CN111268649B - Three-dimensional marigold-shaped bismuth oxyiodate, and preparation method and application thereof - Google Patents
Three-dimensional marigold-shaped bismuth oxyiodate, and preparation method and application thereof Download PDFInfo
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- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 35
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
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- CBACFHTXHGHTMH-UHFFFAOYSA-N 2-piperidin-1-ylethyl 2-phenyl-2-piperidin-1-ylacetate;dihydrochloride Chemical compound Cl.Cl.C1CCCCN1C(C=1C=CC=CC=1)C(=O)OCCN1CCCCC1 CBACFHTXHGHTMH-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000003960 organic solvent Substances 0.000 claims abstract description 11
- 239000011259 mixed solution Substances 0.000 claims abstract description 10
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- 239000000047 product Substances 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 42
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 34
- 239000011941 photocatalyst Substances 0.000 claims description 15
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000003760 magnetic stirring Methods 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 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 description 5
- JLKDVMWYMMLWTI-UHFFFAOYSA-M potassium iodate Chemical compound [K+].[O-]I(=O)=O JLKDVMWYMMLWTI-UHFFFAOYSA-M 0.000 claims description 3
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Abstract
The invention relates to three-dimensional marigold-shaped bismuth oxyiodate and a preparation method and application thereof. The preparation method specifically comprises the following steps: (a) Bi (NO) 3 ·5H 2 O and KIO 3 Uniformly dispersing the mixture in a mixed organic solvent, and uniformly stirring to obtain a mixed solution A; (b) Transferring the mixed solution A into a reaction vessel for solvothermal reaction to obtain a reaction crude product B; (c) And (3) sequentially carrying out centrifugal washing and drying on the reaction crude product B to obtain a three-dimensional marigold-shaped bismuth oxyiodide product, wherein the preparation of the bismuth oxyiodide can be used in the field of catalysis. Compared with the prior art, the three-dimensional marigold-shaped bismuth oxyiodate has excellent electron hole separation capacity, and the biomimetic flower-shaped structure enables the bismuth oxyiodate to have higher photocatalytic activity.
Description
Technical Field
The invention relates to the field of chemical industry, and particularly relates to three-dimensional marigold-shaped bismuth oxyiodate, a preparation method and application thereof.
Background
In recent years, aiming at the problems of energy demand, environmental protection and the like, the photocatalytic technology is considered as a new technology with great prospect, can directly utilize solar energy, is green, environment-friendly and safe, and provides an effective and feasible solution for solving the energy and environmental crisis. However, the existing photocatalyst has low activity, weak response capability under visible light and insufficient industrial application, so that the development of a photocatalyst with a visible light broad-spectrum response is very necessary.
BiOIO 3 The first report in 2011 shows that the material is a polar semiconductor material and has an orthorhombic phase structure. BiOIO 3 Not only possess two isolated cation pairs (Bi) 3+ And I 5+ ) And exhibits an Oriviris type (Bi) 2 O 2 ) 2+ In the layered structure of (1), a polar polyhedron (IO) is present in the middle of the layered structure 3 ) - . Pure BiOIO 3 The band gap of the crystal is about 3.1eV, and the potential of the valence band is +4.08eV, so that the hole of the valence band has extremely strong oxidizability, and is beneficial to the oxidation removal of pollutants. However, due to BiOIO 3 The charge carriers still have a relatively large recombination rate, which adversely affects the photocatalytic efficiency, and thus the modified BiOIO 3 Therefore, the method can be popularized and applied to become a hot spot of research of numerous scholars. At present, designing and constructing a morphology regulating photocatalyst is widely concerned by academia, and is considered to be a modification direction which is simple and has wide application prospect.
