CN112850649B - Preparation method of bismuth oxybromide nanosheet - Google Patents
Preparation method of bismuth oxybromide nanosheet Download PDFInfo
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- 239000002135 nanosheet Substances 0.000 title claims abstract description 37
- OZKCXDPUSFUPRJ-UHFFFAOYSA-N oxobismuth;hydrobromide Chemical compound Br.[Bi]=O OZKCXDPUSFUPRJ-UHFFFAOYSA-N 0.000 title claims abstract description 12
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 46
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims abstract description 38
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 30
- SWLVFNYSXGMGBS-UHFFFAOYSA-N ammonium bromide Chemical compound [NH4+].[Br-] SWLVFNYSXGMGBS-UHFFFAOYSA-N 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000008367 deionised water Substances 0.000 claims abstract description 28
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 28
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000001816 cooling Methods 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 15
- 238000003756 stirring Methods 0.000 claims abstract description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000005303 weighing Methods 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 9
- 235000019270 ammonium chloride Nutrition 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 239000006228 supernatant Substances 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 238000007789 sealing Methods 0.000 claims abstract description 6
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 3
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 30
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 20
- 239000002994 raw material Substances 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 2
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 13
- 230000002194 synthesizing effect Effects 0.000 description 6
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000004729 solvothermal method Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical group [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 238000010335 hydrothermal treatment Methods 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002055 nanoplate Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B11/00—Oxides or oxyacids of halogens; Salts thereof
- C01B11/20—Oxygen compounds of bromine
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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Abstract
The preparation method of the bismuth oxybromine nanosheet comprises the following steps: 1) weighing bismuth nitrate, dissolving the bismuth nitrate in ethylene glycol, and adjusting the concentration of the formed bismuth nitrate solution to be: 0.05-0.4 mol/L; 2) weighing ammonium bromide, dissolving the ammonium bromide in deionized water, and adjusting the concentration of the formed ammonium bromide solution to be: 0.01-0.06 mol/L; 3) pouring the bismuth nitrate solution obtained in the step 1) into the ammonium bromide solution obtained in the step 2), adjusting the molar ratio of ammonium chloride to bismuth nitrate to be 2: 1-3: 1, stirring, and transferring to a high-pressure reaction kettle; 4) sealing the reaction kettle, carrying out heat treatment at 100-160 ℃, cooling to room temperature, pouring out supernatant, adjusting the pH value, stirring, and transferring to a high-pressure reaction kettle; 5) and (3) sealing the reaction kettle, preserving heat at 80-100 ℃ for 8-12 hours for heat treatment, then cooling to room temperature, filtering, sequentially washing with deionized water and absolute ethyl alcohol, and drying at 60-80 ℃ to obtain the bismuth oxybromide nanosheet. The method has the advantages of simple process, easy control, no environmental pollution, low cost and easy large-scale production.
Description
Technical Field
The invention belongs to the technical field of inorganic non-metallic material manufacturing, and particularly relates to a preparation method of a BiOBr nanosheet.
Background
Energy is the most important material basis for human survival development, and with the increasing shortage of traditional fossil energy and the increasing demand of human for energy, new energy, particularly renewable energy, becomes a hot spot for the current social and scientific development. BiOBr is a semiconductor material with excellent photocatalytic performance under visible light, and becomes a hot spot of research in the field of photocatalysis at present. The structure of the BiOBr is a tetragonal lead fluochloride ore type, has the advantages of smaller forbidden bandwidth, better visible light response, abundant halogen resources, environmental friendliness, good stability and the like, and has wide application prospect.
The current main methods for synthesizing BiOBr comprise microwave, deposition, hydrothermal method and the like. The hydrothermal solvothermal method is widely used for preparing various nano materials due to the advantages of easy control of crystal growth reaction kinetics, high product crystallinity and the like, and different particle morphologies show different electrochemical properties. At present, BiOBr synthesized at home and abroad is generally complex in process and large in grain size, and the photocatalytic activity of the BiOBr is inhibited.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a hydrothermal synthesis preparation method of the BiOBr nanosheet, which is simple in process and easy to control.
