CN115007164A - Preparation of rod-shaped bismuth ferrite piezoelectric catalyst and application of rod-shaped bismuth ferrite piezoelectric catalyst in preparation of hydrogen peroxide and hydrogen by catalytic cracking of water - Google Patents
Preparation of rod-shaped bismuth ferrite piezoelectric catalyst and application of rod-shaped bismuth ferrite piezoelectric catalyst in preparation of hydrogen peroxide and hydrogen by catalytic cracking of water Download PDFInfo
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- CN115007164A CN115007164A CN202210744513.8A CN202210744513A CN115007164A CN 115007164 A CN115007164 A CN 115007164A CN 202210744513 A CN202210744513 A CN 202210744513A CN 115007164 A CN115007164 A CN 115007164A
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- 229910001451 bismuth ion Inorganic materials 0.000 claims abstract description 4
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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
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/843—Arsenic, antimony or bismuth
- B01J23/8437—Bismuth
-
- B01J35/50—
-
- 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
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
- B01J37/031—Precipitation
-
- 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
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B15/00—Peroxides; Peroxyhydrates; Peroxyacids or salts thereof; Superoxides; Ozonides
- C01B15/01—Hydrogen peroxide
- C01B15/027—Preparation from water
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/042—Decomposition of water
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
- Y02P20/133—Renewable energy sources, e.g. sunlight
Abstract
The invention belongs to the technical field of catalytic total water decomposition, and particularly relates to a preparation method of a rod-shaped bismuth ferrite piezoelectric catalyst and application of the rod-shaped bismuth ferrite piezoelectric catalyst in preparation of hydrogen peroxide and hydrogen by catalytic water cracking. The rod-shaped bismuth ferrite nano material with the optimized morphology is prepared by simultaneously dissolving bismuth nitrate pentahydrate and ferric nitrate nonahydrate in a surfactant and water, dripping ammonia water to precipitate bismuth ions and ferric ions, dissolving the obtained precipitate in an alkaline solution, and finally utilizing a hydrothermal reaction method and combining a calcination process. Meanwhile, the prepared rod-shaped bismuth ferrite piezoelectric catalyst can be applied to catalytic cracking of intermediate water to prepare hydrogen peroxide and hydrogen, compared with the original bismuth ferrite, the efficiency of hydrogen production and hydrogen peroxide by bismuth ferrite piezoelectric catalysis is greatly improved, and a new way and a new direction are provided for preparing hydrogen peroxide and hydrogen by catalytic cracking of intermediate water by using the piezoelectric catalyst.
Description
Technical Field
The invention belongs to the technical field of catalytic total water decomposition, and particularly relates to a preparation method of a rod-shaped bismuth ferrite piezoelectric catalyst and application of the rod-shaped bismuth ferrite piezoelectric catalyst in preparation of hydrogen peroxide and hydrogen by catalytic water cracking.
Background
Hydrogen is a high energy density chemical fuel with a heating value (140 MJ.kg) -1 ) Is obviously higher than most of the currently used hydrocarbon fuels (such as gasoline, diesel oil, and the like, 45-50 MJ.kg -1 ). Meanwhile, hydrogen is a clean dye, only generates water after being combusted in the air, and does not contain any greenhouse gas or toxic by-products, so that the hydrogen is an effective way for solving the problems of environment and energy. H 2 O 2 As a high-efficiency environmental disinfectant, the demand is increasing, and the disinfectant is widely used in industries such as mining, electronics, paper pulp, packaging, textile bleaching and the like. Although the traditional hydrogen production method can be used for large-scale production, the environmental pollution and the safety problem are generated. Wherein, the production of H by anthraquinone method is mainly used domestically 2 O 2 Although improved, it still results in high energy consumption and serious pollution.