Patent CN107469839A discloses a preparation method of bismuth oxyiodate photocatalyst, bismuth nitrate pentahydrate is added into an ethylene glycol solvent, and stirred for dissolution; adding potassium iodate into the solution, so that the molar ratio of the added potassium iodate to the pentahydrate bismuth nitrate is 1:1, and continuously stirring; placing the obtained precursor solution into a high-speed centrifuge for centrifugal washing, wherein the centrifugal speed is 6000-8000rpm, and washing with deionized water and absolute ethyl alcohol to remove impurities; putting the sample obtained by centrifugation into an oven for drying; and taking out the dried sample, putting the sample into a muffle furnace, and calcining the sample in an air atmosphere for 1-2h at the temperature of 250-350 ℃ to obtain the bismuth oxyiodate photocatalyst. The preparation process is complex, the flaky shape of the obtained bismuth oxyiodide is disordered, and the photocatalytic activity is not high enough.
Disclosure of Invention
The invention aims to solve the problems and provide bismuth oxyiodide and a preparation method and application thereof.
The purpose of the invention is realized by the following technical scheme:
the preparation method of the three-dimensional marigold-shaped bismuth oxyiodate is characterized by comprising the following steps of:
(a) Bi (NO) 3 ·5H 2 O and KIO 3 Uniformly dispersing the mixture in a mixed organic solvent, and uniformly stirring to obtain a mixed solution A;
(b) Transferring the mixed solution A into a reaction vessel for solvothermal reaction to obtain a reaction crude product B;
(c) And (4) sequentially carrying out centrifugal washing and drying on the reaction crude product B to obtain a finished bismuth oxyiodide product.
Preferably, in step (a), bi (NO) 3 ·5H 2 O and KIO 3 Is 1:1. The bismuth oxyiodide consists of (Bi) 2 O 2 ) 2+ And (IO 3) - Ion pairs are made with a stoichiometric ratio of 1:1, so the molar ratio is selected for preparation.
Preferably, the addition ratio of the bismuth nitrate pentahydrate to the mixed organic solvent is (1-4) mmol:60ml. The feeding ratio can ensure that the bismuth nitrate pentahydrate is uniformly and completely dissolved in the mixed organic solvent, and 60ml of the mixed organic solvent ensures that the solvent thermal reaction can be safely and effectively carried out in a 100ml reaction kettle.
Preferably, in step (a), the mixed organic solvent comprises ethylene glycol and ethanol. From the thermodynamic perspective, the growth of the nanocrystals has the characteristic of bipolar differentiation, the low dielectric constant can inhibit the bipolar differentiation, so that the nanocrystals with more uniform distribution can be obtained, the ethanol has a lower dielectric constant, the high viscosity of the solvent has a key effect on the formation of the flower-shaped structure, and the ethylene glycol has a better viscosity, so that the flower-shaped morphology can be formed.
Preferably, the molar ratio of the ethylene glycol to the ethanol is 1 (2-3). (the proportion has proper dielectric constant and viscosity, so that the motion dispersion of the nanocrystalline is greatly reduced, the growing nanocrystalline is aggregated together in the initial growth stage and keeps the aggregated attitude unchanged, and finally, the sheets are connected with each other along with the growth of the nanosheets to finally form a flower-shaped appearance)
Preferably, in the step (a), magnetic stirring is adopted, the rotating speed of the magnetic stirring is 600-900r/min, and the time of the magnetic stirring is 30-50min.
Preferably, in step (b), the reaction temperature of the solvothermal reaction is 160-180 ℃ and the reaction time is 25-48h. (the product obtained in the reaction temperature range has better appearance and crystallinity and higher photocatalytic activity)
Preferably, in the step (b), deionized water and absolute ethyl alcohol are adopted for centrifugal washing, the rotating speed of the centrifugal washing is 5000-6000r/min, and the times of the centrifugal washing are 4-5.
Preferably, in step (b), the drying temperature is 80-100 ℃ and the drying time is 8-10h.
The bismuth oxyiodate prepared by the preparation method is in a marigold nano flower shape.
The bismuth oxyiodate in the invention has excellent light conversion activity in the photocatalyst.
The application of the bismuth oxyiodate is suitable for the fields of hydrogen production by photolysis of water, water treatment, bacterial microorganism inactivation, heavy metal removal, carbon dioxide reduction, nitrogen fixation and the like.
