CN110550658A - preparation method of bismuth titanate visible-light-driven photocatalyst and application of bismuth titanate visible-light-driven photocatalyst - Google Patents
preparation method of bismuth titanate visible-light-driven photocatalyst and application of bismuth titanate visible-light-driven photocatalyst Download PDFInfo
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 32
- 229910002115 bismuth titanate Inorganic materials 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 claims abstract description 93
- HUMNYLRZRPPJDN-UHFFFAOYSA-N benzaldehyde Chemical compound O=CC1=CC=CC=C1 HUMNYLRZRPPJDN-UHFFFAOYSA-N 0.000 claims abstract description 38
- 235000019445 benzyl alcohol Nutrition 0.000 claims abstract description 31
- 239000002243 precursor Substances 0.000 claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- QNGNSVIICDLXHT-UHFFFAOYSA-N para-ethylbenzaldehyde Natural products CCC1=CC=C(C=O)C=C1 QNGNSVIICDLXHT-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000000243 solution Substances 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 10
- FBXVOTBTGXARNA-UHFFFAOYSA-N bismuth;trinitrate;pentahydrate Chemical compound 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 abstract description 9
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims abstract description 9
- 230000001590 oxidative effect Effects 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000001354 calcination Methods 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 239000011259 mixed solution Substances 0.000 claims abstract description 6
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 239000003054 catalyst Substances 0.000 claims description 5
- 239000000463 material Substances 0.000 abstract description 7
- 230000001699 photocatalysis Effects 0.000 abstract description 6
- 239000004065 semiconductor Substances 0.000 abstract description 4
- 229910002118 Bi2Ti2O7 Inorganic materials 0.000 abstract 1
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 238000007254 oxidation reaction Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 229910010413 TiO 2 Inorganic materials 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- ZCDOYSPFYFSLEW-UHFFFAOYSA-N chromate(2-) Chemical compound [O-][Cr]([O-])(=O)=O ZCDOYSPFYFSLEW-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- LBSANEJBGMCTBH-UHFFFAOYSA-N manganate Chemical compound [O-][Mn]([O-])(=O)=O LBSANEJBGMCTBH-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000004729 solvothermal method Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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
- B01J23/18—Arsenic, antimony or bismuth
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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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/04—Mixing
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G29/00—Compounds of bismuth
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/27—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation
- C07C45/29—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation of hydroxy groups
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- 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
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- 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
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Abstract
the invention relates to the technical field of semiconductor photocatalytic materials. Aims to provide a bismuth titanate visible-light-induced photocatalyst with simple process and low cost, and the bismuth titanate visible-light-induced photocatalyst is applied to the reaction of efficiently oxidizing benzyl alcohol into benzaldehyde. The technical scheme is as follows: a preparation method of a bismuth titanate visible-light-driven photocatalyst comprises the following steps: 1) dissolving bismuth nitrate pentahydrate in benzyl alcohol to form a solution, and then dropwise adding tetrabutyl titanate into the solution and stirring for 0.5-3h to obtain a mixed solution; 2) transferring the mixed solution into a reaction kettle with a polytetrafluoroethylene lining, and heating and reacting at the temperature of 100-160 ℃ for 20-24h to obtain a product precursor; then washing the precursor of the product with absolute ethyl alcohol for several times, and drying overnight at 80 ℃ to obtain the precursor; 3) calcining the obtained precursor at the temperature of 500-700 ℃ for 5-20h to obtain the Bi2Ti2O7 visible-light-driven photocatalyst.
Description
Technical Field
The invention relates to the technical field of semiconductor photocatalytic materials, in particular to a preparation method of a bismuth titanate (Bi 2 Ti 2 O 7) photocatalyst and application of the bismuth titanate visible photocatalyst in a reaction of oxidizing benzyl alcohol into benzyl alcohol.
background
the method is characterized in that the method comprises the following steps of preparing a photocatalyst, and carrying out photocatalytic reaction on the photocatalyst, wherein the photocatalyst is prepared from TiO 2 photocatalyst, the photocatalyst is prepared from a plurality of materials, and the materials are mixed to form a mixture, and the mixture is subjected to a reaction treatment, wherein the reaction treatment is carried out by using the photocatalyst.
The reaction in the traditional benzyl alcohol oxidation process is carried out under the conditions of high temperature, high pressure and a large amount of solvents, and a large amount of manganate and chromate are used as catalysts, so that a large amount of energy consumption and environmental pollution are caused to modern industry, and therefore, the photocatalytic semiconductor material is developed, and has good application prospect in the reaction of selective oxidation of benzyl alcohol into benzaldehyde.
Although TiO 2 has stable property, low price and a plurality of unique properties, the TiO 2 has good effect only under ultraviolet radiation, and because a large amount of Bi-containing compounds have good performance of oxidizing benzyl alcohol into benzaldehyde through photocatalysis, and simultaneously have special layered structures, the separation and conduction of photon-generated carriers are facilitated, the semiconductor photocatalyst Bi 2 Ti 2 O 7 containing Bi and Ti is sought to be prepared, has proper forbidden bandwidth and has catalytic activity under visible light, but at present, Bi 2 Ti 2 O 7 with high purity is difficult to prepare, and the preparation method is complex.
