CN112844372A - Oxygen vacancy-containing bismuth molybdate thermal catalyst and preparation method and application thereof - Google Patents
Oxygen vacancy-containing bismuth molybdate thermal catalyst and preparation method and application thereof Download PDFInfo
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- CN112844372A CN112844372A CN202110191014.6A CN202110191014A CN112844372A CN 112844372 A CN112844372 A CN 112844372A CN 202110191014 A CN202110191014 A CN 202110191014A CN 112844372 A CN112844372 A CN 112844372A
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- bismuth
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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 45
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 239000001301 oxygen Substances 0.000 title claims abstract description 33
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 33
- 239000003054 catalyst Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 230000003197 catalytic effect Effects 0.000 claims abstract description 16
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000001354 calcination Methods 0.000 claims abstract description 13
- 150000001621 bismuth Chemical class 0.000 claims abstract description 10
- 150000002751 molybdenum Chemical class 0.000 claims abstract description 10
- 239000002243 precursor Substances 0.000 claims abstract description 10
- 239000001257 hydrogen Substances 0.000 claims abstract description 9
- 229910052739 hydrogen Inorganic materials 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 group CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 29
- 230000015556 catabolic process Effects 0.000 claims description 10
- 238000006731 degradation reaction Methods 0.000 claims description 10
- 238000006243 chemical reaction Methods 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
- 239000000356 contaminant Substances 0.000 claims description 3
- 239000003344 environmental pollutant Substances 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- 231100000719 pollutant Toxicity 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
- 230000007704 transition Effects 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 2
- 229910002900 Bi2MoO6 Inorganic materials 0.000 description 20
- 239000007789 gas Substances 0.000 description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- 238000010586 diagram Methods 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000002086 nanomaterial 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
- 230000001276 controlling effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000003912 environmental pollution Methods 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
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011259 mixed solution 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
- 238000005303 weighing Methods 0.000 description 1
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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
- B01J23/16—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 an oxygen vacancy-containing bismuth molybdate thermal catalyst, and a preparation method and application thereof. The preparation method comprises the following steps: adding molybdenum salt and bismuth salt into deionized water, keeping stirring and fully dissolving the molybdenum salt and the bismuth salt; adding polyethylene glycol, and continuously 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 utilizing the molybdenum salt and the bismuth salt, and the bismuth molybdate is cheap and easily available in raw materials, low in cost and environment-friendly. And the synthesized bismuth molybdate has stable structure and higher thermal catalytic activity. According to the bismuth molybdate thermal catalytic material containing oxygen vacancies, the oxygen vacancies can form donor 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 thermal catalytic materials, and particularly relates to an oxygen vacancy-containing bismuth molybdate thermal catalyst, and a preparation method and application thereof.
Background
With the progress and economic development of society, environmental and energy problems are more urgent, and how to efficiently treat environmental pollution and search for clean energy capable of replacing fossil fuel becomes a core problem of sustainable development of twenty-first century. The catalytic technology has wide development prospect in the aspect of solar energy environmental purification at present, and the degradation of harmful organic matters and inorganic matters is generally carried out by photocatalysis, thermocatalysis, electrocatalytic degradation and the like. Among them, thermal catalysis is an effective degradation approach, and has been widely paid attention to by researchers in recent years.
Bismuth molybdate is a novel photocatalytic material, and has many physical and chemical properties such as ion conduction, 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 abundant oxygen vacancies. The oxygen vacancy can form a donor energy level under a conduction band, so that the band gap width is reduced, and the energy of electron transition is reduced. However, few thermal catalysis of bismuth molybdate has been reported, and it has been studied that bismuth molybdate has good catalytic activity in thermal catalysis, which also facilitates the application of bismuth molybdate in the degradation of gas pollutants.
Disclosure of Invention
The invention aims to provide an oxygen vacancy-containing bismuth molybdate thermal catalyst and a preparation method thereof, and the method is simple, convenient, low in cost, mild in condition and beneficial to large-scale production.
The technical scheme adopted by the invention is as follows: the preparation method of the oxygen vacancy-containing bismuth molybdate thermal catalyst comprises the following steps:
1) adding molybdenum salt and bismuth salt into deionized water, keeping stirring and fully dissolving the molybdenum salt and the bismuth salt;
2) adding polyethylene glycol, and continuously 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, in the above oxygen-vacancy-containing bismuth molybdate thermal catalyst, the molybdenum salt is ammonium molybdate or sodium molybdate.