In the development process of new energy technology, semiconductor catalytic water decomposition is a very advantageous technology. Among the existing semiconductor catalytic water splitting technologies, the intermediate water splitting technology can effectively solve the above problems. In the process of intermediate water decomposition, free electrons can reduce water to H 2 The cavity oxidizes water to H 2 O 2 And further realize high-value utilization of water and obtain clean energy. The semiconductor catalytic water splitting technology can be completed under the driving of various energy sources, such as light energy, electric energy, mechanical energy and the like. Wherein the piezoelectric catalystCan effectively utilize wind energy, water energy, tidal energy and the like in nature, and is an effective catalysis mode. The piezoelectric catalysis can be carried out only by a single material, the separation of carriers is driven by a gravitational field generated inside, and the carriers are transferred to the surface of the material to carry out an oxidation-reduction reaction, so that the process can effectively inhibit the reverse reaction. Meanwhile, the piezo-catalysis is carried out without considering whether the energy band is matched with the reaction potential, because the migration of the carriers can cause the energy band to be inclined, so that the carriers on the conduction band which is originally higher than the reduction reaction potential and the valence band which is lower than the oxidation reaction can also participate in the reaction. Therefore, the piezoelectric catalysis is applied to the full water decomposition reaction, and the green and efficient preparation of the hydrogen peroxide is hopeful to be realized. However, most of the research on the production of hydrogen and hydrogen peroxide by the decomposition of intermediate water is focused on the fields of photocatalysis and photocatalysis, and the methods for preparing hydrogen peroxide and hydrogen by the catalytic cracking of intermediate water by using a piezoelectric catalyst are not many.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a preparation method of a rod-shaped bismuth ferrite piezoelectric catalyst, and the prepared rod-shaped bismuth ferrite piezoelectric catalyst can be applied to catalytic water splitting to prepare hydrogen peroxide and hydrogen, and can improve the yield of the hydrogen peroxide and the hydrogen.
In order to realize the purpose, the invention is realized by the following technical scheme:
the invention provides a preparation method of a rod-shaped bismuth ferrite piezoelectric catalyst, which comprises the following steps:
s1, dissolving bismuth nitrate pentahydrate and ferric nitrate nonahydrate in water and a surfactant, dropwise adding ammonia water to precipitate bismuth ions and ferric ions, and collecting precipitates;
s2, dissolving the precipitate obtained in the step S1 in an alkaline solution, and then heating and reacting at the temperature of 100-500 ℃ for 12-72 h;
s3, calcining the reaction product obtained in the step S2 at the temperature of 450-600 ℃ for 1-3h to obtain the rodlike bismuth ferrite piezoelectric catalyst.
Preferably, the molar ratio of the bismuth nitrate pentahydrate to the ferric nitrate nonahydrate is 1 (0.5-1.5). Further, the molar ratio of the bismuth nitrate pentahydrate to the ferric nitrate nonahydrate is 1: 1.
Preferably, the feed-liquid ratio of the bismuth nitrate pentahydrate to the surfactant is (1-5) g/50mL, the volume ratio of the surfactant to the water is 1:2, and the feed-liquid ratio of the bismuth nitrate pentahydrate to the alkaline solution is (1-5) g/50 mL. Further, the feed-liquid ratio of the bismuth nitrate pentahydrate to the alkaline solution is 3g/50 mL.
Preferably, the surfactant comprises ethylene glycol and the alkaline solution comprises potassium hydroxide. Further, the concentration of the potassium hydroxide is 5M.
Researches show that BiFeO is obtained after the morphology is improved by surfactants such as glycol 3 From irregular spherical particles to rod-like particles, the size also changes from microparticles to nanoparticles. Simultaneously, the rod-shaped BiFeO is prepared 3 The method is applied to preparing hydrogen peroxide and hydrogen by piezoelectric catalytic cracking of intermediate water, and the performances of piezoelectric hydrogen production and hydrogen peroxide production are greatly improved.
Preferably, the temperature of the heating reaction is 180-200 ℃ and the time is 48 h.
Preferably, the calcination temperature is 500 ℃ and the calcination time is 2 h.
Preferably, after the heating reaction of step S2, the product is further washed and dried.
The invention also provides the rod-shaped bismuth ferrite piezoelectric catalyst prepared by the preparation method.
The invention also provides application of the rod-shaped bismuth ferrite piezoelectric catalyst in preparation of hydrogen peroxide and hydrogen by catalytic cracking of water.