Disclosure of Invention
The invention aims to provide a bismuth titanate visible-light-induced photocatalyst which is simple in process and low in cost, and is applied to the reaction of efficiently oxidizing benzyl alcohol into benzaldehyde.
In order to achieve the above purpose, the following scheme is adopted:
A preparation method of a bismuth titanate visible-light-driven photocatalyst comprises the following steps:
1) Dissolving bismuth nitrate pentahydrate in benzyl alcohol to form a solution, and then dropwise adding tetrabutyl titanate into the solution and stirring for 0.5-3h to obtain a mixed solution;
2) Transferring the mixed solution into a reaction kettle with a polytetrafluoroethylene lining, and heating and reacting at the temperature of 100-160 ℃ for 20-24h to obtain a product precursor; then washing the precursor of the product with absolute ethyl alcohol for several times, and drying overnight at 80 ℃ to obtain the precursor;
3) Calcining the obtained precursor at 500-700 ℃ for 5-20h to obtain the Bi 2 Ti 2 O 7 visible-light-driven photocatalyst.
The molar ratio of the bismuth nitrate pentahydrate to the tetrabutyl titanate to the benzyl alcohol is 0.1-0.3: 1: 38.
The bismuth titanate visible-light-driven photocatalyst is applied to the reaction of oxidizing benzyl alcohol into benzaldehyde.
The invention has the beneficial effects that: the method provided by the invention is prepared by mixing the three raw materials, reacting, drying and calcining, and has simple process and low cost; the XRD (X-ray powder diffractometer) tests show that all diffraction peaks of the material appear, the peak intensity is strong, meanwhile, no impurity peak appears, and the material is very consistent with a standard card 32-0118, which shows that the crystal phase is good. In a specific application experiment of oxidizing benzyl alcohol into benzaldehyde by photocatalysis, the selectivity of the benzaldehyde is over 92 percent, and the conversion rate of the benzyl alcohol is over 92 percent.
drawings
fig. 1 is an XRD spectrum of bismuth titanate (Bi 2 Ti 2 O 7) prepared in example 1 of the present invention.
FIG. 2 shows the activity of bismuth titanate (Bi 2 Ti 2 O 7) prepared in example 1 of the present invention in catalyzing the reaction of benzyl alcohol to benzaldehyde with visible light.
The specific implementation mode is as follows:
The preparation method of the Bi 2 Ti 2 O 7 visible-light-driven photocatalyst provided by the invention is completed by combining a solvothermal method and a high-temperature calcination method by taking bismuth nitrate pentahydrate and tetrabutyl titanate as raw materials and benzyl alcohol as a solvent.
The invention is further illustrated by the following examples.
Example 1:
Dissolving 0.02mol of bismuth nitrate pentahydrate in 7.60mol of benzyl alcohol to form a solution, then dropwise adding 0.200mol of tetrabutyl titanate into the solution, fully stirring for 3h, transferring the solution into a reaction kettle with a polytetrafluoroethylene lining, heating and reacting for 24h at 120 ℃, finally obtaining a product precursor, washing the product precursor for several times by using absolute ethyl alcohol, and drying the product at 80 ℃ overnight to obtain the precursor.
A certain amount of precursor is weighed and calcined in a muffle furnace at 500 ℃ for 10 hours to obtain the bismuth titanate (Bi 2 Ti 2 O 7) photocatalyst, the XRD (X-ray diffraction) pattern of the bismuth titanate photocatalyst is shown in figure 1, diffraction characteristic peaks of Bi 2 Ti 2 O 7 exist, and the bismuth titanate photocatalyst is matched with JCPDS Card No.32-0118, and the Bi 2 Ti 2 O 7 with a good crystalline phase is obtained.
the Bi 2 Ti 2 O 7 obtained in this example was subjected to a reaction experiment of catalytic oxidation of benzyl alcohol to benzaldehyde for 8 hours under visible light, and the result is shown in FIG. 2 (the diagonal line in FIG. 2 indicates the selectivity ratio of benzaldehyde, and the cross line indicates the conversion rate of benzyl alcohol; the same is true below). The selectivity of benzaldehyde is 99%, and the conversion rate of benzyl alcohol is 95%, which indicates that the catalyst has very high activity of photocatalytic oxidation of benzyl alcohol to benzaldehyde.
Example 2:
Dissolving 0.02mol of bismuth nitrate pentahydrate in 3.80mol of benzyl alcohol to form a solution, then dripping 0.100mol of tetrabutyl titanate into the solution, fully stirring for 0.5h, transferring the solution into a reaction kettle with a polytetrafluoroethylene lining, heating and reacting for 20h at 140 ℃, finally obtaining a product precursor, washing the product precursor for several times by using absolute ethyl alcohol, and drying the product at 80 ℃ overnight to obtain the precursor.