The invention provides a simple method for preparing three-dimensional marigold-shaped bismuth oxyiodate with visible-light broad-spectrum response, which is used for preparing and synthesizing three-dimensional marigold-shaped bismuth oxyiodate with a bionic flower shape by a solvothermal method.
Compared with the prior art, the invention has the beneficial effects that:
1) The method adjusts the shape self-assembly growth to synthesize the three-dimensional marigold-shaped bismuth oxyiodide by adjusting the ratio of the glycol to the ethanol through the solvothermal method, and has excellent electricityThe bismuth oxyiodide has high photocatalytic activity due to the bionic flower-shaped structure, the removal efficiency of heavy metal mercury under visible light is 78%, the three-dimensional marigold-shaped configuration of the bismuth oxyiodide can increase the absorption and utilization efficiency of visible light, and the photocatalytic reaction active sites can be increased, the three-dimensional marigold-shaped configuration shortens the migration path of electron hole pairs, improves the charge carrier separation efficiency, and is favorable for generating more active oxygen species (O) 2 - and OH) has wide application prospect in the aspects of solar energy utilization, environmental purification and the like.
2) The invention is suitable for the fields of hydrogen production by photolysis of water, water treatment, inactivation of bacteria and microorganisms, heavy metal removal, carbon dioxide reduction, nitrogen fixation and the like, has wide application range, high treatment efficiency, greenness, sustainability, broad spectrum safety and important practical significance for solving the energy crisis and environmental protection, and can provide a solution with a prospect for solving the energy and environmental crisis faced by the current society.
Drawings
FIG. 1 is an XRD pattern of three-dimensional marigold-like bismuth oxyiodate obtained in example 1;
FIG. 2 is an SEM photograph of three-dimensional marigold-like bismuth oxyiodate prepared in example 1;
fig. 3 is data of the heavy metal mercury removal experiment in example 4.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments.
Example 1
The bismuth oxyiodate is prepared by a preparation method comprising the following steps of:
(a) Weighing 1mmol of Bi (NO) 3 ·5H 2 O and 1mmol of KIO 3 Completely dispersing the mixture into 60ml of ethylene glycol and ethanol mixed organic solvent, wherein the proportion of the ethylene glycol to the ethanol is 1:2, and then magnetically stirring the mixture for 50min to obtain a mixed solution, wherein the rotating speed of the magnetic stirring is 600r/min;
(b) Transferring the mixed solution into a 100ml hydrothermal kettle, carrying out hydrothermal reaction at 180 ℃ for 25h, and then cooling to room temperature to obtain a reaction crude product;
(c) And (3) centrifugally washing the reaction crude product for 5 times by using deionized water and absolute ethyl alcohol, setting the centrifugal rotating speed at 5000r/min, and drying the centrifugally collected product in a drying box at 90 ℃ for 10 hours to obtain the three-dimensional marigold-shaped bismuth oxyiodate photocatalyst.
FIG. 1 is an XRD pattern of the prepared three-dimensional marigold-shaped bismuth oxyiodate photocatalyst, and the characteristic peak of the three-dimensional marigold-shaped bismuth oxyiodate photocatalyst can be clearly seen and conforms to a standard XRD card (ICSD # 262019), which proves the successful synthesis and preparation of the sample.
FIG. 2 is an SEM image of the prepared three-dimensional marigold-shaped bismuth oxyiodate photocatalyst, wherein the three-dimensional marigold-shaped structure is clearly shown, and bismuth oxyiodate nanosheets are self-assembled and cured in a solvothermal reaction to form the three-dimensional marigold-shaped bismuth oxyiodate photocatalyst.