The invention adopts the following technical scheme:
a preparation method of bismuth oxybromine nanosheets comprises the following steps:
1) weighing bismuth nitrate in a certain amount, dissolving the bismuth nitrate in ethylene glycol, and adjusting the concentration of the formed bismuth nitrate solution to be: 0.05-0.4 mol/L;
2) weighing ammonium bromide in a metering manner, dissolving the ammonium bromide in deionized water, and adjusting the concentration of the formed ammonium bromide solution to be: 0.01-0.06 mol/L;
3) pouring the bismuth nitrate solution obtained in the step 1) into the ammonium bromide solution obtained in the step 2), adjusting the molar ratio of ammonium chloride to bismuth nitrate to be 2: 1-3: 1, stirring, and transferring to a high-pressure reaction kettle;
4) sealing the high-pressure reaction kettle, carrying out heat treatment at 100-160 ℃, then cooling to room temperature, pouring out supernatant, adjusting the pH value, and stirring;
5) and (3) sealing the high-pressure reaction kettle, preserving heat at 80-100 ℃ for 8-12 hours for heat treatment, then cooling to room temperature, filtering, sequentially washing with deionized water and absolute ethyl alcohol, and drying at 60-80 ℃ to obtain the bismuth oxybromide nanosheet.
Preferably, in the step 4), hydrochloric acid is added to adjust the pH value to 1-3, and then potassium hydroxide is added to adjust the pH value to 8-10.
Preferably, the purity of the used raw materials of ammonium bromide, bismuth nitrate, hydrochloric acid, potassium hydroxide, solvent ethylene glycol, deionized water and absolute ethyl alcohol is not lower than chemical purity.
Preferably, the prepared bismuth oxybromide is in a nano-sheet shape, the width of the bismuth oxybromide nano-sheet is not more than 300 nanometers, the thickness of the bismuth oxybromide nano-sheet is not more than 20 nanometers, and the bismuth oxybromide nano-sheet grows along the (001) plane.
According to the method, bismuth nitrate, ammonium bromide and the like are used as raw materials, the growth process of BiOBr is controlled by regulating and controlling the time and temperature of hydrothermal treatment by regulating and controlling the amount of each raw material substance in a mixed solvent and preferably using hydrochloric acid and potassium hydroxide as pH regulators, so that the synthesis of BiOBr nanosheets is realized. The cleaning of the water/solvothermal synthesis product is to remove excessive reactants and obtain pure BiOBr nano-sheets. Dehydration by absolute ethyl alcohol and drying at the temperature of not higher than 80 ℃ are adopted to obtain the BiOBr nano-sheet with good dispersibility.
The invention has simple process, easy control, no environmental pollution, low cost and easy large-scale production; the width of the prepared BiOBr nano sheet is not more than 300 nanometers, the thickness of the prepared BiOBr nano sheet is not more than 20 nanometers, and the BiOBr nano sheet grows along a (001) plane; the product has stable quality, high purity and good powder particle dispersibility.
Drawings
Figure 1X-ray diffraction (XRD) pattern of the synthetic BiOBr nanoplates of the present invention;
fig. 2 is a Transmission Electron Microscope (TEM) photograph of the synthesized BiOBr nanosheets of the present invention.
Detailed Description
The present invention is further illustrated by the following examples.
Example 1
Synthesizing a BiOBr nano sheet according to the following process steps:
1) measuring bismuth nitrate by a metering amount, dissolving the bismuth nitrate in ethylene glycol, and adjusting the concentration of the formed bismuth nitrate solution to be: 0.2 mol/L;
2) weighing ammonium bromide in a metering manner, dissolving the ammonium bromide in deionized water, and adjusting the concentration of the formed ammonium bromide solution to be: 0.04 mol/L;
3) slowly pouring the solution obtained in the step 1) into the solution obtained in the step 2), adjusting the molar ratio of ammonium chloride to bismuth nitrate to be 3:1, stirring, transferring to a high-pressure reaction kettle, and adjusting 4/5 the volume of which accounts for the volume of the reaction kettle by using deionized water;
4) the reaction kettle with the reaction materials is sealed and heat-treated at 140 ℃ for 8 hours. Then, cooling to room temperature, pouring out supernatant, adding hydrochloric acid to adjust the pH value to 1, then adding potassium hydroxide to adjust the pH value to 10, stirring, and adjusting the volume of 4/5 which accounts for the volume of the reaction kettle by using deionized water;
5) the reaction kettle with the reaction materials is sealed and heat-treated at 100 ℃ for 8 hours. And then, cooling to room temperature, filtering, sequentially washing with deionized water and absolute ethyl alcohol, and drying at the temperature of 60 ℃ to obtain the BiOBr nanosheet.
