CN111533169A - Preparation method of petal-shaped bismuth oxyhalide material - Google Patents
Preparation method of petal-shaped bismuth oxyhalide material 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 34
- 239000000463 material Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 21
- 238000001035 drying Methods 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 238000002485 combustion reaction Methods 0.000 claims abstract description 14
- 239000002243 precursor Substances 0.000 claims abstract description 14
- 150000001621 bismuth Chemical class 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000012153 distilled water Substances 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 238000000498 ball milling Methods 0.000 claims abstract description 9
- 150000004820 halides Chemical class 0.000 claims abstract description 9
- 230000002269 spontaneous effect Effects 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 4
- 238000005303 weighing Methods 0.000 claims abstract description 4
- 150000005846 sugar alcohols Polymers 0.000 claims abstract description 3
- 229920005862 polyol Polymers 0.000 claims description 8
- 150000003077 polyols Chemical class 0.000 claims description 8
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical group [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims description 7
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 6
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical group [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 6
- JHJLBTNAGRQEKS-UHFFFAOYSA-M sodium bromide Chemical compound [Na+].[Br-] JHJLBTNAGRQEKS-UHFFFAOYSA-M 0.000 claims description 6
- FVAUCKIRQBBSSJ-UHFFFAOYSA-M sodium iodide Chemical compound [Na+].[I-] FVAUCKIRQBBSSJ-UHFFFAOYSA-M 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 4
- 229940107816 ammonium iodide Drugs 0.000 claims description 4
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical group [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 claims description 4
- 125000001453 quaternary ammonium group Chemical group 0.000 claims description 4
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- 150000003841 chloride salts Chemical class 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- 229920001451 polypropylene glycol Polymers 0.000 claims description 3
- 239000001103 potassium chloride Substances 0.000 claims description 3
- 235000011164 potassium chloride Nutrition 0.000 claims description 3
- QYIGOGBGVKONDY-UHFFFAOYSA-N 1-(2-bromo-5-chlorophenyl)-3-methylpyrazole Chemical compound N1=C(C)C=CN1C1=CC(Cl)=CC=C1Br QYIGOGBGVKONDY-UHFFFAOYSA-N 0.000 claims description 2
- XZXYQEHISUMZAT-UHFFFAOYSA-N 2-[(2-hydroxy-5-methylphenyl)methyl]-4-methylphenol Chemical compound CC1=CC=C(O)C(CC=2C(=CC=C(C)C=2)O)=C1 XZXYQEHISUMZAT-UHFFFAOYSA-N 0.000 claims description 2
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical class [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 claims description 2
- SWLVFNYSXGMGBS-UHFFFAOYSA-N ammonium bromide Chemical compound [NH4+].[Br-] SWLVFNYSXGMGBS-UHFFFAOYSA-N 0.000 claims description 2
- 235000019270 ammonium chloride Nutrition 0.000 claims description 2
- -1 bismuth halide Chemical class 0.000 claims description 2
- 229910000380 bismuth sulfate Inorganic materials 0.000 claims description 2
- FBXVOTBTGXARNA-UHFFFAOYSA-N bismuth;trinitrate;pentahydrate Chemical group 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 2
- FIMTUWGINXDGCK-UHFFFAOYSA-H dibismuth;oxalate Chemical compound [Bi+3].[Bi+3].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O FIMTUWGINXDGCK-UHFFFAOYSA-H 0.000 claims description 2
- BEQZMQXCOWIHRY-UHFFFAOYSA-H dibismuth;trisulfate Chemical compound [Bi+3].[Bi+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O BEQZMQXCOWIHRY-UHFFFAOYSA-H 0.000 claims description 2
- 150000002496 iodine Chemical class 0.000 claims description 2
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 claims description 2
