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CN112516990B - Synthetic method and application of layered perovskite type photocatalyst - Google Patents

Synthetic method and application of layered perovskite type photocatalyst Download PDF

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CN112516990B
CN112516990B CN202011525565.3A CN202011525565A CN112516990B CN 112516990 B CN112516990 B CN 112516990B CN 202011525565 A CN202011525565 A CN 202011525565A CN 112516990 B CN112516990 B CN 112516990B
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layered perovskite
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sodium hydroxide
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CN112516990A (en
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师红旗
张健
郎俊杰
汤涛
丁毅
沈晓冬
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Jiangsu Ruiying New Material Technology Development Co ltd
Nanjing Tech University
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Nanjing Tech University
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    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/16Catalysts 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
    • B01J23/18Arsenic, antimony or bismuth
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/30Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/39Photocatalytic properties
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    • C01B3/00Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
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    • C01B3/04Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
    • C01B3/042Decomposition of water
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Abstract

The invention discloses a layered perovskite typeThe synthesis method of the photocatalyst comprises the following steps: (1) mixing SrCl2·6H2Dissolving O, a bismuth source and tetrabutyl titanate in a nitric acid solution to obtain a raw material solution; (2) dripping the obtained raw material liquid into a sodium hydroxide solution, and then carrying out hydrothermal synthesis to obtain a white suspension; (3) cooling and filtering the suspension, taking filter residue, washing and drying the filter residue to obtain the layered perovskite Sr2Bi4Ti5O18. Also discloses the application of the lamellar perovskite type photocatalyst in photocatalytic reaction. The preparation process is simple, the reaction controllability is good, and the formed layered perovskite type Sr2Bi4Ti5O18Strong light absorption capacity, wide light absorption range, high activity of photon-generated carriers and strong photocatalytic hydrogen production capacity compared with the traditional TiO2More than 3.2 times of that of the solid phase sintering synthesis, more than 2.8 times of that of the solid phase sintering synthesis, and is Bi4Ti3O12More than 2 times.

Description

Synthetic method and application of layered perovskite type photocatalyst
Technical Field
The invention relates to a synthesis method and application of a layered perovskite type photocatalyst, and belongs to the field of photocatalysts.
Background
With the continuous increase of the world population and the rapid development of industrialization, the energy consumption and the energy demand are high, and the two problems of energy crisis and environmental pollution caused by the high energy consumption and the high energy demand are more and more noticed. In recent years, photocatalytic technology has been rapidly developed, and pollutant decomposition efficiency and hydrogen production efficiency have been continuously improved. However, at present, most of semiconductor materials have short photon-generated carrier life and short average diffusion length, and the photon-generated electron hole pair has low separation efficiency and low photocatalytic activity, and the photocatalytic performance of the semiconductor materials can not meet the requirements of practical application.
The perovskite material has high light absorption rate and energy conversion efficiency in a visible light range, and has good application prospect in the production of renewable energy sources such as photovoltaics, photocatalysis and the like. Sr2Bi4Ti5O18Located at the cross point of the traditional ferroelectric, laminated bismuth-based semiconductor and perovskite structure crystal, integrates a plurality of advantages and shows great photocatalytic potential. However, at present, to Sr2Bi4Ti5O18The research is mainly focused on the application of the ferroelectric ceramic, and the ferroelectric ceramic is not applied to the field of photocatalysis.
