate is a novel photocatalytic material and has many physical and chemical properties such as ion conductivity, dielectric property, gas sensing and catalytic activity. The material has the advantages of high purity, good uniformity and the like, and the synthesized bismuth molybdate has larger specific surface area and rich oxygen vacancies. Oxygen vacancies can form donor levels below the conduction band, thereby reducing the band gap width and reducing the energy of the electron transition. However, few reports on the thermal catalysis of bismuth molybdate have been made, and by research, bismuth molybdate has good catalytic activity in thermal catalysis, which also promotes the application of bismuth molybdate in degrading gaseous pollutants.
Disclosure of Invention
The invention aims to provide the bismuth molybdate thermal catalyst containing oxygen vacancies and the preparation method thereof, and the method is simple, convenient, low in cost, mild in condition and beneficial to mass production.
The invention adopts the technical scheme that: the preparation method of the bismuth molybdate thermal catalyst containing oxygen vacancies comprises the following steps:
1) Adding molybdenum salt and bismuth salt into deionized water, and stirring to fully dissolve the molybdenum salt and the bismuth salt;
2) Adding polyethylene glycol, and continuing stirring to obtain sol;
3) Drying the sol obtained in the step 2) in an oven to obtain a precursor;
4) Grinding the precursor obtained in the step 3), and calcining in a hydrogen environment to obtain a target product.
Preferably, the bismuth molybdate thermal catalyst containing oxygen vacancies is one of ammonium molybdate or sodium molybdate.
Preferably, the bismuth salt is bismuth nitrate pentahydrate, bismuth chloride or bismuth acetate.
Preferably, the bismuth molybdate thermal catalyst containing oxygen vacancies comprises bismuth and molybdenum=2:1 according to the element mole ratio.
Preferably, in the bismuth molybdate thermal catalyst containing oxygen vacancies in the step 3), the drying temperature is 100-120 ℃.
Preferably, in the bismuth molybdate thermal catalyst containing oxygen vacancies in the step 4), the calcination is performed at a temperature of 300-700 ℃ for 2 hours.
The application of the bismuth molybdate thermal catalyst containing oxygen vacancies in thermal catalytic degradation of gas pollutants.
Preferably, for the above application, the gaseous contaminant is isopropanol.
Preferably, the above application, the method is as follows: adding bismuth molybdate thermal catalyst containing oxygen vacancy into a reaction vessel, adding isopropanol, and performing thermal catalytic degradation at 100-180 ℃.
The beneficial effects of the invention are as follows:
1. the bismuth molybdate containing oxygen vacancies is prepared by using the molybdenum salt and the bismuth salt, and the bismuth molybdate containing oxygen vacancies has the advantages of low-cost and easily obtained raw materials, low cost and environmental friendliness. And the synthesized bismuth molybdate has stable structure and good thermocatalytic activity.
2. The bismuth molybdate thermocatalytic material containing oxygen vacancies provided by the invention has the advantages that the oxygen vacancies can form donor energy levels under a conduction band, so that the band gap width is reduced, the energy of electron transition is reduced, and good catalytic activity is shown.
Drawings
FIG. 1 shows pure Bi 2 MoO 6 And the vacancy Bi obtained by calcining under hydrogen of the present invention 2 MoO 6 XRD contrast pattern of (c).
FIG. 2 shows pure Bi 2 MoO 6 And the vacancy Bi obtained by calcining under hydrogen of the present invention 2 MoO 6 FI-IT comparison graph of (c).
FIG. 3 shows pure Bi 2 MoO 6 And the vacancy Bi obtained by calcining under hydrogen of the present invention 2 MoO 6 UV-vis contrast plot of (c).
FIG. 4a is pure Bi 2 MoO 6 Is a theoretical calculated energy band diagram of (2).
FIG. 4b shows the vacancies Bi obtained by calcination under hydrogen in accordance with the present invention 2 MoO 6 Is a theoretical calculated energy band diagram of (2).
FIG. 5 shows pure Bi 2 MoO 6 And the vacancy Bi obtained by calcining under hydrogen of the present invention 2 MoO 6 Isopropanol conversion ratio of (c) is compared with a graph of isopropanol conversion ratio.
Detailed Description
Example 1
Bismuth molybdate thermocatalytic material containing oxygen vacancy
1) 4.85g of bismuth nitrate pentahydrate and 0.88g of ammonium molybdate are respectively dissolved in 50ml of deionized water, stirred for 0.5h, and the aqueous solution of bismuth nitrate pentahydrate and the aqueous solution of ammonium molybdate are uniformly mixed.
2) Weighing 2g of polyethylene glycol, dissolving in 10mL of deionized water, injecting into the mixed solution obtained in the step 1), and uniformly stirring to obtain sol.
3) And (3) placing the sol obtained in the step (2) into a blast drying oven at 120 ℃ for drying for 15-20h to obtain a precursor.
4) Fully grinding the precursor obtained in the step 3), placing the ground precursor into a tube furnace, respectively roasting the ground precursor for 2 hours at 500 ℃ under the air (flow rate of 10 ml/min) or hydrogen (flow rate of 10 ml/min) atmosphere, and controlling the heating rate of the tube furnace to be 3 ℃/min to obtain Bi under the air atmosphere respectively 2 MoO 6 Marked as pure Bi 2 MoO 6 And bismuth molybdate containing oxygen vacancies obtained under a hydrogen atmosphere, labeled as vacancies Bi 2 MoO 6 。
(II) detection
FIG. 1 is Bi 2 MoO 6 Standard card and pure Bi 2 MoO 6 And vacancy Bi 2 MoO 6 As can be seen from fig. 1, the sample is in line with the standard card, demonstrating successful synthesis of bismuth molybdate nanomaterial.