Example 2
The bismuth oxyiodate is prepared by a preparation method comprising the following steps of:
(a) Weighing 4mmol of Bi (NO) 3 ·5H 2 O and 4mmol of KIO 3 Completely dispersing the mixture into 60ml of mixed organic solvent of glycol and ethanol, wherein the ratio of the glycol to the ethanol is 1:3, and then magnetically stirring the mixture for 30min to obtain a mixed solution, wherein the rotating speed of the magnetic stirring is 800r/min;
(b) Transferring the mixed solution into a 100ml hydrothermal kettle, carrying out hydrothermal reaction at 180 ℃ for 48h, and then cooling to room temperature to obtain a reaction crude product;
(c) And (3) centrifugally washing the reaction crude product for 5 times by using deionized water and absolute ethyl alcohol, setting the centrifugal rotating speed at 5500r/min, and drying the centrifugally collected product in a drying box at 100 ℃ for 8 hours to obtain the three-dimensional marigold-shaped bismuth oxyiodate photocatalyst.
Example 3
The bismuth oxyiodate is prepared by a preparation method comprising the following steps of:
(a) 3mmol of Bi (NO) are weighed 3 ·5H 2 O and 3mmol of KIO 3 All dispersed to 60ml ofIn a mixed organic solvent of glycol and ethanol, the ratio of glycol to ethanol is 1;
(b) Transferring the mixed solution into a 100ml hydrothermal kettle, carrying out hydrothermal reaction at 178 ℃ for 36h, and then cooling to room temperature to obtain a reaction crude product;
(c) And (3) centrifugally washing the reaction crude product for 5 times by using deionized water and absolute ethyl alcohol, then centrifugally washing at the rotating speed of 6000r/min, and drying the centrifugally collected product in a drying box at the temperature of 80 ℃ for 10 hours to obtain the three-dimensional marigold-shaped bismuth oxyiodate photocatalyst.
Example 4
Bismuth oxyiodate is used in the photocatalytic reaction for removing heavy metal mercury, 50mg of photocatalyst is weighed under the irradiation of visible light to carry out the heavy metal mercury removal experiment, and the initial concentration is 50 mu g/m 3 The catalyst is firstly adsorbed and desorbed to reach balance in the dark for 15min, and the removal efficiency of the three-dimensional marigold-shaped bismuth oxyiodide reaches 78% in the visible light irradiation photocatalysis removal process for 45min, as shown in figure 3. Meanwhile, the efficiency is not obviously reduced after 6 times of cycle experiments, which shows that the long-acting life is realized.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (6)
1. The preparation method of the three-dimensional marigold-shaped bismuth oxyiodate is characterized by comprising the following steps of:
(a) Bi (NO) 3 ·5H 2 O and KIO 3 Uniformly dispersing in mixed organic solvent, stirring to obtain mixtureSolution A;
(b) Transferring the mixed solution A into a reaction vessel for solvothermal reaction to obtain a reaction crude product B;
(c) Sequentially carrying out centrifugal washing and drying on the reaction crude product B to obtain a finished bismuth oxyiodide product;
in the step (a), the molar ratio of the bismuth nitrate pentahydrate to the potassium iodate is 1:1;
the mixed organic solvent in the step (a) is ethylene glycol and ethanol, and the molar ratio of the ethylene glycol to the ethanol is 1 (2~3);
in the step (b), the reaction temperature of the solvothermal reaction is 160-180 ℃, and the reaction time is 25-48h.
2. The method for preparing three-dimensional marigold-like bismuth oxyiodate according to claim 1, wherein in the step (a), magnetic stirring is adopted, the rotating speed of the magnetic stirring is 600-1000r/min, and the time of the magnetic stirring is 30-50min.
3. The method for preparing three-dimensional marigold-like bismuth oxyiodate according to claim 1, wherein in the step (c), deionized water and absolute ethyl alcohol are adopted for centrifugal washing, the rotating speed of the centrifugal washing is 5000-6000r/min, and the times of the centrifugal washing are 4-5 times.
4. The method for preparing three-dimensional marigold-like bismuth oxyiodate according to claim 1, wherein in the step (c), the drying temperature is 80-100 ℃, and the drying time is 8-10h.
5. The bismuth oxyiodate obtained by the preparation method according to any one of claims 1 to 4, wherein the bismuth oxyiodate is in the shape of a three-dimensional marigold nanoflower.
6. Use of the bismuth oxyiodate according to claim 5 in a photocatalyst.
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