Disclosure of Invention
In order to solve the above problems, the present invention provides a method for synthesizing a layered perovskite photocatalyst, the layered perovskite photocatalyst having the chemical formula: sr2Bi4Ti5O18(ii) a The synthesis method comprises the following steps:
(1) mixing SrCl2·6H2Dissolving O, a bismuth source and tetrabutyl titanate in a nitric acid solution to obtain a raw material solution;
(2) dripping the obtained raw material liquid into a sodium hydroxide solution, and then carrying out hydrothermal synthesis to obtain a white suspension;
(3) cooling and filtering the suspension, taking filter residue, washing and drying the filter residue to obtain the layered perovskite Sr2Bi4Ti5O18
In the step (2), after the dropwise addition of the raw material liquid to the sodium hydroxide solution is completed, the stirring is continued for 30-120 minutes, so that the reaction is fully performed, and simultaneously, the reaction heat can be discharged in time, thereby avoiding the influence on the smooth performance of the subsequent hydrothermal reaction due to the excessive heat released during the acid-base neutralization reaction. The strong basicity of the concentrated sodium hydroxide solution hydrolyzes tetrabutyl titanate into dissolved titanate, and the uniform reaction solution is favorable for the formation of a nano structure. Further hydrothermal reaction makes the reactant dissolve-recrystallize to reach atom level uniform mixing.
Specifically, the bismuth source is bismuth nitrate or bismuth sulfate.
The preparation process is simple, the reaction controllability is good, and the formed layered perovskite type Sr2Bi4Ti5O18Strong light absorption capacity, wide light absorption range, high activity of photon-generated carriers and strong photocatalytic hydrogen production capacity compared with the traditional TiO2More than 3.2 times of that of the solid phase sintering synthesis, more than 2.8 times of that of the solid phase sintering synthesis, and is Bi4Ti3O12More than 2 times.
Sr2Bi4Ti5O18Is a typical bismuth-layer perovskite structure ferroelectric material, and has the basic structural characteristics that a fluorite structure bismuth oxide layer (Bi) is inserted into 5 perovskite layers2O2)2+Due to the insertion of the bismuth-oxygen layer, the material system shows obvious anisotropy, and the anisotropy causes the material system to tend to form a nanosheet shape with high surface area in the process of synthesis and preparation; the valence band energy level of the photocatalyst consists of highly discrete Bi 6s and O2 p hybrid orbitals, and the highly discrete orbital energy level is more beneficial to the migration of photo-generated holes and corresponding photocatalytic oxidation reaction. And due to the presence of the bismuth oxide layer, Sr is enabled2Bi4Ti5O18Has very high structure and performance adjustability. The ferroelectric property of the strontium titanate can be improved to a certain extent by reasonably utilizing the doping and other means, which is very beneficial to effectively separating photon-generated carriers and improving the photocatalytic activity, but the existing Sr is2Bi4Ti5O18The product can not be used as a photocatalyst.
The existing Sr is found through experiments2Bi4Ti5O18The product is mainly applied to ferroelectric ceramics, Sr2Bi4Ti5O18The production of (A) is synthesized by high-temperature solid-phase reaction, which results in larger particle size of the product, insufficient effective reaction point, failure of effective absorption of photons and generation of photon-generated carriers. Sr produced by hydrothermal synthesis method2Bi4Ti5O18The product has proper forbidden band width and nano structure, can effectively absorb photons to the maximum extent and generate photogenerationCarriers and thereby functions as a photocatalyst. Compared with solid-phase sintered crystals, the hydrothermal synthesis has less growth defects and good orientation, and the proper size effectively reduces the recombination of photoproduction electrons and holes, namely Sr2Bi4Ti5O18The spontaneous ferroelectric polarization further promotes the separation and migration of photo-generated electrons and holes, and greatly increases the photocatalytic performance of the photo-generated electrons.
Specifically, the temperature of the hydrothermal synthesis is 180-240 ℃, and the time is 24-72 h. Under the condition, the synthesized Sr2Bi4Ti5O18Presenting a sheet-like morphology. In the temperature and time range, Sr is favored2Bi4Ti5O18The synthesis of (2) and the reduction of the generation of miscellaneous items, and the improvement of the crystallinity along with the increase of the temperature and the prolongation of the time.
Specifically, the concentration of the nitric acid solution is 4-5mol/L, and the concentration of the sodium hydroxide solution is 6-9 mol/L. The volume ratio of the nitric acid solution to the sodium hydroxide solution is 1:1-1: 1.2.