Preferably, in the above thermal catalyst of bismuth molybdate containing oxygen vacancies, the bismuth salt is bismuth nitrate pentahydrate, bismuth chloride or bismuth acetate.
Preferably, the oxygen-vacancy-containing bismuth molybdate thermal catalyst comprises 2:1 of bismuth and molybdenum in element molar ratio.
Preferably, in the step 3), the drying temperature of the bismuth molybdate thermal catalyst containing oxygen vacancies is 100-.
Preferably, in the step 4), the calcination is carried out at the temperature of 300-700 ℃ for 2 h.
The application of the oxygen vacancy-containing bismuth molybdate thermal catalyst in thermal catalytic degradation of gas pollutants is provided.
Preferably, for the above-mentioned application, the gaseous contaminant is isopropanol.
Preferably, the above application, 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 invention has the beneficial effects that:
1. the bismuth molybdate containing oxygen vacancies is prepared by utilizing the molybdenum salt and the bismuth salt, and the bismuth molybdate is cheap and easily available in raw materials, low in cost and environment-friendly. And the synthesized bismuth molybdate has stable structure and good thermal catalytic activity.
2. According to the bismuth molybdate thermal catalytic material containing oxygen vacancies, the oxygen vacancies can form donor 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 Bi2MoO6And vacancy Bi obtained by calcination under hydrogen gas in the invention2MoO6XRD contrast pattern of (a).
FIG. 2 shows pure Bi2MoO6And vacancy Bi obtained by calcination under hydrogen gas in the invention2MoO6FI-IT comparison graph of (a).
FIG. 3 shows pure Bi2MoO6And vacancy B obtained by calcination under hydrogen in accordance with the inventioni2MoO6UV-vis comparison of (A).
FIG. 4a shows pure Bi2MoO6The theoretical calculation of (2) band diagram.
FIG. 4b shows vacancy Bi obtained by calcination under hydrogen gas in accordance with the present invention2MoO6The theoretical calculation of (2) band diagram.
FIG. 5 shows pure Bi2MoO6And vacancy Bi obtained by calcination under hydrogen gas in the invention2MoO6The isopropanol conversion of (a) is compared to (b).
Detailed Description
Example 1
(mono) bismuth molybdate thermocatalytic material containing oxygen vacancies
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) drying the sol obtained in the step 2) in a blast drying oven at 120 ℃ for 15-20h to obtain a precursor.
4) Fully grinding the precursor obtained in the step 3), placing the precursor into a tube furnace, roasting the precursor for 2 hours at 500 ℃ in the air (flow rate of 10ml/min) atmosphere or hydrogen (flow rate of 10ml/min) atmosphere respectively, controlling the temperature rise rate of the tube furnace at 3 ℃/min, and obtaining Bi obtained in the air atmosphere respectively2MoO6Marked as pure Bi2MoO6And oxygen vacancy-containing bismuth molybdate obtained in a hydrogen atmosphere, labeled as vacancy Bi2MoO6。
(II) detection
FIG. 1 shows Bi2MoO6Standard card and pure Bi2MoO6And vacancy Bi2MoO6The XRD contrast diagram of the bismuth molybdate nano material is shown in figure 1, and the sample is in accordance with the standard card, thereby proving that the bismuth molybdate nano material is successfully synthesized.
FIG. 2 shows pure Bi2MoO6And vacancy Bi2MoO6FT-IT comparison chart of (950) --1With extensions of Mo-O bondsReduced mode, 600-400cm-1With a Bi-O stretching and vibration mode of 1620 and 1358cm-1The peak of (a) is a vibration mode of O-H, and the peak is greatly changed compared with the pure bismuth molybdate, which is consistent with high activity in a corresponding hydrogen atmosphere.
FIG. 3 shows pure Bi2MoO6And vacancy Bi2MoO6Compared to pure bismuth molybdate, the calcination of the sample under hydrogen gas shows a shift to the right and a tailing peak after 700nm, indicating that there are oxygen defects in the material and the highest thermal catalytic activity of the sample under hydrogen calcination.