Weighing a certain amount of precursor, and calcining the precursor in a muffle furnace at 600 ℃ for 5 hours to obtain the bismuth titanate (Bi 2 Ti 2 O 7) photocatalyst, wherein the XRD pattern of the bismuth titanate photocatalyst is also the same as that in figure 1.
The Bi 2 Ti 2 O 7 obtained in the example is subjected to a reaction experiment of catalyzing and oxidizing benzyl alcohol into benzaldehyde for 8 hours under visible light, and as can be seen from figure 2, the selectivity of the benzaldehyde is 97%, and the conversion rate of the benzyl alcohol also reaches 92%, so that the catalyst has very high activity of catalyzing the oxidization of the benzyl alcohol into the benzaldehyde.
Example 3:
dissolving 0.02mol of bismuth nitrate pentahydrate in 2.53mol of benzyl alcohol to form a solution, then dropwise adding 0.067mol of tetrabutyl titanate into the solution, fully stirring for 2h, transferring the solution into a reaction kettle with a polytetrafluoroethylene lining, heating and reacting for 15h at 160 ℃, finally obtaining a product precursor, washing the product precursor for several times by using absolute ethyl alcohol, and drying the product at 80 ℃ overnight to obtain the precursor.
Weighing a certain amount of precursor, and calcining the precursor in a muffle furnace at 500 ℃ for 10 hours to obtain the bismuth titanate (Bi 2 Ti 2 O 7) photocatalyst, wherein the XRD pattern of the bismuth titanate photocatalyst is also the same as that in figure 1.
The Bi 2 Ti 2 O 7 obtained in the example is subjected to a reaction experiment of catalyzing and oxidizing benzyl alcohol into benzaldehyde for 8 hours under visible light, and as can be seen from figure 2, the selectivity of the benzaldehyde is 92%, and the conversion rate of the benzyl alcohol is 96%, so that the catalyst has very high activity of catalyzing the oxidization of the benzyl alcohol into the benzaldehyde.
The above embodiments are only intended to illustrate the technical solution of the present invention and not to limit the scope of the present invention, and it should be understood by those skilled in the art that modifications or equivalent substitutions may be made to the technical solution of the present invention without departing from the spirit and scope of the technical solution of the present invention.
Claims (3)
1. a preparation method of a bismuth titanate visible-light-driven photocatalyst comprises the following steps:
1) Dissolving bismuth nitrate pentahydrate in benzyl alcohol to form a solution, and then dropwise adding tetrabutyl titanate into the solution and stirring for 0.5-3h to obtain a mixed solution;
2) Transferring the mixed solution into a reaction kettle with a polytetrafluoroethylene lining, and heating and reacting at the temperature of 100-160 ℃ for 20-24h to obtain a product precursor; then washing the precursor of the product with absolute ethyl alcohol for several times, and drying overnight at 80 ℃ to obtain the precursor;
3) Calcining the obtained precursor at 500-700 ℃ for 5-20h to obtain the Bi 2 Ti 2 O 7 visible-light-driven photocatalyst.
2. The method for preparing a bismuth titanate visible-light-induced photocatalyst according to claim 1, characterized in that: the molar ratio of the bismuth nitrate pentahydrate to the tetrabutyl titanate to the benzyl alcohol is 0.1-0.3: 1: 38.
3. the method of preparing a bismuth titanate visible light catalyst according to claim 1, which is applied to a reaction of oxidizing benzyl alcohol to benzaldehyde.
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| CN201910846632.2A CN110550658B (en) | 2019-09-09 | 2019-09-09 | Preparation method of bismuth titanate visible-light-driven photocatalyst and application of bismuth titanate visible-light-driven photocatalyst |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113145099A (en) * | 2021-04-27 | 2021-07-23 | 陕西科技大学 | Bismuth-loaded bismuth titanate/calcium titanate composite photocatalyst, and preparation method and application thereof |
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| CN102351242A (en) * | 2011-08-17 | 2012-02-15 | 南京师范大学 | Solvent-thermal method for preparing single-phase bismuth titanate Bi2Ti2O7 |
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| CN105036183A (en) * | 2015-07-07 | 2015-11-11 | 陕西科技大学 | Preparation method for nanometer Bi2Ti2O7 powder |
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| CN102351242A (en) * | 2011-08-17 | 2012-02-15 | 南京师范大学 | Solvent-thermal method for preparing single-phase bismuth titanate Bi2Ti2O7 |
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| CN104069848A (en) * | 2014-07-06 | 2014-10-01 | 南京师范大学 | Method for preparing pure phase bismuth titanate and titanium oxide composite material by using alcohol heat method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113145099A (en) * | 2021-04-27 | 2021-07-23 | 陕西科技大学 | Bismuth-loaded bismuth titanate/calcium titanate composite photocatalyst, and preparation method and application thereof |
| CN113145099B (en) * | 2021-04-27 | 2023-01-31 | 陕西科技大学 | Bismuth-loaded bismuth titanate/calcium titanate composite photocatalyst, and preparation method and application thereof |
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