The X-ray diffraction (XRD) pattern of the BiOBr nanosheet synthesized in this example is shown in fig. 1; a Transmission Electron Microscope (TEM) photograph thereof is shown in FIG. 2.
In the embodiment, BiOBr nano sheets with the width not more than 300 nanometers and the thickness not more than 20 nanometers are synthesized by a water/solvothermal method.
Example 2
Synthesizing a BiOBr nano sheet according to the following process steps:
1) measuring bismuth nitrate by a metering amount, dissolving the bismuth nitrate in ethylene glycol, and adjusting the concentration of the formed bismuth nitrate solution to be: 0.1 mol/L;
2) weighing ammonium bromide in a metering manner, dissolving the ammonium bromide in deionized water, and adjusting the concentration of the formed ammonium bromide solution to be: 0.02 mol/L;
3) slowly pouring the solution obtained in the step 1) into the solution obtained in the step 2), adjusting the molar ratio of ammonium chloride to bismuth nitrate to be 2:1, stirring, transferring into a high-pressure reaction kettle, and adjusting 2/3 the volume of which accounts for the volume of the reaction kettle by using deionized water;
4) the reaction kettle with the reaction materials is sealed and heat-treated at 120 ℃ for 24 hours. Then, cooling to room temperature, pouring out supernatant, adding hydrochloric acid to adjust the pH value to 3, then adding potassium hydroxide to adjust the pH value to 8, stirring, and adjusting the volume of 4/5 which accounts for the volume of the reaction kettle by using deionized water;
5) the reaction kettle with the reaction materials is sealed and heat-treated at 100 ℃ for 12 hours. And then cooling to room temperature, filtering, sequentially washing with deionized water and absolute ethyl alcohol, and drying at the temperature of 80 ℃ to obtain the BiOBr nanosheet.
Example 3
Synthesizing a BiOBr nano sheet according to the following process steps:
1) measuring bismuth nitrate by a metering amount, dissolving the bismuth nitrate in ethylene glycol, and adjusting the concentration of the formed bismuth nitrate solution to be: 0.1 mol/L;
2) weighing ammonium bromide in a metering manner, dissolving the ammonium bromide in deionized water, and adjusting the concentration of the formed ammonium bromide solution to be: 0.02 mol/L;
3) slowly pouring the solution obtained in the step 1) into the solution obtained in the step 2), adjusting the molar ratio of ammonium chloride to bismuth nitrate to be 3:1, stirring, transferring to a high-pressure reaction kettle, and adjusting 3/4 the volume of which accounts for the volume of the reaction kettle by using deionized water;
4) the reaction kettle with the reaction materials is sealed and heat-treated at 120 ℃ for 8 hours. Then, cooling to room temperature, pouring out supernatant, adding hydrochloric acid to adjust the pH value to 2, then adding potassium hydroxide to adjust the pH value to 9, stirring, and adjusting the volume of 4/5 which accounts for the volume of the reaction kettle by using deionized water;
5) the reaction kettle with the reaction materials is sealed and heat-treated at 100 ℃ for 12 hours. And then, cooling to room temperature, filtering, sequentially washing with deionized water and absolute ethyl alcohol, and drying at the temperature of 60 ℃ to obtain the BiOBr nanosheet.
Example 4
Synthesizing a BiOBr nano sheet according to the following process steps:
1) measuring bismuth nitrate by a metering amount, dissolving the bismuth nitrate in ethylene glycol, and adjusting the concentration of the formed bismuth nitrate solution to be: 0.4 mol/L;
2) weighing ammonium bromide in a metering manner, dissolving the ammonium bromide in deionized water, and adjusting the concentration of the formed ammonium bromide solution to be: 0.06 mol/L;
3) slowly pouring the solution obtained in the step 1) into the solution obtained in the step 2), adjusting the molar ratio of ammonium chloride to bismuth nitrate to be 2:1, stirring, transferring into a high-pressure reaction kettle, and adjusting 4/5 the volume of which accounts for the volume of the reaction kettle by using deionized water;
4) the reaction kettle with the reaction materials is sealed and heat-treated at 160 ℃ for 12 hours. Then, cooling to room temperature, pouring out supernatant, adding hydrochloric acid to adjust the pH value to 3, then adding potassium hydroxide to adjust the pH value to 10, stirring, and adjusting the volume of 4/5 which accounts for the volume of the reaction kettle by using deionized water;
5) the reaction kettle with the reaction materials is sealed and heat-treated at 100 ℃ for 12 hours. And then cooling to room temperature, filtering, sequentially washing with deionized water and absolute ethyl alcohol, and drying at the temperature of 80 ℃ to obtain the BiOBr nanosheet.