At the above nitric acid solution concentration, the metal ions can be dissolved rapidly and sufficiently, but the layered perovskite type Sr2Bi4Ti5O18Cannot be synthesized under the acidic condition, and in order to compensate the defect, the sodium hydroxide with the concentration is used for providing a strong alkaline environment required by the reaction so as to obtain the desired product. The desired product can be obtained within the limits of the nitric acid solution concentration, the sodium hydroxide solution concentration and the volume ratio of the nitric acid solution to the sodium hydroxide solution. When the alkali concentration is insufficient or the alkali is excessive, the product has excessive impurities, which is not beneficial to obtaining pure phase products.
The volume ratio of the nitric acid solution to the sodium hydroxide solution also plays a role in timely absorbing reaction heat under the condition of ensuring that the effective alkali concentration is improved, and the sufficient volume of the solution can timely absorb the reaction heat, so that the solution volatilization and the high-temperature decomposition of some precursors in the solution caused by the sharp rise of the solution temperature in the dripping process are avoided.
Further, the drying temperature of the filter residue is 60-80 ℃, and the drying time is 7-10 h. After hydrothermal synthesis, the mixture is naturally cooled to room temperature and then filtered. At the temperature, the product after hydrothermal reaction can be dried quickly without affecting the structure of the product.
The layered perovskite type Sr as described in any one of the above2Bi4Ti5O18The photocatalyst is applied as a photocatalyst.
The invention provides the layered perovskite Sr2Bi4Ti5O18The preparation method of the photocatalyst has the advantages that the prepared photocatalyst is pure phase, has regular flaky shape, provides active sites for photocatalytic reaction, has better water decomposition performance than the traditional photocatalyst, has mild synthesis conditions, high product purity, complete crystal grain development, small grain size, uniform distribution, strong shape controllability and simple synthesis route and device, and is beneficial to realizing large-scale production.
Drawings
FIG. 1 is Sr synthesized in example 42Bi4Ti5O18X-ray diffraction (XRD) pattern of (a).
FIG. 2 shows Sr synthesized in example 42Bi4Ti5O18Scanning Electron Microscope (SEM) images of (a).
Detailed Description
Example 1
1. 30mL of 4mol/L nitric acid solution is measured and poured into a beaker according to Sr2Bi4Ti5O18Weighing 1.5mmol SrCl2·6H2O、1.5mmol Bi2(SO4)3And 3.75mmol of tetrabutyl titanate is dissolved in the nitric acid solution, and the mixture is stirred for 10min to obtain a raw material solution.
2. Weighing 7.2g NaOH and dissolving in 30mL deionized water, stirring for 5min, and cooling to room temperature to obtain sodium hydroxide solution.
3. Dropping the raw materials into the sodium hydroxide solution by using a dropper while stirring, stirring for 30min after the dropping is finished to uniformly mix the raw materials, transferring the mixture into a 100mL hydrothermal reaction kettle, and preserving the heat for 72h at the temperature of 180 ℃. After the reaction is finished, cooling the reaction solution to normal temperature, centrifuging to take precipitate, and washing with ethanol and deionized water respectivelyOven drying at 60 deg.C for 10 hr for 3 times, grinding into powder, and making into Sr2Bi4Ti5O18Photocatalyst 1 #.
And (3) detection:
40mg of Sr2Bi4Ti5O18Photocatalyst 1#, 40mg traditional photocatalyst TiO240mg of photocatalyst Bi4Ti3O12And 40mg of solid phase sintered Sr2Bi4Ti5O18Respectively putting into methanol solution to obtain four test solutions, irradiating with 500W medium-pressure mercury lamp for 5 hr, and measuring Sr2Bi4Ti5O18Photocatalyst No. 1 catalyzing to generate 16 mu mol H2,Bi4Ti3O12Photocatalyst catalyzed generation of 7.9 mu mol H2And solid phase sintering of synthesized Sr2Bi4Ti5O18Catalytic generation of H2 5.6μmol,TiO2Photocatalytic generation of H2Only 5. mu. mol. The methanol solution was mixed with 3ml of methanol and 30ml of deionized water.