FIG. 4a shows pure Bi2MoO6And FIG. 4b shows vacancy Bi obtained by calcination under hydrogen in accordance with the present invention2MoO6The band diagram is theoretically calculated. When one of the oxygen points of bismuth molybdate is scratched, a new peak value is formed on the left side of 0(eV), which is shown as a new impurity energy level formed between the donor energy level and the acceptor energy level, which is beneficial to the carrier transportation and conduction consistent with the catalytic activity of FIG. 5 and the ultraviolet data result.
Example 2 use of oxygen vacancy containing bismuth molybdate thermocatalytic materials for the degradation of isopropanol
Separately, pure Bi prepared in example 12MoO6And vacancy Bi2MoO6Placed on top of the glass reactor, connected to the instrument and checked for device hermeticity. Heating isopropanol to 30 deg.C, volatilizing part of isopropanol liquid into gas, regulating gas flowmeter, starting gas compressor, allowing isopropanol gas to flow into glass reactor, simultaneously opening resistor, and heating catalyst to decompose isopropanol into acetone gas. Heating to 120-180 ℃, after 20min, extracting 10mL of gas to detect the content of acetone, and comparing the content of isopropanol in the gas inlet and the content of isopropanol in the gas outlet. The acetone produced was subjected to gas chromatography using a FID detector (GC1690, Jiedo technologies, Ltd.).
FIG. 5 shows pure Bi2MoO6And vacancy Bi2MoO6Comparative graph of isopropanol gas conversion ratio, Bi2MoO6And vacancy Bi2MoO6The conversion rate of the isopropyl alcohol is as followsIt is known that vacancy-containing bismuth molybdate is more catalytically active and more efficient in contaminant degradation at the same time. Oxygen vacancies, one of the most common and important crystal defects, have a significant impact on semiconductor thermal catalytic performance. Bismuth molybdate is a typical n-type semiconductor whose oxygen vacancies localize one or two electrons at its site, and the localized electrons have a direct effect on the electronic structure of bismuth molybdate, i.e., a donor level is generated below the conduction band of bismuth molybdate. These donor levels increase with increasing oxygen vacancies, which sometimes overlap the conduction band if the oxygen vacancy concentration is high enough, and the introduction of oxygen vacancies reduces the band width and energy of the electron transition.
Claims (9)
1. The preparation method of the oxygen-vacancy-containing bismuth molybdate thermal catalyst is characterized by comprising the following steps of:
1) adding molybdenum salt and bismuth salt into deionized water, keeping stirring and fully dissolving the molybdenum salt and the bismuth salt;
2) adding polyethylene glycol, and continuously 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. The oxygen vacancy-containing bismuth molybdate thermal catalyst as claimed in claim 1, wherein the molybdenum salt is ammonium molybdate or sodium molybdate.
3. The oxygen-vacancy-containing bismuth molybdate thermal catalyst as claimed in claim 1, wherein the bismuth salt is bismuth nitrate pentahydrate, bismuth chloride or bismuth acetate.
4. The oxygen vacancy-containing bismuth molybdate thermal catalyst as claimed in claim 1, wherein the molar ratio of bismuth to molybdenum is 2: 1.
5. The oxygen vacancy-containing bismuth molybdate thermal catalyst as claimed in claim 1, wherein in the step 3), the drying temperature is 100-120 ℃.
6. The oxygen-vacancy-containing bismuth molybdate thermal catalyst as claimed in claim 1, wherein in the step 4), the calcination is carried out at the temperature of 300-700 ℃ for 2 h.
7. Use of the oxygen vacancy-containing bismuth molybdate thermal catalyst of any one of claims 1 to 6 for the thermocatalytic degradation of gaseous pollutants.
8. Use according to claim 7, wherein the gaseous contaminant is isopropanol.
9. Use according to claim 8, characterized in that the method is as follows: adding the oxygen vacancy-containing bismuth molybdate thermal catalyst as claimed in any one of claims 1 to 6 into a reaction vessel, adding isopropanol, and performing thermal catalytic degradation at 100 ℃ to 180 ℃.
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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 |
| CN114892272A (en) * | 2022-05-05 | 2022-08-12 | 山东大学 | Preparation method of oxygen-rich vacancy bismuth molybdate single crystal nanorod |
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| CN114892272A (en) * | 2022-05-05 | 2022-08-12 | 山东大学 | Preparation method of oxygen-rich vacancy bismuth molybdate single crystal nanorod |
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