- PNYYBUOBTVHFDN-UHFFFAOYSA-N sodium bismuthate Chemical compound [Na+].[O-][Bi](=O)=O PNYYBUOBTVHFDN-UHFFFAOYSA-N 0.000 claims description 2
- 239000011780 sodium chloride Substances 0.000 claims description 2
- 235000002639 sodium chloride Nutrition 0.000 claims description 2
- 235000009518 sodium iodide Nutrition 0.000 claims description 2
- DNIAPMSPPWPWGF-GSVOUGTGSA-N (R)-(-)-Propylene glycol Chemical compound C[C@@H](O)CO DNIAPMSPPWPWGF-GSVOUGTGSA-N 0.000 claims 1
- 150000003842 bromide salts Chemical class 0.000 claims 1
- XMBWDFGMSWQBCA-UHFFFAOYSA-M iodide Chemical compound [I-] XMBWDFGMSWQBCA-UHFFFAOYSA-M 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 4
- 238000007146 photocatalysis Methods 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 239000002131 composite material Substances 0.000 abstract description 2
- 239000008204 material by function Substances 0.000 abstract description 2
- 229920000642 polymer Polymers 0.000 abstract 1
- 239000000047 product Substances 0.000 description 9
- 239000002245 particle Substances 0.000 description 5
- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 229910052794 bromium Inorganic materials 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- 239000012467 final product Substances 0.000 description 3
- 229910021389 graphene Inorganic materials 0.000 description 3
- 229910052740 iodine Inorganic materials 0.000 description 3
- 239000012856 weighed raw material Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000004070 electrodeposition Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 150000002334 glycols Chemical class 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 238000009827 uniform distribution Methods 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 1
- 239000005997 Calcium carbide Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001805 chlorine compounds Chemical group 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 150000002191 fatty alcohols Chemical class 0.000 description 1
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000000243 photosynthetic effect Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 229940113115 polyethylene glycol 200 Drugs 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000001022 rhodamine dye Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- CLZWAWBPWVRRGI-UHFFFAOYSA-N tert-butyl 2-[2-[2-[2-[bis[2-[(2-methylpropan-2-yl)oxy]-2-oxoethyl]amino]-5-bromophenoxy]ethoxy]-4-methyl-n-[2-[(2-methylpropan-2-yl)oxy]-2-oxoethyl]anilino]acetate Chemical compound CC1=CC=C(N(CC(=O)OC(C)(C)C)CC(=O)OC(C)(C)C)C(OCCOC=2C(=CC=C(Br)C=2)N(CC(=O)OC(C)(C)C)CC(=O)OC(C)(C)C)=C1 CLZWAWBPWVRRGI-UHFFFAOYSA-N 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
Images
Classifications
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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
-
- 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
A preparation method of petal-shaped bismuth oxyhalide material comprises weighing a certain amount of bismuth salt, halide and polyalcohol polymer raw materials, dissolving the raw materials in distilled water, and stirring to obtain uniform solution; placing the obtained solution in an oven to be dried to obtain a precursor, then placing the precursor in a crucible to be heated in the air for spontaneous combustion, and utilizing the reaction heat to enable the synthesis reaction to be self-maintained until the reaction is finished; and (3) washing the combustion product, drying in an oven, naturally cooling, and ball-milling in a high-speed ball mill to obtain the bismuth oxyhalide. The bismuth oxyhalide material synthesized by the method has the petal shape of a three-dimensional reticular structure, and can be widely applied to the aspects of electronic functional materials, photocatalysis, photoelectric materials, medical composite materials and the like.
Description
Technical Field
The invention relates to a preparation technology of a petal-shaped bismuth oxyhalide material, belonging to the fields of photocatalysis and electrochemistry.