Example 2
1. 28.4mL of 4.3mol/L nitric acid solution is weighed and poured into a beaker according to Sr2Bi4Ti5O18Weighing 1.5mmol SrCl2·6H2O、3mmol Bi(NO3)3·5H2Dissolving O and 3.75mmol tetrabutyl titanate in nitric acid solution, and stirring for 10min to obtain a raw material solution.
2. Weighing 8.4g NaOH and dissolving in 30mL deionized water, stirring for 5min, and cooling to room temperature to obtain sodium hydroxide solution.
3. Dropping the raw materials into the sodium hydroxide solution by using a dropper while stirring, stirring for 60min after the dropping is finished to uniformly mix the raw materials, transferring the mixture into a 100mL hydrothermal reaction kettle, and preserving the heat for 56h at the temperature of 200 ℃. After the reaction is finished, cooling the reaction liquid to normal temperature, centrifuging to take precipitate, washing 3 times by using ethanol and deionized water respectively, drying in a 67 ℃ oven for 9 hours, grinding into powder to prepare Sr2Bi4Ti5O18Photocatalyst 2 #.
And (3) detection:
40mg of Sr2Bi4Ti5O18Photocatalyst 2#, 40mg traditional photocatalyst TiO240mg of photocatalyst Bi4Ti3O12And 40mg of solid phase sintered Sr2Bi4Ti5O18Respectively putting into methanol solution to obtain four test solutions, irradiating with 500W medium-pressure mercury lamp for 5 hr, and measuring Sr2Bi4Ti5O18Photocatalyst 2# catalyzes and generates 15.4 mu mol H2,Bi4Ti3O12Photocatalyst catalyzed generation of 7.9 mu mol H2And solid phase sintering of synthesized Sr2Bi4Ti5O18Catalytic generation of H2 5.6μmol,TiO2Photocatalytic generation of H2Only 5. mu. mol. The methanol solution was mixed with 3ml of methanol and 30ml of deionized water.
Example 3
1. 26.7mL of 4.6mol/L nitric acid solution is weighed and poured into a beaker according to Sr2Bi4Ti5O18Weighing 1.5mmol SrCl2·6H2O、1.5mmol Bi2(SO4)3And 3.75mmol of tetrabutyl titanate is dissolved in the nitric acid solution, and the mixture is stirred for 10min to obtain a raw material solution.
2. Weighing 9.6g of NaOH and dissolving in 30mL of deionized water, stirring for 5min, and cooling to room temperature to obtain a sodium hydroxide solution.
3. Dropping the raw materials into the sodium hydroxide solution by using a dropper while stirring, stirring for 90min after the dropping is finished to uniformly mix the raw materials, transferring the mixture into a 100mL hydrothermal reaction kettle, and preserving the heat for 40h at 220 ℃. After the reaction is finished, cooling the reaction liquid to normal temperature, centrifuging to take precipitate, washing 3 times by using ethanol and deionized water respectively, drying in an oven at 73 ℃ for 8 hours, grinding into powder to prepare Sr2Bi4Ti5O18Photocatalyst # 3.
And (3) detection:
40mg of Sr2Bi4Ti5O18Photocatalyst 3#, 40mg traditional photocatalyst TiO240mg lightCatalyst Bi4Ti3O12And 40mg of solid phase sintered Sr2Bi4Ti5O18Respectively putting into methanol solution to obtain four test solutions, irradiating with 500W medium-pressure mercury lamp for 5 hr, and measuring Sr2Bi4Ti5O18Photocatalyst No. 3 catalyzes and generates 15.7 mu mol H2,Bi4Ti3O12Photocatalyst catalyzed generation of 7.9 mu mol H2And solid phase sintering of synthesized Sr2Bi4Ti5O18Catalytic generation of H2 5.6μmol,TiO2Photocatalytic generation of H2Only 5. mu. mol. The methanol solution was mixed with 3ml of methanol and 30ml of deionized water.