The invention also provides a method for preparing hydrogen peroxide and hydrogen by catalytic cracking of intermediate water, which comprises the steps of putting the rodlike bismuth ferrite piezoelectric catalyst into water, vacuumizing, and catalyzing water to generate hydrogen peroxide and hydrogen under the action of ultrasonic treatment.
Preferably, the feed-liquid ratio of the rod-shaped bismuth ferrite piezoelectric catalyst to water is (5-80) mg/50 mL. Further, the feed-liquid ratio of the rod-shaped bismuth ferrite piezoelectric catalyst to water is 5mg/50 mL.
Preferably, the power of the sonication is 200W and the frequency is 68 kHz.
Compared with the prior art, the invention has the beneficial effects that:
the invention discloses a preparation method of a rodlike bismuth ferrite piezoelectric catalyst, which comprises the steps of dissolving bismuth nitrate pentahydrate and ferric nitrate nonahydrate in a surfactant and water simultaneously, dripping ammonia water to precipitate bismuth ions and iron ions, dissolving the obtained precipitate in an alkaline solution, and finally preparing the rodlike bismuth ferrite nano material with optimized morphology by utilizing a hydrothermal reaction method and combining a calcination process. Meanwhile, the prepared rod-shaped bismuth ferrite piezoelectric catalyst can be applied to catalytic cracking of intermediate water to prepare hydrogen peroxide and hydrogen, compared with the original bismuth ferrite, the efficiency of hydrogen production and hydrogen peroxide by bismuth ferrite piezoelectric catalysis is greatly improved, and a new way and a new direction are provided for preparing hydrogen peroxide and hydrogen by catalytic cracking of intermediate water by using the piezoelectric catalyst.
Drawings
FIG. 1 shows a rod-like BiFeO 3 A flow chart of the preparation of the piezoelectric catalyst and the catalytic intermediate water decomposition;
FIG. 2 is the original BiFeO 3 And a rod-like BiFeO 3 SEM picture of (1);
FIG. 3 is the original BiFeO 3 And a rod-like BiFeO 3 XRD pattern of (a);
FIG. 4 is the original BiFeO 3 And a rod-like BiFeO 3 The performance diagram of hydrogen peroxide produced by piezoelectricity;
FIG. 5 is the original BiFeO 3 And a rod-like BiFeO 3 The performance diagram of hydrogen production by piezoelectricity.
Detailed Description
The following further describes the embodiments of the present invention. It should be noted that the description of the embodiments is provided to help understanding of the present invention, but the present invention is not limited thereto. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The experimental procedures in the following examples were carried out by conventional methods unless otherwise specified, and the test materials used in the following examples were commercially available by conventional methods unless otherwise specified.
Example 1 preparation of a Bar-shaped bismuth ferrite piezoelectric catalyst and its use in the preparation of Hydrogen peroxide and Hydrogen gas by catalytic Water splitting
According to the process flow diagram of fig. 1, the present embodiment comprises the following steps:
(1) rod-shaped bismuth ferrite (R-BiFeO) 3 ) Preparation of
3g of Bi (NO) 3 ) 3 ·5H 2 O was dissolved in 50mL of ethylene glycol and vigorously stirred until completely dissolved, and 2.511g of Fe (NO) was added to the solution 3 ) 3 ·9H 2 O and 100mL of deionized water, then dropwise adding ammonia water into the solution under vigorous stirring (750r/min) until the pH of the solution is 10-11, and leading Bi to be 3+ And Fe 3+ Completely precipitating, centrifugally collecting precipitate, washing twice by using deionized water, adding the collected precipitate into 50mL of 5M KOH solution, ultrasonically stirring for 30min (power 200W and frequency 68kHz), transferring the obtained solution into a Teflon-lined high-pressure reaction kettle, heating for 48h at 180 ℃, cooling to room temperature, repeatedly washing the obtained powdery product for 3-5 times by using deionized water, then drying in vacuum at 70 ℃, and finally, calcining the sample at 500 ℃ for 2h to obtain the rod-shaped R-BiFeO 3 A brownish red powder.