Background
With the rapid development of modern industry, the problems of energy shortage and environmental pollution become two major problems affecting the development and quality of life of human society in the world today. The bismuth-based oxide material has smaller bandwidth, can be excited by visible light, can effectively remove pollutants under the irradiation of the visible light, and can be used for photocatalytic degradation of industrial wastewater. In recent years, two-dimensional layered structure materials have been receiving increasing attention from researchers in the fields of electronic devices, catalysis, energy utilization, and the like, such as graphene (including graphene, graphene oxide), boron nitride, two-dimensional transition metal sulfide, two-dimensional calcium carbide, two-dimensional perovskite, layered hydrogen hydroxide, and the like. Bismuth oxyhalide (BiOX, X = Cl, Br, I) material itself has the advantages of graphene-like two-dimensional layered structure, unique crystal structure, suitable energy band position, high chemical stability, low cost, easy preparation and the like, and is widely concerned by researchers.
Bismuth oxyhalide (BiOX, X = Cl, Br, I) is used as a layered material, and the current methods for synthesizing bismuth oxyhalide catalysts mainly include: hydrolysis, hydrothermal (solvothermal) methods, room temperature ultrasound methods, electrodeposition methods, and the like. Zhu et al BiCl3The raw material is ethylene glycol as solvent, spherical BiOCl powder is prepared by a hydrothermal method, and the powder has higher photocatalytic activity (Zhu L P, LiaoG H, Self-Assembled 3D BiOCl hierarchy: Tunable Synthesis and catalysis, Crystal, Eng. Comm,2010,12: 3791-3796); wang et al use of BiBr3As raw materials, BiOBr (Wang Y, Shi Z Q. Synthesis, chromatography, and Photosynthetic Properties of BiOBr catalyst. Journal of Solid State chemistry,2013,199: 224-; preparing oxyhalogen in high-pressure reaction kettle by Zhang Xiaoyang and the like by hydrothermal methodBismuth (chinese patent CN 110104684 a); the yellow march adopts an electrodeposition method to obtain bismuth oxyhalide through an anodic oxidation reaction (Chinese patent CN 108745386A). The hydrolysis method is a common method for preparing (BiOX, X = Cl, Br, I), and has the disadvantages of easy operation, mild conditions and low equipment requirements, but easily causes over-high local concentration, so that the product has poor dispersibility, uneven particle size and difficult control of morphology. The hydrothermal (solvothermal) method can provide extreme conditions of high temperature and high pressure, and can realize primary control on the particle size and the morphology of a product by controlling reaction parameters (pH value, reaction temperature and reaction time). However, the hydrothermal method has the disadvantages of higher equipment cost, complex operation, overlong preparation time, difficulty in large-scale production and certain distance from industrial production. The sol-gel method is an important method for preparing BiOX nano particles, the particle size of the obtained product is small and the distribution is uniform, the catalyst prepared by the method has high purity, mild reaction conditions and uniform distribution of doping components, but the surface tension of the liquid can cause the collapse and shrinkage of pores during drying, so the material has low mechanical strength and poor formability; the normal temperature ultrasonic method can control the size and distribution of particles by controlling the vibration frequency of ultrasonic waves, and the obtained product has small particle size, uniform distribution and difficult agglomeration, but the ultrasonic waves are harmful to human bodies and inconvenient to put into production.
In summary, the operation of the existing operation method for preparing bismuth oxyhalide is complex and time-consuming, and needs to be further perfected. The mature preparation method and the mature preparation process are the key for obtaining the high-performance bismuth oxyhalide material.
Disclosure of Invention
The invention aims to provide a preparation method for synthesizing a petal-shaped bismuth oxyhalide material.
The invention relates to a preparation method of a petal-shaped bismuth oxyhalide material, which comprises the following steps:
weighing a certain amount of bismuth salt, halide and polyol raw materials, dissolving the bismuth salt, the halide and the polyol raw materials in distilled water, and fully stirring to form a uniform solution;
step (2), drying the obtained solution to obtain a precursor, then placing the precursor in a crucible, heating in air for spontaneous combustion, and utilizing reaction heat to enable the reaction to be self-maintained until the reaction is finished;
and (3) washing the combustion product, drying in an oven, naturally cooling, and ball-milling in a high-speed ball mill to obtain the bismuth oxyhalide.