FIG. 2 shows pure Bi 2 MoO 6 And vacancy Bi 2 MoO 6 FT-IT comparison chart of 950-700cm -1 The band is in a flexible mode of Mo-O bond, 600-400cm -1 The bands of (2) are Bi-O expansion and vibration modes 1620 and 1358cm -1 The peak of (2) is the vibration mode of O-H, and the peak is greatly changed compared with pure bismuth molybdate, which is consistent with high activity under the corresponding hydrogen atmosphere.
FIG. 3 shows pure Bi 2 MoO 6 And vacancy Bi 2 MoO 6 The calcined sample under hydrogen showed a shift to the right and a tailing peak after 700nm compared to pure bismuth molybdate, indicating that oxygen defects were present in the material and that the sample had the highest thermocatalytic activity under hydrogen calcination.
FIG. 4a is pure Bi 2 MoO 6 Sum picture4b is the vacancy Bi obtained by calcining under hydrogen gas 2 MoO 6 Theoretical calculation energy band diagram. When bismuth molybdate is oxygen-scratched, a new peak is formed at the left side of 0 (eV), which is expressed as a new impurity energy level formed between a donor energy level and an acceptor energy level, and the transport and conduction of carriers are favorable to be consistent with the catalytic activity of FIG. 5 and the ultraviolet data result.
Example 2 use of bismuth molybdate thermocatalytic Material containing oxygen vacancies in the degradation of isopropanol
The pure Bi prepared in example 1 was separated 2 MoO 6 And vacancy Bi 2 MoO 6 Placed on top of the glass reactor, connected to the instrument and tested for tightness. Heating the isopropanol to 30 ℃, part of the isopropanol liquid can volatilize into gas, regulating a gas flowmeter, turning on a gas compressor, enabling the isopropanol gas to flow into the glass reactor, simultaneously turning on a resistor, and heating a catalyst to decompose the isopropanol into acetone gas. Heating to 120-180 ℃, extracting 10mL of gas after 20min to detect the acetone content, and comparing the isopropanol content of the air inlet and the air outlet. The acetone produced was subjected to gas chromatography using a FID detector (GC 1690, shortcut technologies).
FIG. 5 shows pure Bi 2 MoO 6 And vacancy Bi 2 MoO 6 Comparison chart of isopropyl alcohol gas conversion rate, bi 2 MoO 6 And vacancy Bi 2 MoO 6 The isopropanol conversion rate of the catalyst shows that the bismuth molybdate containing vacancies has higher catalytic activity, and the pollutant degradation is more efficient in the same time. Oxygen vacancies, one of the most common and important crystal defects, have an important impact on semiconductor thermocatalytic properties. Bismuth molybdate is a typical n-type semiconductor whose oxygen vacancies localize one or both electrons at their locations, the localized electrons having a direct effect on the bismuth molybdate's electronic structure, i.e., creating donor levels below the bismuth molybdate conduction band. These donor levels increase with increasing oxygen vacancies, which sometimes overlap the conduction band if the oxygen vacancy concentration is high enough, the introduction of oxygen vacancies reduces the band width and energy of the electron transition.
Claims (6)
1. The application of the bismuth molybdate thermal catalyst containing oxygen vacancies in thermal catalytic degradation of gas pollutants is characterized in that the gas pollutants are isopropanol, and the method is as follows: adding a bismuth molybdate thermal catalyst containing oxygen vacancies into a reaction vessel, adding isopropanol, and performing thermal catalytic degradation at 100-180 ℃; the preparation method of the bismuth molybdate thermal catalyst containing oxygen vacancies comprises the following steps:
1) Adding molybdenum salt and bismuth salt into deionized water, and stirring to fully dissolve the molybdenum salt and the bismuth salt;
2) Adding polyethylene glycol, and continuing stirring to obtain sol;
3) Drying the sol obtained in the step 2) in an oven to obtain a precursor;
4) Grinding the precursor obtained in the step 3), and calcining in a hydrogen environment to obtain a target product.
2. Use according to claim 1, characterized in that the molybdenum salt is ammonium molybdate or sodium molybdate.
3. The use according to claim 1, wherein the bismuth salt is bismuth nitrate pentahydrate, bismuth chloride or bismuth acetate.
4. Use according to claim 1, characterized in that bismuth: molybdenum=2:1 in terms of element molar ratio.
5. The use according to claim 1, wherein in step 3) the drying is carried out at a temperature of 100-120 ℃.
6. The use according to claim 1, wherein in step 4) the calcination is carried out at a temperature of 300-700 ℃ for a time of 2 hours.
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| CN114471536A (en) * | 2022-02-17 | 2022-05-13 | 辽宁大学 | MnCr with adjustable oxygen vacancy concentration2O4Photocatalyst and preparation method and application thereof |
| CN114892272B (en) * | 2022-05-05 | 2024-03-29 | 山东大学 | Preparation method of oxygen-enriched vacancy bismuth molybdate monocrystal nanorod |
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| WO2013117017A1 (en) * | 2012-02-10 | 2013-08-15 | 武汉理工大学 | Preparation method for ceo2-mno2 composite catalyst with efficient photothermal concerted catalytic purification function for vocs |
| CN109012654A (en) * | 2018-08-22 | 2018-12-18 | 延安大学 | A kind of bismuth molybdate catalysis material and preparation method thereof rich in surface oxygen defect |
| CN110302824A (en) * | 2019-08-06 | 2019-10-08 | 辽宁大学 | Molybdenum doping graphite phase carbon nitride catalyst and its preparation method and application |
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| CN111217398A (en) * | 2020-01-21 | 2020-06-02 | 辽宁大学 | Zinc ferrite thermal catalyst containing oxygen vacancies and preparation method and application thereof |
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