Example 4
1. 25mL of 5mol/L nitric acid solution is weighed and poured into a beaker according to Sr2Bi4Ti5O18Weighing 1.5mmol SrCl2·6H2O、3mmol Bi(NO3)3·5H2Dissolving O and 3.75mmol tetrabutyl titanate in nitric acid solution, and stirring for 10min to obtain a raw material solution.
2. Weighing 10.8g of NaOH to be dissolved in 30mL of deionized water, stirring for 5min, and cooling to room temperature to obtain a sodium hydroxide solution.
3. Dropping the raw materials into the sodium hydroxide solution by using a dropper while stirring, stirring for 120min after the dropping is finished to uniformly mix the raw materials, transferring the mixture into a 100mL hydrothermal reaction kettle, and preserving the heat for 24h at the temperature of 240 ℃. After the reaction is finished, cooling the reaction liquid to normal temperature, centrifuging to take precipitate, washing 3 times by using ethanol and deionized water respectively, drying for 7 hours in an oven at 80 ℃, grinding into powder, and preparing Sr2Bi4Ti5O18Photocatalyst No. 4.
And (3) detection:
40mg of Sr2Bi4Ti5O18Photocatalyst 4#, 40mg traditional photocatalyst TiO240mg of photocatalyst Bi4Ti3O12And 40mg of solid phase sintered Sr2Bi4Ti5O18Respectively adding into methanol solution to obtain productThe test solutions were inoculated, and then after irradiating the four test solutions for 5 hours with a 500W medium-pressure mercury lamp, Sr was measured2Bi4Ti5O18Photocatalyst No. 4 catalyzed generation of 16.1. mu. mol H2,Bi4Ti3O12Photocatalyst catalyzed generation of 7.9 mu mol H2And solid phase sintering of synthesized Sr2Bi4Ti5O18Catalytic generation of H2 5.6μmol,TiO2Photocatalytic generation of H2Only 5. mu. mol. The methanol solution was mixed with 3ml of methanol and 30ml of deionized water.
The above examples show that the layered perovskite Sr prepared by the present application2Bi4Ti5O18The water decomposition performance of the photocatalyst is greatly superior to that of the traditional photocatalyst TiO2、Bi4Ti3O12Sr synthesized by photocatalyst and solid phase sintering2Bi4Ti5O18

Claims (6)

1. A method for synthesizing a layered perovskite photocatalyst is characterized in that,
the layered perovskite type photocatalyst has a chemical formula as follows: sr2Bi4Ti5O18
The synthesis method comprises the following steps:
(1) mixing SrCl2·6H2Dissolving O, a bismuth source and tetrabutyl titanate in a nitric acid solution to obtain a raw material solution;
(2) dripping the obtained raw material liquid into a sodium hydroxide solution, and then carrying out hydrothermal synthesis to obtain a white suspension;
(3) cooling and filtering the suspension, taking filter residue, washing and drying the filter residue to obtain the layered perovskite Sr2Bi4Ti5O18
The temperature of the hydrothermal synthesis is 180 ℃ and 240 ℃, and the time is 24-72 h; the concentration of the sodium hydroxide solution is 6-9 mol/L.
2. The synthesis method according to claim 1, wherein the concentration of the nitric acid solution is 4 to 5 mol/L.
3. The synthesis method according to claim 2, wherein the volume ratio of the nitric acid solution to the sodium hydroxide solution is 1:1-1: 1.2.
4. The method of synthesis of claim 1, wherein the bismuth source is bismuth nitrate or bismuth sulfate.
5. The synthesis method according to claim 1, wherein the drying temperature of the filter residue is 60-80 ℃ and the drying time is 7-10 h.
6. Use of a layered perovskite photocatalyst as defined in any one of claims 1 to 5 in photocatalytic reactions.
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