The method has the beneficial effects of solving the problems that the existing method for preparing the bismuth oxyhalide is complex in operation, long in time consumption and easy to cause environmental pollution. The bismuth oxyhalide material synthesized by the method has the shape of petals with a three-dimensional net structure. Can be widely applied to electronic functional materials, photocatalysis, photoelectric materials and medical composite materials.
Drawings
Fig. 1 is a scanning electron microscope atlas of a single petal-shaped BiOCl material prepared in example 1, fig. 2 is a scanning electron microscope atlas of a plurality of petal-shaped BiOCl materials prepared in example 1, and fig. 3 is a kinetic graph of photocatalytic degradation of rhodamine dye of a petal-shaped bismuth oxyhalide material prepared in example 1.
Detailed Description
The invention relates to a preparation method of a petal-shaped bismuth oxyhalide material, which comprises the following steps:
weighing a certain amount of bismuth salt, halide and polyol raw materials, dissolving the bismuth salt, the halide and the polyol raw materials in distilled water, and fully stirring to form a uniform solution;
step (2), drying the obtained solution to obtain a precursor, then placing the precursor in a crucible, heating in air for spontaneous combustion, and utilizing reaction heat to enable the reaction to be self-maintained until the reaction is finished;
and (3) washing the combustion product, drying in an oven, naturally cooling, and ball-milling in a high-speed ball mill to obtain the bismuth oxyhalide.
According to the preparation method of the petal-shaped bismuth oxyhalide material, the bismuth salt is bismuth nitrate pentahydrate, or bismuth sulfate, or bismuth acetate, or bismuth oxalate, or sodium bismuthate, or halogenated bismuth.
In the preparation method of the petal-shaped bismuth oxyhalide material, the halide is chloride, or bromide, or iodide; the chloride salt is potassium chloride, or sodium chloride, or ammonium chloride, or quaternary ammonium chloride; the bromine salt is potassium bromide, or sodium bromide, or ammonium bromide, or quaternary ammonium bromide; the iodine salt is potassium iodide, or sodium iodide, or ammonium iodide, or quaternary ammonium iodide.
In the preparation method of the petal-shaped bismuth oxyhalide material, the polymeric polyol is polyethylene glycol series, polypropylene glycol series, fatty alcohol or pentaerythritol.
According to the preparation method of the petal-shaped bismuth oxyhalide material, the mass ratio of the polyhydric alcohol to the bismuth salt is 1: 1-8: 1.
According to the preparation method of the petal-shaped bismuth oxyhalide material, the drying temperature is 50-150 ℃, and the drying time is 1-5 hours.
According to the preparation method of the petal-shaped bismuth oxyhalide material, the ball milling time in the step (3) is 1-30 minutes.
The following embodiments are further described, but not limited to, the technical solutions of the present invention are modified or equivalent substitutions and modifications are made without departing from the spirit and scope of the technical solutions of the present invention.
Example 1:
weigh 4.85gBi (NO)3)3▪5H2O and 0.82 g KCl, and 15.0 g polyethylene glycol 2000; dissolving the weighed raw materials in distilled water at 60 ℃, and fully stirring to form a uniform solution; placing the obtained solution in a drying oven at 120 ℃ for drying for 3 hours to obtain a precursor, and placing the obtained precursor in a crucible to heat in air for spontaneous combustion; the combustion products are cooled, washed twice with distilled water and absolute ethyl alcohol in turn, and dried at 120 ℃. And finally, performing ball milling in a high-speed ball mill for 5 minutes to obtain a final product.
Example 2:
3.86g of C are weighed2H3BiO2And 1.10g NaBr, mixed with 10.0 g polyethylene glycol 200; dissolving the weighed raw materials in distilled water at 80 ℃, and fully stirring to form a uniform solution; and then, placing the solution in an oven at 140 ℃ for drying for 2 hours to obtain a dry precursor.Placing the obtained precursor in a crucible, and heating in air for spontaneous combustion; the combustion products are cooled, washed twice with distilled water and absolute ethyl alcohol in turn, and dried at 130 ℃. And finally, performing ball milling in a high-speed ball mill for 10 minutes to obtain a final product.