(2) The preparation method of the bismuth ferrite uses original bismuth ferrite with common morphology as a reference, and comprises the following steps:
weighing 3g Bi (NO) 3 ) 3 ·5H 2 O was dissolved in 50mL of water and vigorously stirred (750r/min) until completely dissolved, and 2.511g of Fe (NO) were added to the solution 3 ) 3 ·9H 2 O and 100mL of a large amount of deionized water, adding the solution into 50mL of 12M KOH solution, carrying out ultrasonic treatment for a period of time, stirring, transferring the obtained solution into a Teflon-lined high-pressure reaction kettle, heating at 180 ℃ for 48h, cooling to room temperature, repeatedly washing the obtained powdery product with deionized water for 3-5 times, carrying out vacuum drying at 70 ℃, and finally calcining the sample at 500 ℃ for 2h to obtain BiFeO 3 A brownish red powder.
For BiFeO respectively 3 And R-BiFeO 3 XRD and SEM tests are carried out. As can be seen from FIGS. 2 and 3, after the morphology is improved, BiFeO 3 From irregularly spherical particles to rod-like particles, i.e. the original BiFeO 3 BiFeO with irregular spherical shape and processed by glycol 3 Presenting a rod-like shape; the size is changed from microparticles to nanoparticles.
(3) Piezoelectric catalytic water splitting
Respectively weighing 5mg of BiFeO in the steps (1) and (2) 3 Powder and R-BiFeO 3 The powder was dispersed in 50mL of deionized water, the vessel containing the mixture was sealed, argon was introduced to remove the air from the vessel, and the vessel was placed in an ultrasonic generator at a power of 200W and a frequency of 68kHz for ultrasonic treatment.
The hydrogen content was measured by gas chromatography using a closed sampling needle to take a 0.4mL sample bottle of gas. Measuring the catalytic solution in a 1mL sample bottle by using a pipette, transferring the catalytic solution into a 10mL volumetric flask, then respectively adding 3mL phosphate buffer solution, 50 mu L N-diethyl-p-phenylenediamine (DPD) solution (10mg/mL) and Peroxidase (POD) solution (1mg/mL), finally adding deionized water to constant volume to 10mL, and detecting the content of hydrogen peroxide in the mixed solution with constant volume by using an ultraviolet spectrophotometer.
From the hydrogen production performance test result of fig. 4 and the hydrogen production performance test result of fig. 5, it can be known that after the morphology growth is regulated, the piezoelectric hydrogen production and hydrogen production performance of the bismuth ferrite crystal are greatly improved, which are 2.5 and 2.6 times of the piezoelectric catalytic hydrogen production and hydrogen peroxide of the original bismuth ferrite respectively. Description of the rod-shaped BiFeO 3 Compared with the original BiFeO 3 Presents better hydrogen peroxide generation performance and is rod-shaped BiFeO 3 Compared with the original BiFeO 3 And the hydrogen production performance is better.
Example 2 preparation of a Bar-shaped bismuth ferrite piezoelectric catalyst and its use in catalytic Water splitting for the preparation of Hydrogen peroxide and Hydrogen gas
According to the process flow diagram of fig. 1, the present embodiment comprises the following steps:
(1) rod-shaped bismuth ferrite (R-BiFeO) 3 ) The preparation of (1): the specific preparation method is the same as that of example 1.
(2) The preparation method is the same as that of example 1, taking the original bismuth ferrite with common morphology as a reference.
Likewise, after morphology improvement, BiFeO 3 The irregular spherical particles are changed into rod-shaped particles, and the size of the particles is changed from micro-particles to nano-particles.
(3) Piezoelectric catalytic water splitting
And (3) respectively weighing 20mg of the powder in the step (1) and the step (2), dispersing the powder in 50mL of deionized water, sealing a container containing the mixed solution, and introducing argon to remove air in the bottle. Then, the mixture was placed in an ultrasonic generator with a power of 200W and a frequency of 68kHz to be subjected to ultrasonic treatment. Finally, the hydrogen content and the hydrogen peroxide content were measured by the method of example 1.
Similarly, the performance of the rodlike bismuth ferrite is greatly improved compared with the performance of the original bismuth ferrite with common morphology for producing hydrogen and hydrogen peroxide through piezoelectric catalysis.