Example 5
Synthesizing a BiOBr nano sheet according to the following process steps:
1) measuring bismuth nitrate by a metering amount, dissolving the bismuth nitrate in ethylene glycol, and adjusting the concentration of the formed bismuth nitrate solution to be: 0.05 mol/L;
2) weighing ammonium bromide in a metering manner, dissolving the ammonium bromide in deionized water, and adjusting the concentration of the formed ammonium bromide solution to be: 0.01 mol/L;
3) slowly pouring the solution obtained in the step 1) into the solution obtained in the step 2), adjusting the molar ratio of ammonium chloride to bismuth nitrate to be 2:1, stirring, transferring into a high-pressure reaction kettle, and adjusting 3/4 the volume of which accounts for the volume of the reaction kettle by using deionized water;
4) the reaction kettle with the reaction materials is sealed and heat-treated at 100 ℃ for 9 hours. Then, cooling to room temperature, pouring out supernatant, adding hydrochloric acid to adjust the pH value to 1, then adding potassium hydroxide to adjust the pH value to 8, stirring, and adjusting the volume of 4/5 which accounts for the volume of the reaction kettle by using deionized water;
5) the reaction kettle with the reaction materials is sealed and heat-treated at 80 ℃ for 8 hours. And then, cooling to room temperature, filtering, sequentially washing with deionized water and absolute ethyl alcohol, and drying at the temperature of 60 ℃ to obtain the BiOBr nanosheet.
The preparation method is simple to operate, adopts common raw material reagents, and is low in cost. The thickness of the BiOBr nano sheet prepared by the simple hydrothermal method is not more than 20nm, the particle size of the BiOBr is reduced, the specific surface area of the material is increased, and the subsequent load treatment is facilitated.
Claims (3)
1. A preparation method of bismuth oxybromine nanosheets is characterized by comprising the following steps:
1) weighing bismuth nitrate in a certain amount, dissolving the bismuth nitrate in ethylene glycol, and adjusting the concentration of the formed bismuth nitrate solution to be: 0.05-0.4 mol/L;
2) weighing ammonium bromide in a metering manner, dissolving the ammonium bromide in deionized water, and adjusting the concentration of the formed ammonium bromide solution to be: 0.01-0.06 mol/L;
3) pouring the bismuth nitrate solution obtained in the step 1) into the ammonium bromide solution obtained in the step 2), adjusting the molar ratio of ammonium chloride to bismuth nitrate to be 2: 1-3: 1, stirring, and transferring to a high-pressure reaction kettle;
4) sealing the high-pressure reaction kettle, carrying out heat treatment at 100-160 ℃, then cooling to room temperature, pouring out supernatant, adjusting the pH value, firstly adding hydrochloric acid to adjust the pH value to 1-3, and then adding potassium hydroxide to adjust the pH value to 8-10;
5) and (3) sealing the high-pressure reaction kettle, preserving heat at 80-100 ℃ for 8-12 hours for heat treatment, then cooling to room temperature, filtering, sequentially washing with deionized water and absolute ethyl alcohol, and drying at 60-80 ℃ to obtain the bismuth oxybromide nanosheet.
2. The method for preparing bismuth oxybromide nanosheets as claimed in claim 1, wherein the raw materials used are ammonium bromide, bismuth nitrate, hydrochloric acid, potassium hydroxide, and the solvents ethylene glycol, deionized water and absolute ethyl alcohol, all of which have a purity not lower than chemical purity.
3. A method for preparing bismuth oxybromide nanosheets as claimed in any one of claims 1 to 2, wherein the bismuth oxybromide prepared is nanosheets, having a width of no greater than 300 nm and a thickness of no greater than 20nm, and growing along a surface.
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