Example 3:
8.08g of Bi are weighed2(C2O4)3.7H2O and 0.75g KI, and mixed with 8.0g polypropylene glycol 400; dissolving the weighed raw materials in distilled water at 70 ℃, and fully stirring to form a uniform solution; and (3) placing the obtained solution in an oven at 150 ℃ for drying for 1 hour to obtain a dry precursor. Placing the obtained precursor in a crucible, and heating in air for spontaneous combustion; the combustion products are cooled, washed twice with distilled water and absolute ethyl alcohol in turn, and dried at 150 ℃. And finally, ball-milling the mixture in a high-speed ball mill for 15 minutes to obtain a final product.
Claims (7)
1. A preparation method of petal-shaped bismuth oxyhalide material is characterized by comprising the following steps:
weighing a certain amount of bismuth salt, halide and polyol raw materials, dissolving the bismuth salt, the halide and the polyol raw materials in distilled water, and fully stirring to form a uniform solution;
step (2), drying the obtained solution to obtain a precursor, then placing the precursor in a crucible, heating in air for spontaneous combustion, and utilizing reaction heat to enable the reaction to be self-maintained until the reaction is finished;
and (3) washing the combustion product, drying in an oven, naturally cooling, and ball-milling in a high-speed ball mill to obtain the bismuth oxyhalide.
2. The method of preparing petal-shaped bismuth oxyhalide material of claim 1, wherein the bismuth salt is bismuth nitrate pentahydrate, or bismuth sulfate, or bismuth acetate, or bismuth oxalate, or sodium bismuthate, or bismuth halide.
3. The method of preparing a petal bismuth oxyhalide material of claim 1, wherein the halide is a chloride salt, or a bromide salt, or an iodide salt; the chloride salt is potassium chloride, or sodium chloride, or ammonium chloride, or quaternary ammonium chloride; the bromine salt is potassium bromide, or sodium bromide, or ammonium bromide, or quaternary ammonium bromide; the iodine salt is potassium iodide, or sodium iodide, or ammonium iodide, or quaternary ammonium iodide.
4. The method of claim 1, wherein the polymeric polyol is selected from the group consisting of polyethylene glycol, polypropylene glycol, aliphatic alcohol, and pentaerythritol.
5. The preparation method of the petal-shaped bismuth oxyhalide material according to claim 1, wherein the mass ratio of the polyhydric alcohol to the bismuth salt is 1: 1-8: 1.
6. The method for preparing petal-shaped bismuth oxyhalide material according to claim 1, wherein the drying temperature is 50-150 ℃ and the drying time is 1-5 hours.
7. The method for preparing petal-shaped bismuth oxyhalide material according to claim 1, wherein the ball milling time in the step (3) is 1-30 minutes.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113649029A (en) * | 2021-08-18 | 2021-11-16 | 吉林建筑大学 | Preparation method and application of BiOCl nano photocatalyst with high visible light catalytic activity |
| CN114797907A (en) * | 2022-03-08 | 2022-07-29 | 中国石油大学(北京) | Bismuth oxyhalide solid solution photoelectric film, and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN113649029B (en) * | 2021-08-18 | 2023-12-12 | 吉林建筑大学 | Preparation method and application of BiOCl nano photocatalyst with high visible light catalytic activity |
| CN114797907A (en) * | 2022-03-08 | 2022-07-29 | 中国石油大学(北京) | Bismuth oxyhalide solid solution photoelectric film, and preparation method and application thereof |
| CN114797907B (en) * | 2022-03-08 | 2024-04-05 | 中国石油大学(北京) | Bismuth oxyhalide solid solution photoelectric film, and preparation method and application thereof |
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