Example 3 preparation of a Bar-shaped bismuth ferrite piezoelectric catalyst and its use in catalytic Water splitting for the preparation of Hydrogen peroxide and Hydrogen gas
According to the process flow diagram of fig. 1, the present embodiment comprises the following steps:
(1) rod-shaped bismuth ferrite (R-BiFeO) 3 ) The preparation of (1): the preparation method is the same as that of example 1, except that the obtained solution is transferred to a Teflon-lined autoclave and then heated at 200 ℃ for 48 hours.
(2) The preparation method is the same as that of example 1, taking the original bismuth ferrite with common morphology as a reference.
Likewise, after morphology improvement, BiFeO 3 The irregular spherical particles are changed into rod-shaped particles, and the size of the particles is changed from micro-particles to nano-particles.
(3) Piezoelectric catalytic water splitting
80mg of the powder obtained in the step (1) and the powder obtained in the step (2) are respectively weighed and dispersed in 50mL of deionized water, then a container containing the mixed solution is sealed, and argon is introduced to remove air in the bottle. Then, the mixture was placed in an ultrasonic generator with a power of 200W and a frequency of 68kHz to be subjected to ultrasonic treatment. Finally, the hydrogen content and the hydrogen peroxide content were measured by the method of example 1.
Similarly, the performance of the rodlike bismuth ferrite is greatly improved compared with the performance of the original bismuth ferrite with common morphology for producing hydrogen and hydrogen peroxide through piezoelectric catalysis.
The embodiments of the present invention have been described in detail, but the present invention is not limited to the described embodiments. It will be apparent to those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, and the scope of protection is still within the scope of the invention.
Claims (10)
1. A preparation method of a rod-shaped bismuth ferrite piezoelectric catalyst is characterized by comprising the following steps:
s1, dissolving bismuth nitrate pentahydrate and ferric nitrate nonahydrate in water and a surfactant, dropwise adding ammonia water to precipitate bismuth ions and ferric ions, and collecting precipitates;
s2, dissolving the precipitate obtained in the step S1 in an alkaline solution, and then heating and reacting at the temperature of 100-500 ℃ for 12-72 h;
s3, calcining the reaction product obtained in the step S2 at the temperature of 450-600 ℃ for 1-3h to obtain the rodlike bismuth ferrite piezoelectric catalyst.
2. The method for preparing the rod-shaped bismuth ferrite piezoelectric catalyst according to claim 1, wherein the molar ratio of the bismuth nitrate pentahydrate to the iron nitrate nonahydrate is 1 (0.5-1.5).
3. The preparation method of the rod-shaped bismuth ferrite piezoelectric catalyst according to claim 1, wherein the feed-liquid ratio of the bismuth nitrate pentahydrate to the surfactant is (1-5) g/50mL, the volume ratio of the surfactant to water is 1:2, and the feed-liquid ratio of the bismuth nitrate pentahydrate to the alkaline solution is (1-5) g/50 mL.
4. The method of claim 1, wherein the surfactant comprises ethylene glycol, and the alkaline solution comprises potassium hydroxide.
5. The method as claimed in claim 1, wherein the temperature of the heating reaction is 180-200 ℃ and the time is 48 h.
6. The method for preparing a bismuth ferrite rod piezoelectric catalyst according to claim 1, wherein the calcination temperature is 500 ℃ and the calcination time is 2 hours.
7. The bismuth ferrite piezoelectric catalyst in rod form obtained by the production method according to any one of claims 1 to 6.
8. The use of the bismuth ferrite rod-shaped piezoelectric catalyst according to claim 7 for the catalytic cracking of water to produce hydrogen peroxide and hydrogen.
9. A method for preparing hydrogen peroxide and hydrogen by catalytic cracking of intermediate water, characterized in that the rod-shaped bismuth ferrite piezoelectric catalyst of claim 7 is put into water, and the water is catalyzed to generate hydrogen peroxide and hydrogen under the action of ultrasonic treatment after being vacuumized.
10. The method of claim 9, wherein the ratio of the bismuth ferrite rod-shaped piezoelectric catalyst to water is (5-80) mg/50 mL.
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